****************************************************************************** From: dieter.zimmer.dz@bayer-ag.de Date: Tue, 2 Jan 2001 09:23:20 +0100 Subject: Re: 61.5 Da increase Organization: * "Jeongkwon Kim" wrote in message news:903rp4$svi$1@news-int.gatech.edu... } Hi! } I am doing CE/MS in analyzing peptide sequences. Recently I have seen a } peak, 61.5Da higher peak along with its original peak. I know if it is } 22Da higher, then it is from Na adduct and 38Da higher then it is from K } adduct. Theoretically it should be 60Da higher if it is Na+K adduct. Is } there anybody who has the same experience? Mr. Skoog answered: "Could it be a copper adduct?" I guess, it could be, if your Molecule is doubly charged and you se two peaks, since copper is 62.93 amu with an additional M+2 isotope peak with 44.6 % We often see these copper adducts with "small" (chelating) drug molecules with the above described isotope pattern characteristic for copper (TurboIonspray, positive, API 300, 365 or 3000). Best regards Dieter Zimmer ___________________ Dr. Dieter Zimmer Bayer AG Preclinical Pharmacokinetics PF 101709, Building 468 42096 Wuppertal Germany Phone: +49-202-36 4173 Fax: +49-202-36 4224 e-mail:Dieter.Zimmer.DZ@Bayer-Ag.de ****************************************************************************** From: sabine.bobin@libertysurf.fr Date: Tue, 02 Jan 2001 13:28:19 GMT Subject: mass spectra database Organization: Deja.com HELP I am searching web site with mass spectra database. We analyze drugs in plasma and urine samples. Sent via Deja.com http://www.deja.com/ ****************************************************************************** From: "CARRERA Francesc" Date: Tue, 02 Jan 2001 16:58:35 +0100 Subject: Re: N2 generators for lc/ms Organization: * To Gary A. Lombaert, We have a Whatman nitrogen generator (purchased to Agilent) that feeds two mass spectrometers. The compressed air is taken from an in-house net and it is produced by an oil-lubricated compressor followed by a filter system. The nitrogen generator is located inside the lab and the connections between the tap of the compressed air, the generator and mass specs are plastic tubes with Swagelok connectors. I am very satisfied with the system; it is absolutely quiet and it needs maintenance only once a year. The only con is that when the pressure of the compressed air fluctuates the pressure of outgoing nitrogen fluctuates in the same way. It hasn´t been a problem for me, however it would be solved by adding a reservoir between the generator and the MS. Francesc Carrera Mass Spectrometry System Manager Analysis R&D Department Research Center ALMIRALL PRODESFARMA S.A. Cardener 68-74 08024-Barcelona CATALONIA e-mail: fcarrera@almirallprodesfarma.com "Freedom consists in being able to choose the chains that tie you" ****************************************************************************** From: kmurray@kkm02.chem.emory.edu (K. Murray) Date: 2 Jan 2001 17:29:49 GMT Subject: Re: mass spectra database Organization: Emory University In article <92sll7$pkt$1@news-int.gatech.edu> sabine.bobin@libertysurf.fr writes: } HELP I am searching web site with mass spectra database. } We analyze drugs in plasma and urine samples. Try http://www.ualberta.ca/~gjones/mslib.htm Other databases at http://base-peak.wiley.com/links/Resources/Information_Sources_and_Archi ves/ -- Kermit Murray http://kkm02.chem.emory.edu/ ****************************************************************************** From: KCROCKET@ci.tacoma.wa.us Date: Tue, 2 Jan 2001 10:40:15 -0800 Subject: Re: ETP electron multipliers ? Organization: * Herbert, Concerning your interest in ETP multipliers: We use them in all 4 of our HP MSDs. I find them to be excellent in sensitivity and long life. We installed our first one June 6, 1997 and it's still going strong. They are quite simple to install, at least in the HP sytems. I'm sure they are probably just as easily installed in a Varian. ETP claims to have a shelf like of like forever. We will never go back to the old style multiplier. It is my understanding that SGE now owns, or at least distributes the ETP multipliers. Regards, Karen Crockett Senior Lab Analyst, Organics Environmental Services Science and Engineering City of Tacoma, WA. (253) 502-2132 kcrocket@ci.tacoma.wa.us ****************************************************************************** From: "Christopher R Lee" Date: Tue, 2 Jan 2001 21:17:21 +0100 Subject: Re: ETP electron multipliers ? Organization: Freesurf I installed one in a VG 70-70 (a long time ago), and also in a HP MS-engine. They last a long time, and have a major advantage over continuous dynode types: they die slowly and gracefully instead of suddenly giving the impression there's no ion beam. Regards a écrit dans le message news: 92t89v$1fe$1@news-int.gatech.edu... } Herbert, } } Concerning your interest in ETP multipliers: } } We use them in all 4 of our HP MSDs. I find them to be excellent in } sensitivity and long life. We installed our first one June 6, 1997 and it's } still going strong. } } They are quite simple to install, at least in the HP sytems. I'm sure they } are probably just } as easily installed in a Varian. } } ETP claims to have a shelf like of like forever. We will never go back to } the old style } multiplier. } } It is my understanding that SGE now owns, or at least distributes the ETP } multipliers. } } Regards, } } Karen Crockett } Senior Lab Analyst, Organics } Environmental Services } Science and Engineering } City of Tacoma, WA. } (253) 502-2132 } kcrocket@ci.tacoma.wa.us } } } ****************************************************************************** From: "Christopher R Lee" Date: Tue, 2 Jan 2001 21:31:13 +0100 Subject: Re: N2 generators for lc/ms Organization: Freesurf We tap into one of the site's 3 cubic m liquid nitrogen tanks, as there are several uses for the gas, including quite a few mass specs. As a precaution, and as most of the distribution network is beyond our control, I asked for a separate feed line to be tapped in just after the evaporator. Clean copper pipework should be OK, but they used stainless steel with high purity type fittings, just in case. I mention this because, unfortunately, the plumber used an anaerobic-curing sealant (Loktite) to glue the joints. Loktite bleeds volatiles that give the same ESI spectrum as you get from a methanol extract of a fragment of hardened sealant. A few pg/second doesn't amount to many grams per century. Moral: if your nitrogen seems dirty, have a look at the plumbing before blaming the purifier or reservoir! Regards a écrit dans le message news: 92fo2a$70c$1@news-int.gatech.edu... } } } We are considering the purchase of a membrane N2 generator to supply a proposed } lc/ms with 99.5% purity N2. I would like to hear from users of this technology } - are they satisfied, why or why not? I'm particularly interested in knowing } whether users have placed the generator in the lab or in a remote location. } Also, are oil-less air compressors necessary as an air supply, or can } oil-lubricated compressors be used in combination with the proper filtration? } Finally, what material of piping can / has been used between the compressor and } the generator , and between the generator and the lc/ms? } } Your views and experience are much appreciated, } ________________ } Gary A. Lombaert } Natural Toxins Specialist } Health Canada, Health Products and Food Branch } 510 Lagimodiere Blvd } Winnipeg, MB, CANADA R2J 3Y1 } Phone: (204) 984-2088 } Fax: (204) 983-5547 } } } } ****************************************************************************** From: Jens Ohnesorge Date: Wed, 03 Jan 2001 15:37:19 +0100 Subject: VG Trio-2000 Organization: TU Braunschweig, Germany Recently we aquired a VG Trio-2000 quadrupole mass spectometer with an ESI-ion source and MassLynx 1.6. Unfortunately we are unable to tune the RF-generator. Our second problem is to calibrate the instrument. It is impossible to keep the new calibration parameters stored in the computer. Does anybody know what to do ? Thank you very much for help Jens Ohnesorge ****************************************************************************** From: "M Sweeney - MSMS Consulting" Date: Wed, 03 Jan 2001 17:49:23 GMT Subject: Re: ID of glycoproteins by MALDI-TOF? ? Organization: EarthLink Inc. -- http://www.EarthLink.net Steve- If you don't know about the ABRF group you should. It is at http://www.abrf.org/ The has a nice searchable archive at http://www.abrf.org/archives/index.html This type of question is more in the domain of ABRF although this is a fine place to ask it as well. The archives might be searched for tips in this area. If you just need to ID the protein and don't care about coverage or post-translational mods...then don't bother to de-glycosylate. The proteolytic enzyme may not work as well but you should get at least enough hits to ID the puppy (x your fingers). It may be true in some cases that it works much better to de-glycosylate but as a shot-gun method leaving it glycosylated should work Matt Sweeney mattsweeney@earthlink.net Mass Spec Consulting Training/Operations/Consulting/Method Development LC/MS Pharmacokinetics, Peptides, Proteins, Metabolism, Maintenance Classes, Specialist in Finnigan Equipment and Software -----Original Message----- sroff@my-deja.com wrote: }Do we need to remove the carbohydrate chains }sometime before MALDI-TOF analysis? } Our main purpose is identification of the proteins }(antigens) rather than studying post-translational }modifications. }Thanks, }Steve ****************************************************************************** From: "M Sweeney - MSMS Consulting" Date: Wed, 03 Jan 2001 17:49:21 GMT Subject: Re: In Source Fragmentation versus MS/MS spectra Organization: EarthLink Inc. -- http://www.EarthLink.net James- Dr. Jonathan Josephs (JJ) worked with me at Finnigan...he did a paper on the use of API-CID in building a library of cough syrup components from pure stds. Then he ran a variety of commercial formulations and IDd the species. I think he published. If not he wrote it up as an Application note which is still in circulation at Finnigan. I saw it in the file cabinet in the literature area at Finnigan SJ last time I visited. Historically there has been the issue of differences in MS/MS spectra between different machines and CID gases. I think that this is a bit over-blown and in fact most things give a fairly unique spectra. Especially if you data-reduce the library entries to 20 peaks or so....either a fragment is present or it is not! I don't think peak height ratios are really that important in most cases of unknown ID. Take SEQUEST for example! Or Mascot! It should work. Getting the pure std spectra into the library is the most important thing. You might also have a method for generating synth std spectra...that way when you are working on a compound series whose behavior you understand you can create hypothetical spectra for species for which no analytical reference yet exists. That can help in metabolism also. If you are wrong then it may still come up as a good hit- although of a lower quality. The MW of the unk can REALLY help here. Matt Sweeney mattsweeney@earthlink.net Mass Spec Consulting Training/Operations/Consulting/Method Development LC/MS Pharmacokinetics, Peptides, Proteins, Metabolism, Maintenance Classes, Specialist in Finnigan Equipment and Software Little, James L wrote in message <92fqo2$7rs$1@news-int.gatech.edu>... } }I am interested in comparing "in-source" fragmentation to ion-trap and }triple quadrupole MS/MS spectra. Especially in using either "in-source" or }MS/MS to create databases for searching. I used Sci-Finder but didn't find }but one useful reference. Does anyone know of any literature references, }papers given at ASMS, personal experiences, etc. } }James L. Little }Bldg 150 }Eastman Chemical Company }Kingsport, TN 37662-5150 }Tel 423-229-8685 }FAX 423-229-4558 } }"A Little Mass Spectrometry and Sailing": }http://users.chartertn.net/slittle } } } } ****************************************************************************** From: "Rich Yelton" Date: Wed, 03 Jan 2001 17:59:46 GMT Subject: Re: VG Trio-2000 Organization: Excite@Home - The Leader in Broadband http://home.com/faster The inability to tune the RF could be indicative of a short between the rod(s) and ground, or possibly the rod(s) to each other. Remove the RF leads and use a VOM ( 20Meg range) to see if this is the source of the problem........... -- Richard O. Yelton Spectratek Mass Spectrometry Services Phone:859-341-6599 Fax: 859-341-6598 E-Mail: ryelton@massspecrepair.com Web: http://www.massspecrepair.com ****************************************************************************** From: Tobias Kind Date: Wed, 03 Jan 2001 23:18:00 +0100 Subject: Finding unknown substances Organization: UFZ - Leipzig Dear Colleagues, finding unknown "known" substances (identified by GC-MS) is sometimes horrible. In most cases customers of GC-MS services want a little background knowledge about the identified substance. Costs for 24h-online databases (CA,WOS,STN) can exceed the cost of a GC-MS device by a factor of 10. Again, all the following links may be well known, therefore --> to whom it may concern. I suppose you identified a substance manually or you have a proposal by NISTor Wiley databases. As an arbitrary example I take CAS: [205-43-6] - Benzo(b)naphtho(1,2-d)thiophene. You have to find retention data (boiling point), toxicity, and source and standards. (and you have no money) (1) ***** 49 hits (by toxline//SIS//NLM) http://chem.sis.nlm.nih.gov/chemidplus/ The people at toxline should win a prize for cleverness - they have dozens of CAS numbers. Especially many old chromatography abstracts (its an eldorado). Don't forget to check medline. And in the near future other clever people will link the whole databases to NIST an Wiley... :-) (2) ***** 0 usefull links (by chemfinder) http://www.chemfinder.camsoft.com/ Don't wonder - in this case Chemfinder found nothing - but this is the NUMBER ONE if you want to find anything about a substance. Ever wondered what "grass hopper ketone" is? Try it! Or find out all the features of chemfinder - using a substance like lindane. (people at chemfinder also should win a prize) They link to NIST Chemistry WebBook and ECR Physprop (and many many other databases). (3) ***** 3 hits (CAS), 19 hits name (by google) http://www.google.com Forget all other search engines, google is double sized (1,4E9 pages) and truly at time the biggest internet-engine. Use the cache function - even if the other side is offline, you can read the page, because google has a carbon copy! Remember, stemming (using wildcards *) is not allowed, and no phonetic search... (4) *** 10-14 hits (by Beilstein) http://www.chemweb.com/databases/beilstein This is the free Beilstein abstract service by chemweb (you can join for free). ... and if you are a lucky subscriber (sorry) (5) *** 4 hits (by sciencedirect) www.sciencedirect.com together with the (german based) document delivery service SUBITO I know that there are a lot more of services, databases, meta engines, full-text libraries, but I think that these are the most useful free services one can use without professional help. With kind regards Tobias Kind PS: If someone finds more (useful) hits with 4 other free services he/she will also win a price :-) ****************************************************************************** From: sroff@my-deja.com Date: Thu, 04 Jan 2001 03:06:26 GMT Subject: Re: ID of glycoproteins by MALDI-TOF? ? Organization: Deja.com Thanks for the help. I didn't know about the ABRF group. Steve In article <92vrhb$p6p$1@news-int.gatech.edu>, "M Sweeney - MSMS Consulting" wrote: } Steve- } If you don't know about the ABRF group you should. It is at } http://www.abrf.org/ The has a nice searchable archive at } http://www.abrf.org/archives/index.html This type of question is more in } the domain of ABRF although this is a fine place to ask it as well. The } archives might be searched for tips in this area. } } If you just need to ID the protein and don't care about coverage or } post-translational mods...then don't bother to de-glycosylate. The } proteolytic enzyme may not work as well but you should get at least enough } hits to ID the puppy (x your fingers). It may be true in some cases that } it works much better to de-glycosylate but as a shot-gun method leaving it } glycosylated should work } } Matt Sweeney } mattsweeney@earthlink.net } Mass Spec Consulting } Training/Operations/Consulting/Method Development } LC/MS Pharmacokinetics, Peptides, Proteins, Metabolism, } Maintenance Classes, Specialist in Finnigan Equipment and Software } } -----Original Message----- } sroff@my-deja.com wrote: } } }Do we need to remove the carbohydrate chains } }sometime before MALDI-TOF analysis? } } Our main purpose is identification of the proteins } }(antigens) rather than studying post-translational } }modifications. } }Thanks, } }Steve } } Sent via Deja.com http://www.deja.com/ ****************************************************************************** From: Steven C Pomerantz Date: Thu, 04 Jan 2001 15:35:26 -0700 Subject: Re: Any suggestion on TOF machines ? Organization: University of Utah "C.L. Chan" wrote: } Dear All, } } Our laboratory would like to aquire a TOF machine for analysis of } natural products and biopolymers (proteins and carbohydrates). Which } vendor could give TOF machine with promising dynamic range, } sensitivity, robustness and easy of use. } } Moreover, how about the pros and cons for the following machines in } natural products research ? } } - BIFLEX III from Bruker Daltonics } - Ominflex from PE } - Voyager-DE from PerSeptive Biosystems } } Thanks in advance ! } } C.L. Voyager - DE from PerSeptive Biosystems is the best. I have Voyager DE-STR for three years. I stiil have the femtomole sensitivity and very high resolution even at 5000 Da. You can stiil resolve isotopic peaks at 4 kDa with reflectron mode without any problem. Vajira Nanayakkara Manager/Mass Spec. Facility University of Utah 311A Skaggs Hall 30S 2000E Salt Lake City, UT 84112 ****************************************************************************** From: davidkovacs@my-deja.com Date: Thu, 04 Jan 2001 23:21:55 GMT Subject: HP 5971-2 MSD mass spectrometer glitch Organization: Deja.com Has anyone had a problem running sample sequences on their G1701 HP 5971 or 5972, related to an intermittent failure of the electron multiplier to start following the initial solvent delay off period? This failure results in termination of the sequence at the end of the sample run. If you've had this problem, you know how frustrating it can be. Ever since we switched (in late 1999) from the G1034 to the G1701 system on our 5971A, as part of a Y2K upgrade (purchased from Alpha Omega, Inc.), we have had this problem. Neither Agilent nor Alpha Omega have been able to suggest a fix that works, so far. We've tried all new mass spec. boards (including upgrade to the 5972 main board, new cable (HPIB), Smartcard II+ board, new computer and ChemStation software (from Windows 95 to Windows NT) and none of this has solved the problem. QUESTION: Does anyone out there use the "Enhanced" mode data analysis WITHOUT seeing this problem? QUESTION: Does anyone out there use (pay for) Agilent software (ChemStation) support? If so, do you recommend that we spend the money to have them think about this particular problem? Sent via Deja.com http://www.deja.com/ ****************************************************************************** From: kottenhahn@icdd.com Date: Fri, 05 Jan 2001 17:35:03 GMT Subject: ICDD® 2001 X-ray Clinics for 2001 Organization: Deja.com ICDD® 2001 X-ray Clinics The International Centre for Diffraction Data announces its X-ray clinic schedule for 2001. Fundamentals of X-ray Fluorescence Spectrometry, April 30-May 4, 2001 Advanced Methods in X-ray Fluorescence Spectrometry, May 7-11, 2001 Fundamentals of X-ray Powder Diffraction, June 4-8, 2001 Advanced Methods in X-ray Powder Diffraction, June 11-15, 2001 For information contact: Education Coordinator International Centre for Diffraction Data 12 Campus Boulevard, Newtown Square, PA 19073 Tel: (610) 325-9814 Fax: (610) 325-9823 E-mail: clinics@icdd.com Web-site: http://www.icdd.com/education/clinics.htm Web-site: www.dxcicdd.com Sent via Deja.com http://www.deja.com/ ****************************************************************************** From: "K. Verge" Date: Fri, 05 Jan 2001 10:54:33 -0800 Subject: Help with 'ghost peak' Organization: Simon Fraser University Hi all, Been banging my head against the wall for a while now on this one and thought I would ask for help. I'm running a teledyne 3DQ iontrap with either an in-house electrospray source or APCI source. I'm trying to do kinetic studies on in-trap species, which requires longish delay times. My 'ghost peak' is actually two peaks, located at m/z 371 and 391. These appear (via MS/MS) to be independant peaks. Basically, it looks like these species are acting as proton sinks in the system, skewing any quantitative process. I want to at least ID these species and then (hopefully) remove them. I've tried every contaminant source I can think of to no avail (new o-rings, new curtain gas, new buffer gas, new ES apparatus, new solvent sources, I've even baked the entire ion trap at high T for a weekend). All the evidence collected thus far points to an airborne contaminant, especially since I can generate the 'ghost peak' signal simply by creating a corona discharge at the sampling orifice (without any sample solution present). While I've done MS/MS experiments on the contaminants, they are extremely broad (6 m/z) peaks, very hard to isolate and fragment - the resulting spectra is tentative to say the least. Any ideas out there on possible culprits/further experiments to try or experience with this type of situation? Thanks in advance for your attention and help. ****************************************************************************** From: Reinhard Stroh Date: Fri, 05 Jan 2001 19:01:36 +0000 Subject: Re: N2 generators for lc/ms Organization: KPNQwest customer news service We use three Whatman Nitrogen Generators successfully since one year or so. They work well. We use a central compressor for all Nitrogen Generators (with oil, of course) and apply proper filtering: oil filter, fine - dust filter, de-watering (thawing point of 4-8 centigrade), fine-dust filter and carbon filter. We were told, that oil free compressors need more assistance than conventional ones. Indeed, we dont have any experience with oil free compressors. If you need further details, please dont hesitate to contact me via mail reinhard.stroh@NO SPAMeunet.at ****************************************************************************** From: kottenhahn@icdd.com Date: Fri, 05 Jan 2001 19:46:13 GMT Subject: The International Centre for Diffraction Data announces the Call for Papers for the 50th Annual Denver X-ray Conference. Organization: Deja.com 50th Annual Denver X-ray Conference Celebration! The International Centre for Diffraction Data announces the Call for Papers for the 50th Annual Denver X-ray Conference. 50th Annual Denver X-ray Conference July 30-August 3, 2001 Sheraton Steamboat Resort, Steamboat Springs, Colorado, U.S.A. Call For Papers; deadline March 16, 2001. For information contact: Conference Coordinator International Centre for Diffraction Data 12 Campus Boulevard, Newtown Square, PA 19073 Tel: (610) 325-9814 Fax: (610) 325-9823 E-mail: dxc@icdd.com Web-site: www.dxcicdd.com Sent via Deja.com http://www.deja.com/ ****************************************************************************** From: "James Duckworth" Date: Fri, 5 Jan 2001 15:44:15 -0500 Subject: Re: mass spectra database Organization: Galactic Industries We've put a small database called "Spectra Online" on our company web site (http://www.galactic.com/spconline). It actualily includes the AAFS database from U Alberta mentioned below and some other MS data as well as NMR, IR and other spectroscopic techniques. If you are looking for newer drugs, you may find them here despite the small size of the database. The AAFS collection contains a large number of spectra of drugs and their metabolites. -- James Duckworth Galactic Industries Corp. 395 Main Street Salem, NH 03079 USA Tel: 603-898-7600 Fax: 603-898-6228 jhd@galactic.com http://www.galactic.com "K. Murray" wrote in message news:92t40k$2n$1@news-int.gatech.edu... } In article <92sll7$pkt$1@news-int.gatech.edu> } sabine.bobin@libertysurf.fr writes: } } } HELP I am searching web site with mass spectra database. } } We analyze drugs in plasma and urine samples. } } Try http://www.ualberta.ca/~gjones/mslib.htm } } Other databases at } http://base-peak.wiley.com/links/Resources/Information_Sources_and_Archi } ves/ } } -- } Kermit Murray } http://kkm02.chem.emory.edu/ } } ****************************************************************************** From: Drew Gibson Date: Fri, 5 Jan 2001 21:53:53 +0000 Subject: Re: Help with 'ghost peak' Organization: is sadly lacking In an article about "Help with 'ghost peak'", K. Verge wrote... Hi there, The m/z 391 peak is likely to be M+H for DOP - dioctyl phthalate (actually di-2-ethylhexylphthalate, if memory serves). Its a plasticizer and we see it regularly in our analyses also. Try to minimize all contact with plastics / rubbers during sample preparation - gloves, pasteur pipette teats, almost anything can give rise to this contaminant. If plastic contact is inevitable, try and give a rinse with your solvent prior to sample contact. It could also be in your HPLC - change all solvents and give the system a thorough rinse with clean solvent. Don't forget that your column might also be contaminated - rinse it or dump it. Give the source a thorough clean - again, beware of the gloves that you use. In the past, I have put my nitrile (or whatever) gloves on and then thoroughly washed my hands with them on - has worked for me. I'm not sure what the m/z 371 peak is - do you have an MS/MS spectrum of it ? There is a book that lists common analytical contaminants, but I'm afraid I cannot remember the author or publisher at the moment. I have access to one at my work library, so if no-one else comes up with a possibility, I'll have a look then if I get the chance ! Do you have any MS data on it ??? }Hi all, } }Been banging my head against the wall for a while now on this one and }thought I would ask for help. I'm running a teledyne 3DQ iontrap with }either an in-house electrospray source or APCI source. I'm trying to do }kinetic studies on in-trap species, which requires longish delay times. }My 'ghost peak' is actually two peaks, located at m/z 371 and 391. }These appear (via MS/MS) to be independant peaks. Basically, it looks }like these species are acting as proton sinks in the system, skewing any }quantitative process. } }I want to at least ID these species and then (hopefully) remove them. }I've tried every contaminant source I can think of to no avail (new }o-rings, new curtain gas, new buffer gas, new ES apparatus, new solvent }sources, I've even baked the entire ion trap at high T for a weekend). }All the evidence collected thus far points to an airborne contaminant, }especially since I can generate the 'ghost peak' signal simply by }creating a corona discharge at the sampling orifice (without any sample }solution present). } }While I've done MS/MS experiments on the contaminants, they are }extremely broad (6 m/z) peaks, very hard to isolate and fragment - the }resulting spectra is tentative to say the least. } }Any ideas out there on possible culprits/further experiments to try or }experience with this type of situation? } }Thanks in advance for your attention and help. } } } -- Cheers, >>> mailto:drew@thegibsons.demon.co.uk <<< }}} ICQ 392790 IRC Gibby <<< Drew ;^) >>> http://www.thegibsons.demon.co.uk <<< ****************************************************************************** From: cody@jeol.com (Chip Cody) Subject: Re: Help with 'ghost peak' Date: Fri, 5 Jan 2001 22:24:21 GMT Organization: JEOL USA, Inc. If this is positive-ion mode, I would be highly suspicious that the 391 peak is [M+H+ from the plasticizer bis(ethylhexylphthalate). Chip Cody JEOL USA, Inc. In <9356gk$osk$1@news-int.gatech.edu> "K. Verge" writes: }Hi all, }Been banging my head against the wall for a while now on this one and }thought I would ask for help. I'm running a teledyne 3DQ iontrap with }either an in-house electrospray source or APCI source. I'm trying to do }kinetic studies on in-trap species, which requires longish delay times. }My 'ghost peak' is actually two peaks, located at m/z 371 and 391. ...rest of posting omitted -- "For purposes of ... New Jersey Right to Know Act. Contents partially unknown." |____________ |_ Robert B. Cody, Ph.D |________________________________ Product Development Manager |__ Mass Spectrometry |________________________ JEOL USA, Inc. |_ http://www.jeol.com |__________ e-mail: cody@nojunkmail.jeol.com |_ (REMOVE 'nojunkmail' TO REPLY) ==============[ Do not send me spam or advertising via e-mail !! ========= ****************************************************************************** From: "K. Verge" Date: Fri, 05 Jan 2001 15:00:27 -0800 Subject: Re: Help with 'ghost peak' Organization: Simon Fraser University Drew Gibson wrote: } In an article about "Help with 'ghost peak'", K. Verge } wrote... } } Hi there, } } The m/z 391 peak is likely to be M+H for DOP - dioctyl phthalate } (actually di-2-ethylhexylphthalate, if memory serves). Its a } plasticizer and we see it regularly in our analyses also. Try to } minimize all contact with plastics / rubbers during sample preparation - } gloves, pasteur pipette teats, almost anything can give rise to this } contaminant. If plastic contact is inevitable, try and give a rinse } with your solvent prior to sample contact. It could also be in your } HPLC - change all solvents and give the system a thorough rinse with } clean solvent. Don't forget that your column might also be contaminated } - rinse it or dump it. Give the source a thorough clean - again, beware } of the gloves that you use. In the past, I have put my nitrile (or } whatever) gloves on and then thoroughly washed my hands with them on - } has worked for me. } } I'm not sure what the m/z 371 peak is - do you have an MS/MS spectrum of } it ? There is a book that lists common analytical contaminants, but I'm } afraid I cannot remember the author or publisher at the moment. I have } access to one at my work library, so if no-one else comes up with a } possibility, I'll have a look then if I get the chance ! Do you have } any MS data on it ??? } -- } Cheers, >>> mailto:drew@thegibsons.demon.co.uk <<< } }}} ICQ 392790 IRC Gibby <<< } Drew ;^) >>> http://www.thegibsons.demon.co.uk <<< Drew, Thanks for the speedy reply - I didn't want to mention DOP in the original post, would've been even longer. My problem with it being DOP is that I'm almost positive it's airborne. I've gone so far as to construct an entirely plastic-free apparatus and sprayed a simple solution of purified NaCl in spectro-grade MeOH directly into the trap (No HPLC) - the peak still appears (as to the other ghost, a similar likely candidate is the analogous diethylhexyl adipate). As well, if i simply hook up a bare needle to high voltage (~5kV) and position in front of the sampling orifice (atmospheric pressure) to create a discharge (proton source), I still detect it - this in the absence of any sample whatsoever - I *should* get a normal discharge spectrum with various water/nitrogen/oxygen clusters, shouldn't I? Given DOP's extremely low vapour pressure (only 1.32mm Hg @ 200C in lit) and high b.p. (386.9C), it seems unlikely that it would be airborne in any meaningful concentrations. However, your post provides another confirmation of my fears, so I think further attempts at system purification may be required. As a footnote, I bought standard DOP from sigma and have not been able to generate much of a signal during electrospray, even under acidic (or heavily sodiated) conditions - any advice there? Thanks again, enjoy your weekend. Kent Verge Dept. of Chemistry Simon Fraser University *************************************************************** Some see a half-empty glass, some half-full I say I need another beer. ****************************************************************************** From: "rockFish" Date: Fri, 05 Jan 2001 22:20:36 -0800 Subject: Re: HP 5971-2 MSD mass spectrometer glitch Organization: Aracnet Internet In article <9334sk$4go$1@news-int.gatech.edu>, davidkovacs@my-deja.com wrote: } Has anyone had a problem running sample sequences on their G1701 HP } 5971 or 5972, related to an intermittent failure of the electron } multiplier to start following the initial solvent delay off period? This } failure results in termination of the sequence at the end of the sample } run. If you've had this problem, you know how frustrating it can be. It sounds to me like it might be a loose filament connection - right where the two-line twisted filament cable is plugged into the mainboard (close to the CI/EI toggle switch). The four 5971-72's that I've worked on all had the same thing happen at one time or another, and showed exactly the same failure. It only showed up after the solvent delay, because that's when the filament got power. You can check for the loose connection by gently moving the wires around while scanning. The fix was to pinch the female connector ends for a better contact. Rich ****************************************************************************** From: Markus Piotrowski Date: Sat, 06 Jan 2001 14:17:37 +0100 Subject: Re: N2 generators for lc/ms Organization: Ruhr-Universitaet Bochum, Rechenzentrum Dear Gary, you may also asked your LC/MS-supplier for his recommendations. We ordered our nitrogen supply (compressor and generator) together with our MS (QTOF2) from Micromass. Our first LC-MS, a TSQ-7000, was served with nitrogen from a big liquid nitrogen tank, but it lasts (in our case) some days to get a new one if it runs empty. For our QTOF2 we therefore ordered (via Micromass) a Nitrox UHPLCMS18 from Domnick Hunter. It makes 18l/min but needs an additional compressor (we have a JunAir 2000-40M). They also sell a smaller one, UHPLCMS12, which makes 12l/min (which is enough to make APCI with one mass-spec and more than enough for ESI) and has a built-in compressor. Both components (compressor and generator) needs maintainance every 3 to 6 months. We made the connections (MS-generator-compressor) with plastic tubings (maybe it's teflon, I'm not sure about this yet) and Swagelok connetors (both was delivered with the MS and the generator). The sound... The nitrogen generator itsels makes nearly no noise, but the compressor is the problem. We now have both MS in one room and the rotary pumps (if possible) and the nitrogen generator and the compressor in a second room, and I really appreciate this solution. The MSs are loud enough (especially the QTOF which has a built-in rotary pump) and I would recommed anyone asking, to get rid of any additional source of sound. Markus ****************************************************************************** From: "rockFish" Date: Sat, 06 Jan 2001 11:41:57 -0800 Subject: Re: HP 5971-2 MSD mass spectrometer glitch Organization: Aracnet Internet In article <9378ua$7d1$1@news-int.gatech.edu>, "rockFish" wrote: } It sounds to me like it might be a loose filament connection - right } where the two-line twisted filament cable is plugged into the mainboard } (close to the CI/EI toggle switch). Just to clarify. I meant the connection location was on the *analyzer board*. Not to the mainboard for the MS. It's the same two-line plug that's disconnected whenever the analyzer is lifted out. Rich ****************************************************************************** From: "chris.lee" Date: Sun, 7 Jan 2001 19:06:02 +0100 Subject: Re: Help with 'ghost peak' Organization: Infonie See my reply to N2 generators for lc/ms (2nd January). I don't remember the masses (it was a few years ago), but the problem was due to Loktite pipe sealant in the plumbing of the nitrogen supply. I didn't find the cause myself - I was given the information by a supplier (reseller) of gas purifiers (Spin, Paris region), who thereby lost a sale! Regards "K. Verge" a écrit dans le message news: 9378t6$79j$1@news-int.gatech.edu... } } } Drew Gibson wrote: } } } In an article about "Help with 'ghost peak'", K. Verge } } wrote... } } } } Hi there, } } } } The m/z 391 peak is likely to be M+H for DOP - dioctyl phthalate } } (actually di-2-ethylhexylphthalate, if memory serves). Its a } } plasticizer and we see it regularly in our analyses also. Try to } } minimize all contact with plastics / rubbers during sample preparation - } } gloves, pasteur pipette teats, almost anything can give rise to this } } contaminant. If plastic contact is inevitable, try and give a rinse } } with your solvent prior to sample contact. It could also be in your } } HPLC - change all solvents and give the system a thorough rinse with } } clean solvent. Don't forget that your column might also be contaminated } } - rinse it or dump it. Give the source a thorough clean - again, beware } } of the gloves that you use. In the past, I have put my nitrile (or } } whatever) gloves on and then thoroughly washed my hands with them on - } } has worked for me. } } } } I'm not sure what the m/z 371 peak is - do you have an MS/MS spectrum of } } it ? There is a book that lists common analytical contaminants, but I'm } } afraid I cannot remember the author or publisher at the moment. I have } } access to one at my work library, so if no-one else comes up with a } } possibility, I'll have a look then if I get the chance ! Do you have } } any MS data on it ??? } } -- } } Cheers, >>> mailto:drew@thegibsons.demon.co.uk <<< } } }}} ICQ 392790 IRC Gibby <<< } } Drew ;^) >>> http://www.thegibsons.demon.co.uk <<< } } Drew, } } Thanks for the speedy reply - I didn't want to mention DOP in the original } post, would've been even longer. My problem with it being DOP is that I'm } almost positive it's airborne. I've gone so far as to construct an entirely } plastic-free apparatus and sprayed a simple solution of purified NaCl in } spectro-grade MeOH directly into the trap (No HPLC) - the peak still appears } (as to the other ghost, a similar likely candidate is the analogous } diethylhexyl adipate). As well, if i simply hook up a bare needle to high } voltage (~5kV) and position in front of the sampling orifice (atmospheric } pressure) to create a discharge (proton source), I still detect it - this in } the absence of any sample whatsoever - I *should* get a normal discharge } spectrum with various water/nitrogen/oxygen clusters, shouldn't I? } } Given DOP's extremely low vapour pressure (only 1.32mm Hg @ 200C in lit) and } high b.p. (386.9C), it seems unlikely that it would be airborne in any } meaningful concentrations. However, your post provides another confirmation } of my fears, so I think further attempts at system purification may be } required. As a footnote, I bought standard DOP from sigma and have not been } able to generate much of a signal during electrospray, even under acidic (or } heavily sodiated) conditions - any advice there? } } Thanks again, enjoy your weekend. } } Kent Verge } Dept. of Chemistry } Simon Fraser University } } *************************************************************** } Some see a half-empty glass, some half-full } I say I need another beer. } } } ****************************************************************************** From: "A.P. Bruins" Date: Mon, 8 Jan 2001 10:53:49 +0100 Subject: Re: Help with 'ghost peak' Organization: * "K. Verge" wrote: }Hi all, } }Been banging my head against the wall for a while now on this one and }thought I would ask for help. I'm running a teledyne 3DQ iontrap with }either an in-house electrospray source or APCI source. I'm trying to do }kinetic studies on in-trap species, which requires longish delay times. }My 'ghost peak' is actually two peaks, located at m/z 371 and 391. }These appear (via MS/MS) to be independant peaks. Basically, it looks }like these species are acting as proton sinks in the system, skewing any }quantitative process. } }I want to at least ID these species and then (hopefully) remove them. }I've tried every contaminant source I can think of to no avail (new }o-rings, new curtain gas, new buffer gas, new ES apparatus, new solvent }sources, I've even baked the entire ion trap at high T for a weekend). }All the evidence collected thus far points to an airborne contaminant, }especially since I can generate the 'ghost peak' signal simply by }creating a corona discharge at the sampling orifice (without any sample }solution present). } }While I've done MS/MS experiments on the contaminants, they are }extremely broad (6 m/z) peaks, very hard to isolate and fragment - the }resulting spectra is tentative to say the least. } }Any ideas out there on possible culprits/further experiments to try or }experience with this type of situation? } }Thanks in advance for your attention and help. Answer: These are MH+ of dioctyl adipate and dioctyl phthalate. Check your gas lines and also your room (floor cover etc) for sources of emissions of these plasticizers. Andries Bruins Dr. A.P. Bruins University of Groningen Centre for Pharmacy Mass Spectrometry Facility A. Deusinglaan 1 9713 AV Groningen tel +31-50-3633262 fax +31-50-3638347 a.p.bruins@farm.rug.nl ****************************************************************************** From: Drew Gibson Date: Mon, 8 Jan 2001 18:40:59 +0000 Subject: Re: Help with 'ghost peak' Organization: is sadly lacking Chip Cody wrote: } } If this is positive-ion mode, I would be highly suspicious that the } 391 peak is [M+H+ from the plasticizer bis(ethylhexylphthalate). } Any reason why ? We routinely see MH+ 391 in our +ve electrospray analyses, and the MSMS spectrum of it is typical of a phthalate (m/z 149) and the spectrum obtained is consistent with the structure (not proof I know, but...). As far as the other post about airborne contamination is concerned, we have had problems in our lab in the past with other components (not DOP). One particularly troublesome episode was with a compound which turned out to be dodecamethylcyclohexasiloxane (MH+ 445) - commonly called cyclomethicone (and dimethicone I think) which turned out to be coming from our air conditioning systems - possibly after a service where the engineer used something during the service which leached this stuff out. -- Cheers, >>> mailto:drew@thegibsons.demon.co.uk <<< }}} ICQ 392790 IRC Gibby <<< Drew ;^) >>> http://www.thegibsons.demon.co.uk <<< ****************************************************************************** From: Drew Gibson Date: Mon, 8 Jan 2001 18:42:08 +0000 Subject: Re: Help with 'ghost peak' Organization: is sadly lacking The book I was thinking of below, is... Analytical Artifacts Journal of Chromatography Library Vol 44 Elsevier 1989 Author B.S. Middleditch. If I get the chance I'll go and have a look for m/z 371. I wrote: } I'm not sure what the m/z 371 peak is - do you have an MS/MS spectrum of } it ? There is a book that lists common analytical contaminants, but I'm } afraid I cannot remember the author or publisher at the moment. I have } access to one at my work library, so if no-one else comes up with a } possibility, I'll have a look then if I get the chance ! Do you have } any MS data on it ??? -- Cheers, >>> mailto:drew@thegibsons.demon.co.uk <<< }}} ICQ 392790 IRC Gibby <<< Drew ;^) >>> http://www.thegibsons.demon.co.uk <<< ****************************************************************************** From: Daniel Boismenu Date: Mon, 08 Jan 2001 20:20:34 GMT Subject: Re: Help with 'ghost peak' Organization: McGill University Mass Spectrometry Unit Greetings, There is a good chance that your 371 m/z peak is siloxane of formula C10H31O5Si5 and your 391 m/z peak is phthalate of formula C24H38O4. What you should do is to look at your MS/MS spectra and look for the following product ions. In the case of the phthalate, you should have the following ions: 57, 71, 113, 149, 167, 261 and 278. Check if you have used chloroform to to prepare samples lately. It is well known that chloroform is contaminated with phthalates. In the case of the siloxane found at 371, you should have the following ions: 73, 267 and 354. Concerning the siloxanes, examine carefully your scan spectrum, you might have several different molecules from three different series. For example, lets say that the first ion of one of the series would have the formula C4H13OSi2 (134 m/z), you might find the first ion of the oxydated serie with the formula C4H13O2Si2 (134 m/z + 16 = 150 m/z ). You might also another series which would correspond to the first series minus a methylene with the formula C3H11OSi2 (134 m/z - 14 = 120 m/z). For all series, the next ion will be 74 m/z higher, up to 355, 371 and 341, then depending of your contamination, you could get even higher masses. Siloxane contamination is coming from using silicon based materials: Silicon grease, silicon oil or even disposable plastic syringes (the plunger of such syringe is lubricated with silicon grease). Best Regards, Daniel Boismenu, Ph.D. Assistant Director McGill University Mass Spectrometry Unit "K. Verge" wrote: } Hi all, } } Been banging my head against the wall for a while now on this one and } thought I would ask for help. I'm running a teledyne 3DQ iontrap with } either an in-house electrospray source or APCI source. I'm trying to do } kinetic studies on in-trap species, which requires longish delay times. } My 'ghost peak' is actually two peaks, located at m/z 371 and 391. } These appear (via MS/MS) to be independant peaks. Basically, it looks } like these species are acting as proton sinks in the system, skewing any } quantitative process. } } I want to at least ID these species and then (hopefully) remove them. } I've tried every contaminant source I can think of to no avail (new } o-rings, new curtain gas, new buffer gas, new ES apparatus, new solvent } sources, I've even baked the entire ion trap at high T for a weekend). } All the evidence collected thus far points to an airborne contaminant, } especially since I can generate the 'ghost peak' signal simply by } creating a corona discharge at the sampling orifice (without any sample } solution present). } } While I've done MS/MS experiments on the contaminants, they are } extremely broad (6 m/z) peaks, very hard to isolate and fragment - the } resulting spectra is tentative to say the least. } } Any ideas out there on possible culprits/further experiments to try or } experience with this type of situation? } } Thanks in advance for your attention and help. ****************************************************************************** From: Giovanna.Tripepi@bruker.it (Giovanna Tripepi) Date: Tue, 9 Jan 2001 14:57:25 +0100 Subject: Re: Any suggestions on TOF machines ? Organization: * Dear Steven, The FLEX series of MALDI-TOF mass spectrometers of Bruker Daltonics Inc. offers a full range of performance from the REFLEX III with the ultimate performance and flexibility, to the research grade high-throughput BIFLEX III, the new and innovative automated high-throughput autoflexT and finishing with high performance and easy to use walk up bench-top OmniFLEX. NOTE: OmniFlex is a Bruker product, not a PE one. As far as technical specs and applications notes of our machines, please visit our web-sites: http://www.daltonics.bruker.com http://www.bruker-daltonik.de/ and feel free to call our local representative who'll be willing to give you comparative tables between ours and competitors instrumentation. Best regards, Giovanna T. Dr.ssa Giovanna Tripepi Bruker Daltonics S.r.l. Via Pascoli 70/3 I-20133 Milano ITALY Voice: +39-02-7063-6370 Fax: +39-02-2361-294 Email: giovanna.tripepi@bdal.it web: www.bruker.it Steven C Pomerantz wrote: } "C.L. Chan" wrote: } } Dear All, } } } } Our laboratory would like to aquire a TOF machine for analysis of } } natural products and biopolymers (proteins and carbohydrates). } } Which vendor could give TOF machine with promising dynamic range, } } sensitivity, robustness and easy of use. } } } } Moreover, how about the pros and cons for the following machines in } } natural products research ? } } } } - BIFLEX III from Bruker Daltonics } } - Ominflex from PE } } - Voyager-DE from PerSeptive Biosystems } } } } Thanks in advance ! } } } } C.L. } } Voyager - DE from PerSeptive Biosystems is the best. I have Voyager } DE-STR for three years. I stiil have the femtomole sensitivity and = very } high resolution even at 5000 Da. You can stiil resolve isotopic peaks = at } 4 kDa with reflectron mode without any problem. } Vajira Nanayakkara } Manager/Mass Spec. Facility } University of Utah } 311A Skaggs Hall } 30S 2000E } Salt Lake City, UT 84112 } ****************************************************************************** From: Joel Eary Date: Tue, 09 Jan 2001 14:59:01 -0500 Subject: PE Sciex "Analyst" Software Organization: Millennium Pharmaceuticals, Inc. I have four years experience developing lc-ms/ms methods for the detection of novel pharmaceutical compounds. The majority of my experience has been with Micromass' software package (Masslynx/Metabolynx). I have just begun a new job where I will be utilizing PE Sciex's (Applied Biosystems) Analyst software using both an API2000 and an API3000. Does anyone have experience with the day to day use of this software? If so, what are your opinions? What flaws have been the most aggravating? Thank you, Joel Eary ****************************************************************************** From: "Aaron M. Kitchen" Date: Wed, 10 Jan 2001 03:26:27 GMT Subject: silanizing glass injector inlets Organization: Excite@Home - The Leader in Broadband http://home.com/faster What is the process for silanization of injector inlet glassware inside of injector sleeves. We currently use split inlets and buy new ones although we would like to start cleaning our own. Thanks. Aaron ****************************************************************************** From: "gary_bauer" Date: Tue, 9 Jan 2001 19:32:06 -0800 Subject: Alan Marshall at January BAMS meeting Organization: * Please follow the link to www.bams.org to make your reservation. "Scaling Mass Spectrometric Plateaus: A Celebration of Nature's Isotopic Complexity" Alan Marshall, Florida State University Abstract : Most mass analysis relies on "nominal" mass accuracy (i.e., to within 1 Da). However, an increasing number of applications are based on much more accurate mass measurement. The Figure shows that mass spectrometric resolution (defined here as the spacing between resolved peaks) does not increase monotonically with increasing spectrometer resolving power for electrosprayed biomolecules. Rather, resolution improves by a series of steps. First, one must resolve different charge states. No additional peaks appear until adducts are resolved, then not again until isotopic peaks are resolved (unit mass resolution), and finally when isotopic "fine structure" (i.e., different elemental compositions of same nominal mass) is resolved. High mass resolving power (m/{delta}m50% > 50,000 over a wide mass range) offers two major advantages. First, it becomes possible to separate complex mixtures without prior chromatographic or gel separation. Second, elemental composition may be determined from accurate (to ~1 ppm) mass measurement alone for unknown molecules up to ~300 Da (or to ~ 1000 Da if isotopically enriched molecules are available. Examples from environmental, petrochemical, analytical, and biological problems will be presented, including some new world records for mass resolution. Acknowledgments. Work supported by NSF (CHE-99-09502), NIH (GM-31683), Florida State University, and the National High Magnetic Field Lab in Tallahassee, Florida. Biography: Alan Marshall was born in Ohio, and grew up in San Diego. He received his B.A. from Northwestern University and Ph.D. from Stanford University under John Baldeschwieler. He joined the faculty of the University of British Columbia in 1969, moving to The Ohio State University in 1980 and to Florida State University in 1993. Alan is currently Kasha Professor of Chemistry at FSU and directs the Ion Cyclotron Resonance Program at the National High Magnetic Field Laboratory in Tallahassee. Prof. Marshall's research concentrates on development of new techniques and applications of Fourier transform ion cyclotron resonance mass spectrometry, a technique for which he is co-inventor. Alan has produced 3 books, 3 patents, and 310 refereed journal papers and has presented ~875 talks/posters at institutions and conferences. He edits or is an editorial board member of six journals. He is a Fellow of AAAS and Fellow of the American Physical Society, and has received two American Chemical Society national awards, the Spectroscopy Society of Pittsburgh Maurice F. Hasler Award, and awards from the American and International mass spectrometry societies. Thanks to Julie Leary for sharing her NSF-sponsored, internationally acclaimed mass spec speakers with BAMS. ****************************************************************************** From: "Matthew Clabaugh" Date: Wed, 10 Jan 2001 09:23:41 -0600 Subject: NCI of the TraceMS Organization: * Hello All, I am a Field Marketing Specialist for ThermoFinnigan and I was forwarded you messages by a colleague. I have been doing extensive work with the new TraceMS (the next step since the MD800) in Neg CI. The new digital (I will see if it can be retrofitted to a MD800) makes the sensitivity, stability and resistance to contamination unmatchable. The Projects I have been working with are large derivitized molecules and the sensitivity is 100 to 1000 times better than anything I have seen before. I would be happy to talk with you via e-mail or live at the number listed below. I look forward to speaking with all of you. Matthew Clabaugh Field Marketing Specialist 512-251-1585 ****************************************************************************** From: "David Sparkman" Date: Thu, 11 Jan 2001 05:35:14 -0800 Subject: Re: silanizing glass injector inlets Organization: CompuServe Interactive Services Aaron, The procedure is detailed in Jack Watson's "Introdcution to Mass Spectrometry", 3rd ed. It is also in earlier editions of his book. The 3rd ed was published in 1997. You can get this book at http://www.LCMS.com. Regards; David O. David Sparkman ods@compuserve.com -- O. David Sparkman Consultant-At-Large ods@compuserve.com "Aaron M. Kitchen" wrote in message news:93hnk0$la1$1@news-int.gatech.edu... } What is the process for silanization of injector inlet glassware inside } of injector sleeves. We currently use split inlets and buy new ones } although we would like to start cleaning our own. Thanks. } } Aaron } } ****************************************************************************** From: Tobias Kind Date: Thu, 11 Jan 2001 17:56:21 +0100 Subject: Re: silanizing glass injector inlets (+++ bargain) Organization: UFZ - Leipzig Dear Mr. Kitchen, } What is the process for silanization of injector inlet glassware inside } of injector sleeves. We currently use split inlets and buy new ones } although we would like to start cleaning our own. Thanks. Answer: (c)Alltech All untreated glass surfaces contain –OH or silanol groups. These groups interact with most compounds that are injected into your GC. The interaction usually takes the form of tailing peaks (reversible adsorption) or irreversible adsorption of the compound, both of which make quantitation difficult. However, you have several options to counteract this problem. You can either buy deactivated liners or deactivate the liners yourself. To deactivate the liner, you must first prepare it for silylation. Rinse the new liner with your sample solvent to remove any manufacturing residues that might interfere with this process. The liner must then be dehydrated. Silylation reagents preferentially react with small polar compounds such as water, alcohols, and amines, so these compounds must be removed before beginning the silylation process. To dehydrate the liner place it in an oven and heat it at 180°C for 1 hour. Cool the oven to approximately 50°C and immediately place the liner in a 5% solution of dimethyldichlorosilane (DMDCS) preferably in toluene, but methylene chloride and pentane will also work. Place a piece of laboratory stretch film such as Saran Wrap™ or Dura Seal™ over the reaction vessel. Soak the liner in the 5% DMDCS solution for 10 minutes. Use caution when removing the liner from the reaction vessel because anhydrous hydrochloric acid is formed during this reaction as demonstrated by Figure 1. Due to their volatile and flammable nature, silylating reagents (and their solvents in some cases) should be kept away from open flames and sources of heat and should be handled only in a hood. The liner should be rinsed with the same solvent used in the DMDCS solution and then soaked in methanol for 10 minutes. Once again cover the reaction vessel with laboratory stretch film. This step takes the reaction to completion and Residual reagent, if left on the liner, will often mimic column bleed which could require several hours to stabilize. The liner should then be removed from the methanol and allowed to air dry. Once dry, the liner is thoroughly deactivated and ready for use. Do not store opened solutions or leave covered for long periods of time. Alltech has created a new deactivation kit specifically designed for deactivating injection port liners. The kit comes with 4 x10mL ampules of 5% dimethyl- dichlorosilane (DMDCS) solution, a pair of tweezers for easy liner handling, four test tubes which act as the reaction vessel, and detailed instructions. This kit includes enough DMDCS to deactivate four injection port liners. This is was taken from Alltech catalog: “Specialists in Chromatography” Deactivation Kit 18107 $33.00 http://www.alltechweb.com/literature/brochure/363p7.pdf or http://www.alltechweb.com/searchmain.asp (search for DMDCS - use Adobe Acrobat reader for reading PDF files) With kind regards Tobias Kind PS: OK - here comes the bargain basement: Additionally to my previous post: Finding unknown substances (stuff,junk,everything) I add another useful service: The "Search Adobe PDF Online" In most cases you can instantly read "PDF-files" and you will find exclusive documents which are not covered by other search services! http://searchpdf.adobe.com/ Enter: silylation liner dmdcs If the links contain no usefull information - try "more like this document" (...theres a gap - I walked manually to alltechweb...) PPS: Sorry - J. Throck Watson :-) ****************************************************************************** From: "Antony Williams" Date: Fri, 12 Jan 2001 12:00:53 -0500 Subject: Re: New NIST Library Search with Structural Search Added Organization: * "Little, James L " wrote >NIST is introducing Version 2.0 their of library search program. It has >a "Windows Standard" interface plus many new capabilities. The most >exciting new capability in my opinion is the ability to search commercial >and user libraries by structure! See some of the screen shots of the >interface on my Web site: "A Little Mass Spectrometry and Sailing": >http://users.chartertn.net/slittle >We are successfully using this software as our standard method for >searching our corporate EI, NIST, Wiley, MS/MS datatbases, Eastman Plant >Material, and TSCA databases. >My web site includes a user's manual for using the NIST software with >commercial drawing programs and other manufacturers' data processing >software. The page also includes information on accuate mass, unusual >doubly charged ions, CI manifolds, useful CI mixtures, diazomethane >artifacts, silylation artifacts, etc. > >James L. Little >Bldg 150 >Eastman Chemical Company >Kingsport, TN 37662-5150 >Tel 423-229-8685 >FAX 423-229-4558 > Just for information, please note that the NIST database has been available in a structure searchable format for almost two years. http://www.acdlabs.com/products/spec_lab/exp_spectra/spec_libraries/nist_ms. html The database plugs in directly to MS Manager (description below)and we also make free databases available from our Free Stuff page at our website. The package includes the structure drawing package ACD/Chemsketch which has over 85,000 users. ACD/MS Processor processes MS and LC-MS data with features such as import/export of JCAMP, HP, Xcalibur, Finnigan LCQ, Sciex, Millennium and ASCII data files; peak picking; and fragment assignment. Automatically designate molecular ions and known fragments. Display/print customized TIC, RI, delta and annotation tables. Component detection analysis (CODA) compares adjacent mass spectra to eliminate spurious signals from LC-MS dataset. Isotope pattern calculator predicts peak shape. Auto-assignment option compares the spectrum with that predicted for the attached chemical structure. Additional DB available: NIST DB (107,000 entries).The database capability of ACD/SpecDB gives high-level organization to spectra, data, structures and related files in a single package. You can buy databases, build your own, and download some for free from www.acdlabs.com . A Database Forms Manager standardizes and speeds up data input with your own customized input form containing pop-up menus, default values and mandatory fields. A Spectrum Parameters Field allows read-only access to spectrum conditions, details of analysis, etc. In SpecDB any database can be searched according to structure, structure fragment, spectrum, sub-spectrum, molecular formula, formula weight, spectrum parameter, and user-defined data values, text strings, etc. Multiple databases can be searched sequentially. User Notes section has customizable font. View DB in Virtual Plates or 96 Well modes. SQL product also available. PLEASE NOTE MY NEW CELL PHONE NUMBER BELOW ************************************* Dr. Antony Williams, B.Sc. Ph.D, Advanced Chemistry Development, US Office, The Settlement, 225 Jamestown Road, Pittsboro, NC-27312 Office 919-928-9035 Cellular 919-201-1516 Efax 425-790-3749 Email tony@acdlabs.com Head office 416-368-3435 Support 416-368-3435 Support support@acdlabs.com ************************************* ____________________________________________ ACD/MS Manager 4.5 is now released. Import experimental LC-MS or GC-MS data or a single mass spectrum, attach a chemical structure and generate a table of associated molecular fragments. Tools for manipulation and annotation of spectra prior to building searchable spectral databases are available. New features include COmponent Detection Algorithm (CODA), accurate mass support, Auto Assignment and macro capabilities. For more info please visit: http://www.acdlabs.com/products/spec_lab/exp_spectra/ms/ ___________________________________________ ****************************************************************************** From: Ken Matuszak Date: Fri, 12 Jan 2001 16:06:30 -0600 Subject: Help needed with TurboIonspray source Organization: Abbott Labs Pharmaceutical Products Division Hi: I am operating a Sciex Pulsar (qqTof). Up until now, I have been using the normal Ionspray and Heated Nebulizer sources with great success. However, I have been working on an LC/MS method which requires flow rates (500 uL/min with a gradient from 100% aqueous to 100% organic) greater than the normal Ionspray source can handle. In my initial attempts at setting up a borrowed turboionspray, it appears that my sensitivity is significantly less (orders of magnitude) than with either the heated nebulizer or the standard ionspray sources. Is this normal? If not, it is totally possible that I am not even close to the correct parameters for this source. The manuals I have are pretty vague on generic params for this source.. Can anyone suggest some standard source parameters for this flow rate? In addition, the source I borrowed (two years old and barely used), had a fused silica line, between where the tubing from the LC should hook up, and running all the way through and into the spray probe. My manuals, vaguely indicate that a PEEK connection can be made between the LC inlet and the spray probe inlet. I removed the long fused silica line and replaced it with a short piece of PEEK tubing between the two connectors. Does anyone know if this is OK, or possibly I have an older model turboionspray source which requires the fused silica? Sincerely, Ken Matuszak Abbott Laboratories ****************************************************************************** From: "Justin Withers" Date: Fri, 12 Jan 2001 18:30:32 -0800 Subject: Re: PE Sciex "Analyst" Software Organization: Posted via Supernews, http://www.supernews.com Joel, We would be happy to help you in any way we can to transition into your new job with the new software and instruments. Please refer to our web site at appliedbiosystems.com for tech support options and training calendars and feel free to contact me as you progress with Analyst, Regards, Justin Withers Software Marketing, Applied Biosystems | MDS Sciex, witherjm@appliedbiosystems.com "Joel Eary" wrote in message news:93fr2h$lfq$1@news-int.gatech.edu... } I have four years experience developing lc-ms/ms methods for the } detection of novel pharmaceutical compounds. The majority of my } experience has been with Micromass' software package } (Masslynx/Metabolynx). I have just begun a new job where I will be } utilizing PE Sciex's (Applied Biosystems) Analyst software using both an } API2000 and an API3000. Does anyone have experience with the day to day } use of this software? If so, what are your opinions? What flaws have } been the most aggravating? } } Thank you, } Joel Eary } } } ****************************************************************************** From: calvin_li@my-deja.com Date: Sat, 13 Jan 2001 12:08:52 GMT Subject: Any suggestion for LC/MS/MS traps ? Organization: Deja.com I Would like to seek your expert advice on the selection of new, affortable bench-top LC/MS/MS systems with APCI and ESI source. Especially, I am looking for comment / experience sharing on the systems with Ion Traps, for use in the detection/identification of drugs/metabolites from urine samples, e.g. : a. Agilent 1100 MSD Trap b. Finnigan LCQ DECA Any other suggestions of comparable capacity will be appreciated. Sent via Deja.com http://www.deja.com/ ****************************************************************************** From: rglab Date: Sun, 14 Jan 2001 19:32:50 +0100 Subject: Re: PE Sciex "Analyst" Software Organization: tp.internet - http://www.tpi.pl } "Joel Eary" wrote in message } news:93fr2h$lfq$1@news-int.gatech.edu... } } I have four years experience developing lc-ms/ms methods for the } } detection of novel pharmaceutical compounds. The majority of my } } experience has been with Micromass' software package } } (Masslynx/Metabolynx). I have just begun a new job where I will be } } utilizing PE Sciex's (Applied Biosystems) Analyst software using both an } } API2000 and an API3000. Does anyone have experience with the day to day } } use of this software? If so, what are your opinions? What flaws have } } been the most aggravating? We are using API200 with Analyst working on WindowsNT. We are in a process of developing a software for neonatal screening. Analyst provides an ActiveX/COM interface that can be used from external applications (Visual Basic mostly). There is access for all Analyst features - although the documentation is not as good as it should be. There are also some bugs since WinNT version is not widely tested as MacIntosh version. Regards, Ryszard ****************************************************************************** From: "Scott MacDonald" Date: Mon, 15 Jan 2001 09:59:24 -0500 Subject: Free ACD Spectroscopic Databases Organization: * Advanced Chemistry Development has made a number of spectroscopic databases available free of charge from our website at: These are freely available for all users of our SpecManager modules which allow processing and data management for NMR, 2D NMR, MS, LC- and GC-MS, IR (all flavors), Raman and UV-Vis. All databases are fully searchable by structure, sub-structure, spectrum and subspectrum as well as text. For MS Manager (Mass Spectrometry) users visit: http://www.acdlabs.com/download/db/ms.html . For UVIR Manager (IR, Raman and UV-Vis) users visit: http://www.acdlabs.com/download/db/uv_ir.html For NMR Manager users visit: http://www.acdlabs.com/download/db/nmr.html Continue to visit..we will be updating the pages with new DBs shortly.. Best wishes, Scott MacDonald _______________________ Scott MacDonald Account Manager Advanced Chemistry Development, Inc. 90 Adelaide St. W., Suite 702, Toronto, Ontario, Canada M5H 3V9 Tel: (416) 368-3435 x229 Fax: (416) 368-5596 Toll: 1-800-304-3988 x229 email: mailto:scott@acdlabs.com URL: www.acdlabs.com _______________________ Time is running out for the ACD Scholar of the Year Contest -- you and your university can qualify for prizes! www.acdlabs.com/educators/scholar.html "James Duckworth" wrote: >We've put a small database called "Spectra Online" on our company web >site (http://www.galactic.com/spconline). It actually includes the AAFS >database from U Alberta mentioned below and some other MS data as well as >NMR, IR and other spectroscopic techniques. If you are looking for newer >drugs, you may find them here despite the small size of the >database. The AAFS collection contains a large number of spectra of >drugs and their metabolites. > >-- >James Duckworth >Galactic Industries Corp. >395 Main Street >Salem, NH 03079 >USA > >Tel: 603-898-7600 >Fax: 603-898-6228 >jhd@galactic.com >http://www.galactic.com > >"K. Murray" wrote in message >news:92t40k$2n$1@news-int.gatech.edu... >} In article <92sll7$pkt$1@news-int.gatech.edu> >} sabine.bobin@libertysurf.fr writes: >} >} } HELP I am searching web site with mass spectra database. >} } We analyze drugs in plasma and urine samples. >} >} Try http://www.ualberta.ca/~gjones/mslib.htm >} >} Other databases at >} >}http://base-peak.wiley.com/links/Resources/Information_Sources_and_Archives/ >} >} -- >} Kermit Murray >} http://kkm02.chem.emory.edu/ >} >} ****************************************************************************** From: joerg.hau@rdls.nestle.com Date: Mon, 15 Jan 2001 17:46:08 +0100 Subject: S: ESI source for TSQ700 Organization: * Dear All, Our laboratory would like to acquire an Electrospray Source for our second Finnigan TSQ700 instrument. Preferably an "ESI-2" source with the wide-bore heated transfer capillary (the one that was introduced in 1998 or so), with the line-of-sight sprayer head. If somebody has such a complete source with the related electronics etc. for sale, please drop me a mail. Thanks, -- Joerg ---------------------------------------------------------------------- Joerg Hau NESTLE Research Center, Lausanne, Switzerland joerg.hau@rdls.nestle.com "All standard disclaimers apply." ---------------------------------------------------------------------- Never take life seriously. Nobody gets out alive anyway. ---------------------------------------------------------------------- ****************************************************************************** From: Nicki Hughes Subject: Multi-experiment acquisition Date: Mon, 15 Jan 2001 12:38:30 -0500 Organization: * Hi. I need help processing data from a multi-experiment acquisition (Loop) I am acquiring data looping 2 experiments (ion polarity switch). After data acquisition I can spilt the 2 sets of data in Multiview but cannot process using Macquan. I keep getting the message "......contains more then one experiment per period, Macquan cannot handle it". Can anyone help me? Nicki ****************************************************************************** From: "Peter Frank" Date: Mon, 15 Jan 2001 14:52:12 -0500 Subject: Free ACD/ChemSketch Tools for Mass Spectrometrists Organization: UUNET Canada News Reader Service Advanced Chemistry Development's ChemSketch software, coupled with the ChemBasic programming language "Goodies" can provide some powerful tools for the Mass Spectrometrists. ChemSketch helps you develop theories about likely cleavages or rearrangements in a mass spectrometer by generating structure drawings of cation and radical-cation fragments. With our free ChemBasic program, you can obtain monoisotopic masses accurate to the fourth decimal place for the drawn structures. These mass values can now be compared with your high-resolution experimental spectra to guide your interpretation. As an added benefit, you will have publication-quality structure drawings that can be attached to your presentations, spectra, and articles. The full application note is available at: http://www.acdlabs.com/appnotes/ms/mschemsk.html Regards, Peter Frank M.Sc. Customer Support Specialist Advanced Chemistry Development, Inc. 90 Adelaide St. West, Suite 702 Toronto, ON Canada M5H 3V9 Phone: 416-368-3435 x243 Fax: 416-368-5596 URL: http://www.acdlabs.com/ ****************************************************************************** From: "C.L. Chan" Date: Tue, 16 Jan 2001 11:42:29 +0800 Subject: Low energy CID of Na or K adduct Organization: Hong Kong Baptist University Dear ALL, I need help to get a meaningful MS/MS spectrum in low energy CID of Na or potassium adduct of ginsenosides on a Triple-Q. Is there any advice on the low energy CID of Na or potassium adduct of ginsenosides since no meaningful product ion spectrum could be obtained except the alkali metal ions. Should high energy CID be employed for such adducts of ginsenosides ? Thanks in advance ! C.L. ****************************************************************************** From: Derek Bradley Date: Tue, 16 Jan 2001 10:59:40 +0000 Subject: Bruker MALDI Tof Data Processing Software Organization: * Hi Guys, Further to a previous post we have decided it's time to bite the bullet and upgrade our data processing software. As a quick resume, we are currently running a Bruker Biflex III MALDI MS on Bruker's 'Data Analysis for Tof 1.5j' PC software having eschewed our installed version of XMASS 5.0 as it runs at less than snails pace and is prone to crashing. However 'Data Analysis for Tof' is less than perfect being very unwieldy, relentlessly unreliable and similarly susceptible to taking a dive at crucial moments. Having spoken to Bruker about this they have suggested that we look into their XMASS for PCs and/or Bioworks(?) software as no upgrades/patches exist for our current software. Having seen what Bruker can do with a UNIX based system I am naturally wary when it comes to their Windows based software, my question is this: Does anyone have any experiences with these two programs that would be useful to me or be able to suggest any viable alternatives? Thanks very much. Derek Bradley Dept. of Medicine UCL London ****************************************************************************** From: rehaufler@my-deja.com Date: Tue, 16 Jan 2001 14:33:42 GMT Subject: Re: Help needed with TurboIonspray source Organization: Deja.com In article <93nvoh$o96$1@news-int.gatech.edu>, Ken Matuszak wrote: } Hi: } } I am operating a Sciex Pulsar (qqTof). Up until now, I have been using } the normal Ionspray and Heated Nebulizer sources with great success. } However, I have been working on an LC/MS method which requires flow } rates (500 uL/min with a gradient from 100% aqueous to 100% organic) } greater than the normal Ionspray source can handle. } } In my initial attempts at setting up a borrowed turboionspray, it } appears that my sensitivity is significantly less (orders of magnitude) } than with either the heated nebulizer or the standard ionspray sources. } Is this normal? If not, it is totally possible that I am not even close } to the correct parameters for this source. The manuals I have are } pretty vague on generic params for this source.. } } Can anyone suggest some standard source parameters for this flow rate? } } In addition, the source I borrowed (two years old and barely used), had } a fused silica line, between where the tubing from the LC should hook } up, and running all the way through and into the spray probe. My } manuals, vaguely indicate that a PEEK connection can be made between the } LC inlet and the spray probe inlet. I removed the long fused silica } line and replaced it with a short piece of PEEK tubing between the two } connectors. Does anyone know if this is OK, or possibly I have an older } model turboionspray source which requires the fused silica? } } Sincerely, } } Ken Matuszak } Abbott Laboratories } The way that we use the TIS ion source is to run a single piece of 0.005" PEEK from the machined union, through the ion source, and into the union to which the sprayer tip is connected. I cannot see how the partial PEEK partial silica connection is better than that. Plus it is really easy to completely replumb the ion source. Problems with using the TIS ion source include clogging of the flow pathway, which will show up as back pressure on your system, spitting, which can be caused by leaky air connections, poor tip condition, too high temperature, turbo-gas blowing hot gas on the sprayer tip leading to boiling in the tip. I would recommend replacing the silica with PEEK tubing, the PEEK tubing, and sprayer tip on an ion source the condition of which is unknown. Operations parameters that need to be optimized include spray trajector (do not spray at the orifice), sprayer position, nebulizer gas, temperature, and turbo gas flow. E-mail me if you have questions robert.haufler@richmond.ppdi.com Sent via Deja.com http://www.deja.com/ ****************************************************************************** From: "Justin Withers" Date: Wed, 17 Jan 2001 06:14:15 -0800 Subject: Re: Multi-experiment acquisition Organization: Posted via Supernews, http://www.supernews.com Yes, MacQuan was designed in an age when we the user did not do the things we do now. More precisely for the API-III, which could not do pos-neg switching. Therefore the short answer to your question is that MacQuan will never be able to process that type of data. For that reason a while ago we made TurboQuan and more recently we released a whole new acquisition and processing package called Analyst. All instruments since the API-III can use this in it's entireity and it will handle your data and a great deal more. For more info. please see www.appliedbiosystems.com or contact us at our tech. support no. 800 831 6844 or at support@sciex.com or via our web site's FAQ page or directly, Regards, Justin Withers Applied Biosystems | MDS Sciex witherjm@appliedbiosystems.com "Nicki Hughes" wrote in message news:93vqq9$gij$1@news-int.gatech.edu... } Hi. } } } I need help processing data from a multi-experiment acquisition (Loop) } } I am acquiring data looping 2 experiments (ion polarity switch). After } data acquisition I can spilt the 2 sets of data in Multiview but cannot } process using Macquan. I keep getting the message "......contains more } then one experiment per period, Macquan cannot handle it". } } Can anyone help me? } } } Nicki } } } } ****************************************************************************** From: "Jason Ellis" Date: Wed, 17 Jan 2001 07:51:04 -0800 Subject: Re: silanizing glass injector inlets Organization: Agilent Technologies Hello Aaron, You can find a basic description of liner deactivation on our web site at: http://www.jandw.com/GCReference/injectors-ref.htm I hope that this helps. Please let me know if you have any questions about the procedure. Jason Ellis Technical Support Agilent Technologies jason_ellis@agilent.com Aaron M. Kitchen wrote in message <93hnk0$la1$1@news-int.gatech.edu>... }What is the process for silanization of injector inlet glassware inside }of injector sleeves. We currently use split inlets and buy new ones }although we would like to start cleaning our own. Thanks. } }Aaron } } ****************************************************************************** From: "James L. Loo" Date: Wed, 17 Jan 2001 10:56:40 -0700 Subject: For Sale VG70E-HF Mass Spectrometer Organization: * The University of California at Santa Cruz, Chemistry Department has available for sale: VG70E-HF MASS SPECTROMETER *Refurbished July, 1996 by GB SCIENTIFIC, 701 DeLong Ave, Novato, CA 94945 (415) 898-7606 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ NOTE: We are also willing to sell individual parts and/or components in lieu of parting with an intact instrument: Available are: All Digital and Analog components, Power Supplies, FAB Probe, EI probe, (2) EI/CI Sources, FAB Source, PDB 11/73, Winchester Drive, Printronix Printer, etc, etc. ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Instrument includes: 1) EI/CI, FAB capabilities 2) VG 11/250J data system comprising DEC 11/73 computer, VG acquisition interface and digital scan controller, Printonix Printer. 3) HX-150 water chiller This medium performance mass spectrometer has a perfomance range at 6kV of 1-2000 amu. It has EI/CI/FAB Sources, Peak Matching as well a Mass Measuement capability into the Data System. The Mass Resolution is continuously variable up to 10,000 (10% valley) Please make inquires to Mary Howe, UCSC, (831)459-3692, howe@chemistry.ucsc.edu or James Loo, (831) 459-2485, loo@chemistry.ucsc.edu We will consider any reasonable offer. Thanks ================================================================== As Zeus said to Narcissus, "Watch Yourself." loo@chemistry.ucsc.edu http://www.nmr.ucsc.edu (831) 459-2485 Office (831) 459-4923 Lab (831) 459-2935 FAX ============================================================================== : ================================================================== As Zeus said to Narcissus, "Watch Yourself." loo@chemistry.ucsc.edu http://www.nmr.ucsc.edu (831) 459-2485 Office (831) 459-4923 Lab (831) 459-2935 FAX ============================================================================== ****************************************************************************** From: "Dave Russel" Subject: Sequest and Mascot software systems Date: Thu, 18 Jan 2001 08:04:25 -0000 Organization: * Dear all, I have some experience in LC-MS but I am just starting with peptide analysis and proteomics. I am aware of two software systems i.e. "Sequest" and "Mascot" on the market. Is there anyone who could explain me the similarities and differences (pro's and con's) of both systems. Or maybe I overlooked other software packages wortwhile considering? Thank you very much in advance, best regards Dave e-mail: DaveRussel@hotmail.com _________________________________________________________________________ Get Your Private, Free E-mail from MSN Hotmail at http://www.hotmail.com. ****************************************************************************** From: "O. A. Mamer" Date: Thu, 18 Jan 2001 13:47:49 GMT Subject: Re: silanizing glass injector inlets Organization: * Dear Aaron: We chemically clean liners by soaking them for a minute or two in hot dilute hydrofluoric acid (2 ml conc HF (CAUTION!!), 50 ml very hot tapwater in a small plastic beaker, and then rinsing in cold water) after removal of surface dirt and glass wool. This provides for a very clean hydrophillic surface for silanization, otherwise one only has a very imperfectly silanized surface. Orval A. Mamer, PhD, Director, The Mass Spectrometry Unit, and Professor of Medicine, McGill University 1130 Pine Ave West Montreal Que Canada H3A 1A3 Tel 514 398-3661 Fax: 514 398-2488 Email: omamer@po-box.mcgill.ca ****************************************************************************** From: "Stephen Eyles" Date: Fri, 19 Jan 2001 09:38:45 -0500 Subject: Re-crystallization of DHB? Organization: University of Massachusetts, Amherst I have some old 2,5-DHBA which is very yellow. Does anyone know the best solvent for re-crystallization? Cheers, Steve ****************************************************************************** From: "Michael Sherrell" Date: Fri, 19 Jan 2001 08:19:20 -0800 Subject: Q-TOF, mass specs, MALDIs for sale Organization: * LC/Mass specs and MALDIs for sale: LC/MS & MS/MS: Micromass Q-TOF: $305,000. ~1 yr. old; was $457,000 new. Sciex API 365: $97,500. Installed w/ 90-day warranty Sciex API 300: $55,000. Installed w/ 30-day warranty Sciex API III+: $48,000. Triple quad: ES, APCI; +$15K/intall w/ 90-day warr. Micromass Platform: call. 2 yrs. old; Waters 2690. hplc included Finnigan Navigator: $55,000. Install & 90-day warr. included Finnigan TSQ 7000: $125,000. EI/CI, APCI; 1995 model w/ API-2 upgrade Finnigan SSQ 7000: $55,000. ES, APCI; ISIS data system; API 1 source; install included Finnigan TSQ 700: $60,000. 1993; API 1, electrospray, APCI, DCI; new Alpha workstn (Y2K-ok); includes factory install + factory 90-day warranty Fisons VG Platform: Offer. to 3000 daltons; under service contract AMD 604 S: $150,000. Double-focusing mag sector; very low detection limits, <4ppm mass, ESI/EI and FD sources. Install/service available. Offers condered. MAT 95: $260,000. Hi res mag sector. 1994, ES, APCI, FAB, Thermospray, GC interface, install, delivery, 1 yr warr. Finnigan MAT 90: $15,000. Hi-resolution magnetic sector Waters Integrity: $60,000. Current EI instrument; includes autosampler, pump, PDA, Millenium 32, install, 90-day warranty. Kratos Concept: $20,000. 4-sector; LSIMS, EI, FD; 10,000. mass range. VG70E-HF: $20,000. Hi-res mag sector; EI/CI, FAB. Recent refurb. Xtrell 400 ELQ. Make offer. LC/MS/MS, GC/MS/MS; 10. yrs. old, floor model, well-maintained Fisons VG 2000. <$100,000 Fisons VG Trio: $25,000. LC + GC: 3000. amu; thermospray, EI/CI, HP 5890 included. Install, license & 90-day warr. +: $14,500 HP 5989: $30,000. Electrospray; 2000. amu. +$20,000/HP 1090. w/ ternery pump, autosampler, DAD, install and 90-day warr. Nermag R10. 10c <$10,000. Like new; make offer VG Quattro Bio-Q: $2,000. For parts Service and service contracts available for PESciex API 3000, 365 and III+. MALDI-TOFs: Voyager DE RP: $99,000. <4 yrs. old; very little use; under service contract now. Voyager Elite: $50,000. Asking price. 5 yrs. old. Navigator: Call for price. 1998; virtually unused. Thermosep HPLC, robotic liquid handling, current software. Voyager LBT2: $40,000. ~1993. Excellent condition. Non-DE. Voyager/Vestek: $25,000. Non-DE, non-RP. LaserMAT 2000: $24,000. New detector & laser; +$2,000/install; service available HP G2025A: $60,000 ICP-MS: VG PQ3: $99,500. Asking price. 3 yrs. old. GC/MS/MS: Finnigan GCQ: $35,000. 4 yrs. old; well-maintained; install/svc contract avail. Other mass specs, NMRs, DNA/protein sequencers & synthesizers available; check the website. Michael Sherrell Grizzly Analytical (USA) 707 887 2919/fax 707 887 9834 www.grizzlyanalytical.com ****************************************************************************** From: "Karl J. Treier" Date: Fri, 19 Jan 2001 15:47:57 -0500 Subject: Wanted. Finnigan ITD700/800 GCMS Organization: OneNet Communications News Hub If anyone is disposing of a ITD700/800 GCMS I would be interested in procuring one. It does not need to pull vacuum or produce ions anymore but the PCBA's must be functional and it must include the PC interface card. Karl ktreier@fuse.net ****************************************************************************** From: calvin_li@my-deja.com Date: Sat, 20 Jan 2001 03:53:56 GMT Subject: Parent ion scan possible by Traps MS/MS ? Organization: Deja.com I was told it may be possible to do precursor ion scan using Ion Traps, just like a Triple Q does. Any practical advice on this naive qeury? Sent via Deja.com http://www.deja.com/ ****************************************************************************** From: Ernest Fung Date: Mon, 10 Apr 2000 15:21:48 GMT Subject: re: metabolic origin of... Organization: Calgary Regional Health Authority I have identified the presence of two compounds in human urine using GC/MS solvent extraction-TMS method: 3-hydroxy phenylpropionic acid or aka 3-(3-hydroxy phenyl)propionic acid; and 4-hydroxy phenylpropionic acid or aka 3-(4-hydroxy phenyl)propionic acid or aka p-OH-hydrocinnamic acid Can anyone enlighten me as to what are the metabolic precursors for these compounds? Are they from medications or natural diet? Many thanks... 2000/04/10 . ****************************************************************************** From: jr2893@my-Deja.com Date: 21 Jan 2001 16:07:44 GMT Subject: Re: Parent ion scan possible by Traps MS/MS ? Organization: CompuServe Interactive Services Hi, this is not possible in real time measurement. You have to collect a datafield in a defined mass range and make a normal daughter scan mass by mass. At the end of this procedure you are able to get an ion map as a data reprocessing and there you can get all data of parent scans and neutral loss data in this data field. As an result you are able to do this with stop flow techniques or loop injections. So if you have time enough to do this, then you have all options of data: normal scan, product ion scan, parent scan and neutral loss data of all posibilities and this is much more than you can get with an triple quad istrument. The bottleneck is time. with best regards On Sat, 20 Jan 2001 03:53:56, calvin_li@my-deja.com wrote: } I was told it may be possible to do precursor ion scan using Ion Traps, } just like a Triple Q does. } } Any practical advice on this naive qeury? } } } Sent via Deja.com } http://www.deja.com/ } } ****************************************************************************** From: gunter@elnhuk.de (Gunter Kuhnle) Date: 22 Jan 2001 09:00:23 GMT Subject: Survey on number and type of ms instruments used Organization: * Hallo, there are frequently mails or postings asking for information for a survey on MS instruments used. At the moment, I am looking for data like this (what sources, analysers etc are used). Could anyone help me, please? Gunter -- Gunter Kuhnle * http://www.elnhuk.de * ICQ: 70020937 ****************************************************************************** From: l.c.packman@bioc.cam.ac.uk (Len Packman) Date: Mon, 22 Jan 2001 09:13:23 +0000 Subject: Re: Parent ion scan possible by Traps MS/MS ? Organization: Cambridge University In article <94fdm9$kqi$1@news-int.gatech.edu>, jr2893@my-Deja.com wrote: } Hi, } this is not possible in real time measurement. You have to collect a } datafield in a defined mass range and make a normal daughter scan mass } by mass. At the end of this procedure you are able to get an ion map } as a data reprocessing and there you can get all data of parent scans } and neutral loss data in this data field. As an result you are able to } do this with stop flow techniques or loop injections. So if you have } time enough to do this, then you have all options of data: normal } scan, product ion scan, parent scan and neutral loss data of all } posibilities and this is much more than you can get with an triple } quad istrument. The bottleneck is time. } } with best regards } } } } } } } } On Sat, 20 Jan 2001 03:53:56, calvin_li@my-deja.com wrote: } } } I was told it may be possible to do precursor ion scan using Ion Traps, } } just like a Triple Q does. } } } } Any practical advice on this naive qeury? } } } } } } Sent via Deja.com } } http://www.deja.com/ } } } } Could you possibly elaborate on this methodology? Exactly how does one go about setting up such a run, say, to locate phosphopeptides in an lcms run? A how-to-do type reply would be incredibly useful to those of us unfamiliar with much more than standard triple plays. Thanks Len -- Dr Len C. Packman Department of Biochemistry, University of Cambridge 80 Tennis Court Road, Cambridge, CB2 1GA, UK l.c.packman@bioc.cam.ac.uk ****************************************************************************** From: Markus Piotrowski Date: Mon, 22 Jan 2001 14:56:01 +0100 Subject: Identification of ADP-ribosylated peptide by LC-MS/MS Organization: Ruhr-Universitaet Bochum, Rechenzentrum Hello, I want to identify the site of ADP-ribosylation in a certain protein by LC-MS/MS. We have got a Q-TOF2 MS. The amino acid to be ADP-ribosylated should be an arginine. I know the expected mass difference, and I'm also aware that the ribosylated arginine will not cleaved by trypsin. I'm looking for some hints which will help me to identify the ribosylated peptides. Is there anyone around having experience with identification of ADP-ribosylated peptides by LC-MS? Are there techniques to enrich the ribosylated peptide (like IMAC for phosphopeptides) or are there known neutral losses which can be used (like 98 for phosphoserine/phosphothreonine) to screen for the peptide? Possible ions for parent-ion-scanning? Is the ADP-ribose stable during fragmentation? I know this are a lot of questions but till know I was not successful in finding literature concerning this topic. Any help would be appreciated. Thanks Markus Markus Piotrowski Ruhr-Universitaet Bochum Dep. Plant Physiology, ND3 44801 Bochum Germany Markus.Piotrowski@ruhr-uni-bochum.de ****************************************************************************** From: Jens Ohnesorge Date: Mon, 22 Jan 2001 15:27:27 +0100 Subject: MassLynx1.3 Organization: TU Braunschweig, Germany Does anybody still work with MassLynx 1.3 or is experienced with this version? Jens Ohnesorge ****************************************************************************** From: Skoog Date: Tue, 23 Jan 2001 09:12:19 -0000 Subject: Indoleacrylic Acid MALDI Matrix Organization: University College London Hi All, I've been asked to do MALDI analysis on some phthalocyanine derivatives using indoleacrylic acid as the matrix. Never having used this matrix before is there anything I need to be aware of with it e.g. handling, sample prep., performance, disposal etc ? Comments welcome!! Thanks, Derek Bradley Dept. of Medicine UCL London ****************************************************************************** From: "M Sweeney - MSMS Consulting" Date: Tue, 23 Jan 2001 20:49:38 GMT Subject: Re: Any suggestion for LC/MS/MS traps ? Organization: EarthLink Inc. -- http://www.EarthLink.net DECA without a DOUBT! Compare the literature refs...# on LCQ vs. # on 1100 MSD! Ease of use and the Finnigan folks wrote the book in the trap area...take a look at the patents and the work of Cooks and March! Don't think twice. Just get a DECA. It is not to say that HP does not make some awesome equipment...I love the LCs. Matt Sweeney mattsweeney@earthlink.net Mass Spec Consulting Training/Operations/Consulting/Method Development LC/MS Pharmacokinetics, Peptides, Proteins, Metabolism, Maintenance Classes, Specialist in Finnigan Equipment and Software }a. Agilent 1100 MSD Trap } }b. Finnigan LCQ DECA } ****************************************************************************** From: "M Sweeney - MSMS Consulting" Date: Tue, 23 Jan 2001 20:35:29 GMT Subject: Re: Parent ion scan possible by Traps MS/MS ? Organization: EarthLink Inc. -- http://www.EarthLink.net Len- I'll bite on this one. Chris Turck at UCSF and I set up a method that generates data sets that can be mined this way. I put a poster up at the link below which is really a brief from of our ASMS 2000 poster(#820) in html format. If anyone wants more details, feel free to ask. I also made a figure of the entire data set in one figure (with captions). They are at the following links. The information is identical in them...but one has been fancied up to look like a marketing brochure;) poster @ http://home.earthlink.net/~mattsweeney/820.html entire data set figures (first is simple and second 'fancy') @ http://home.earthlink.net/~mattsweeney/zomwalk2.htm http://home.earthlink.net/~mattsweeney/zomwalk.htm Ok...here goes...sorry if it is not as to the point as some might like. I will not consider chromatography initially in this explanation (I'll bring it in later). You all have not had a real big post from me for awhile so here goes....heehee. 1) Infuse a sample (nanospray?). 2) Start at low mass (say 250) and get ms/ms on 250, then 251, then 252, then 253, up to the max say 2000. You don't want to do this manually!...I'll explain later how to automate it. You generate a file of containing all the ms/ms spectra that are possible from your sample in this manner. 3) Now you have about 1500 ms/ms scans in a data file (less if you use our technique). Now you can mine this with the data system. 4) To get the parent that give a neutral loss of say 18 you just go through each of the 1500 ms/ms scans and plot the intensity of the progeny ions occurring at 18 less than the ms/ms parent mass. So for ms/ms 250 you plot the intensity of the signal at 250-18=232, then take the ms/ms 251 scan and plot the signal at 233 (251-18), etc. Now when you plot it you don't put the intensity from ms/ms250's 232 actually at 232...you put it on your graph at 250. That is because you want to know 'who' looses 18 (250 in this case)...the point of a Neutral Loss scan. Thankfully this is all done using the mapping features of the latest Xcalibur release. You end up with a single "scan" or display which looks like a normal scan but is really a plot which shows how much -18 each of the parent masses loose. Similarly you do Parent scans. Except here you take each scan and look at say 76...then plot the intensity of m/z 76 in each ms/ms scan and put the intensity value at the ms/ms parent mass value...then you have a plot of how much 76 fragment comes from each parent mass. Again Xcalibur does all this for you using the mapping feature. ISSUES: A)giant data files-that's life. At least the data file has more ms/ms per unit time than usual. No bigger than lc/ms B)ion-suppression/salts due to co-elution in infusion lead to killing of signal for minor species lc/ms fixes this issue...but is more time/equipment intensive. The trap can still get good ms/ms on the faintest signals where the full/zoom-scan barely shows anything. Combined with the implicit parent mass value, dbase searching can still result in hits even from the faintest scrappy ms/ms spectra! Pretty cool. C)two species with different structures and the same m/z may give overlayed ms/ms spectra lc/ms fixes this as well D)multiply charged species contribute to this overlay in both parent and progeny spectra lc/ms E)time runs out on your 1ul nano-sprayed sample! time windows are perhaps even briefer with lc/ms! But spectra better! So how do we do it? 1)Chris and I do a moving window triple/double play where we set up an experiment method that looks at small (I think 50-75 amu) windows for defined periods of time. We split a 40 minute method up into say fifteen 100amu windows(segments) so 1500amu. might be covered. There are some limits on the # segments and so forth in the experiment method that this explanation may violate...but you'll get the drift...the precise details will reveal themselves as you build it. Part of the limit with static nanospray is the sample dwell time in the source. If it runs out before the end of the experiment you may miss big and/or important ions at masses you have not examined yet. Still it is quick, automated and has given good protein IDs from gel bands in our hands.We have gotten easily 10 hits on peptides from 25fmol of standards with clearly unambiguous identification using Sequest. Creating a single element FASTA library from the top hit and re-running Sequest against the data set results in even more 'hits'. Seg # time range m/z range for the full-scan ************************************* 1 0-3 minutes 250-325 2 3-6 minutes 326-400 3 6-9 minutes 401-475 etc. Each of these segments contains data-dependent triple play variants. Then we use dynamic exclusion which has a 25(+/-5) element limit. So the triple play variant (penta-play?) for segment 1 might be 1) full-scan ms 250-325 2) data-dep zoom on 1st largest from 1) 3) data-dep ms/ms on 1st largest from 1) 4) data-dep zoom on 2nd largest from 1) 5) data-dep zoom on 2nd largest from 1) The enabling of the dynamic exclusion means that once an ion gets selected for ms/ms it will not be again. Dynamic exclusion has a limit on the number of ions that are kept track of...that is why we had to use the multiple segments with different full-scan ranges. I'd love it to just keep a big list. Then we'd be able to just do a dynamic exclusion enabled data-dependent penta-play on 250-2000 and the LCQ would never hit the same ion twice. As it is after the list gets 25 or so elements, it rolls off the old (first/most intense) m/z values and replaces them with the 25th and so likely then hits the first one again. Then you'd have a data-file with numerous ms/ms duplications. So we were forced to use this solution. The experiment takes about 45 minutes to set-up...but once it is done you can use it for years. It also may be possible to tweak other parameters in the dynamic exclusion/data-dependent set-ups to improve all this (we constantly are!). This gives you the concept however...build from here! The idea of steps 4) and 5) is to not waste time on going back to the full-scans. The sample has a limited dwell in the source and we balance all these values to get through the whole mass range. Many of the parameters inter-play to change the rate the LCQ works through the sample...so use your own judgement. We also let the max inj/ u-scans on the ms/ms be quite large to get faint ions better. The full scan and zoom are short (and 1 u-scan) as we don't really use them for anything...they are used to drive the ms/ms ion selection is all! Then you save the experiment method and run it. I was describing this to someone and needed to give the instructions for getting the LCQ to start the exp. method when doing infusion...Bill Haddon at the USDA in Albany, CA gave me a nice clear instruction set from my hazy original set of instructions...so I'll quote him here. ************************************************************ *START Bill Haddon's instructions* ************************************************************ To run a sample on the LCQ using Syringe Pump Infusion and a Method File (triple play for ex) ************************************************************ Xcalibur ROADMAP SEQUENCE SETUP -- Actions -- Run this sample | run this sequence (Alt A s or Alt A h) RUN SEQUENCE box "Change Instruments" Button Remove LC and Autosampler Designate LCQ MS as Start Instrument ************************************************************ *END Bill Haddon's instructions* ************************************************************ While it is running I like to keep an eye on it to make sure it is still spraying OK. Then you mine the data set with the mapping feature of Xcalibur. +2/+1 ions have different neutral loss masses for phosphopeptides potentially- look for both of them. Now combined with the relative low abundance of phosphorylated forms vs un-modified forms and the potential of ion-suppression to mask minor species...this method is not so great potentially as a phosphorylation screening methodology! And you wasted all this time to read this????!!!!! LC/MS methods If you got this far...you should be realizing that the use of the dynamic exclusion feature combined with a data-dependent triple play should work even better with LC/MS...with out all the fancy 15 pt exp method to get around the dynamic exclusion list element limit. No ion-suppression! But to get back to the minor % that may be phosphorylated...you may miss them as they are too small and come and go with the lc peak width before you ever get to scan them! That is the issue with LC/MS. You may have only 1 minute to collect data on an LC peak! That is why some people do the peak parking where the lc is slowed down or stopped when a species elutes (or phosphorylated form enrichment). Just as you can mine a set of ms/ms from an infusion run, you can mine all the ms/ms from and lc/ms run using the ion-mapping feature of Xcalibur. I will leave it as an exercise for you to figure out your own best parameters for lc/ms dynamic exclusion/data-dependent using lc/ms. any questions??? Matt Sweeney mattsweeney@earthlink.net Mass Spec Consulting Training/Operations/Consulting/Method Development LC/MS Pharmacokinetics, Peptides, Proteins, Metabolism, Maintenance Classes, Specialist in Finnigan Equipment and Software }Could you possibly elaborate on this methodology? Exactly how does one go }about setting up such a run, say, to locate phosphopeptides in an lcms }run? A how-to-do type reply would be incredibly useful to those of us }unfamiliar with much more than standard triple plays. Thanks } }Len } }-- } }Dr Len C. Packman }Department of Biochemistry, University of Cambridge }80 Tennis Court Road, Cambridge, CB2 1GA, UK }l.c.packman@bioc.cam.ac.uk } } } } ****************************************************************************** From: "Georg Voelkle" Date: Wed, 24 Jan 2001 01:27:44 +0100 Subject: Re: Any suggestion for LC/MS/MS traps ? Organization: T-Online I must agree Matt, take a closer look at the DECA, it´s my favourite. George. schrieb im Newsbeitrag news:93prdo$8lj$1@news-int.gatech.edu... } I Would like to seek your expert advice on the } selection of new, affortable bench-top LC/MS/MS } systems with APCI and ESI source. } } Especially, I am looking for comment / experience } sharing on the systems with Ion Traps, for use in } the detection/identification of drugs/metabolites } from urine samples, e.g. : } } a. Agilent 1100 MSD Trap } } b. Finnigan LCQ DECA } } Any other suggestions of comparable capacity will } be appreciated. } } } } Sent via Deja.com } http://www.deja.com/ } } ****************************************************************************** From: calvin_li@my-deja.com Date: Wed, 24 Jan 2001 02:56:44 GMT Subject: Re: Parent ion scan possible by Traps MS/MS ? Organization: Deja.com Many thanks all who gave expert advice on my naive query. It sounds promising if the described procedures using a Trap could be fully automated for real-life identification works, just like a triple Q can (without LC), e.g.: a) Newborn screening for abnormal blood Amino Acids / Acylcarnitines based on parent ion / neutral loss scans. b) Toxicology screening for abused substances in urine. Any comment on the potential along this line...? Best regards, Calvin Li HKUST In article <94l85h$er5$1@news-int.gatech.edu>, "M Sweeney - MSMS Consulting" wrote: } Len- } } I'll bite on this one. Chris Turck at UCSF and I set up a method that } generates data sets that can be mined this way. I put a poster up at the } link below which is really a brief from of our ASMS 2000 poster(#820) in } html format. If anyone wants more details, feel free to ask. I also made a } figure of the entire data set in one figure (with captions). They are at the } following links. The information is identical in them...but one has been } fancied up to look like a marketing brochure;) } } poster @ http://home.earthlink.net/~mattsweeney/820.html } entire data set figures (first is simple and second 'fancy') @ } http://home.earthlink.net/~mattsweeney/zomwalk2.htm } http://home.earthlink.net/~mattsweeney/zomwalk.htm Sent via Deja.com http://www.deja.com/ ****************************************************************************** From: Heino Prinz Date: Wed, 24 Jan 2001 13:15:47 +0100 Subject: Re: Any suggestion for LC/MS/MS traps ? Organization: GWDG, Goettingen Am Tue, 23 Jan 2001 20:49:38 GMT schrieb "M Sweeney - MSMS Consulting" }DECA without a DOUBT! Compare the literature refs...# on LCQ vs. # on 1100 }MSD! Ease of use and the Finnigan folks wrote the book in the trap }area...take a look at the patents and the work of Cooks and March! Don't }think twice. Just get a DECA. It is not to say that HP does not make some }awesome equipment...I love the LCs. } Yes, and their open software concept allows you to run most LC Systems (such as Agilent HP1100) with the excalibur (Finnigan) software. Viele Gruesse Heino Prinz Tel.:(++49)-231-133-2480 Fax: (++49)-231-133-1038 ****************************************************************************** From: "Rick Flurer" Date: Wed, 24 Jan 2001 13:37:40 GMT Subject: Re: Low energy CID of Na or K adduct Organization: * try using lithium instead "C.L. Chan" wrote in message news:941he3$5m1$1@news-int.gatech.edu... } Dear ALL, } } I need help to get a meaningful MS/MS spectrum in low energy CID of Na } or potassium adduct of ginsenosides on a Triple-Q. Is there any advice } on the low energy CID of Na or potassium adduct of ginsenosides since no } meaningful product ion spectrum could be obtained except the alkali } metal ions. } } Should high energy CID be employed for such adducts of ginsenosides ? } } Thanks in advance ! } } C.L. } } } ****************************************************************************** From: "Servizio, Paul" Date: Wed, 24 Jan 2001 16:40:58 -0500 Subject: filament burnout Organization: * A forensic drug chemist wants to know if anyone is experiencing early filament burnout on their Agilent 5973 GC-MS. The solvent used is usually methanol. The rate of burnout is about 1 per month and a half. ****************************************************************************** From: "Rich Yelton" Date: Thu, 25 Jan 2001 03:53:35 GMT Subject: Re: Any suggestion for LC/MS/MS traps ? Organization: Excite@Home - The Leader in Broadband http://home.com/faster I would highly recommend the Agilent 1100 LC/MSD system including the Autosampler and Mass based fraction collector. This instrument is highly reliable, requires little day to day maintenance and is easily switched from ESI to APCI in a matter of seconds. It has a built in calibrant delivery system with pre mixed calibration mixtures for both APCI and ESI calibrations. ( No need to mix your own or gunk up the instrument with historic tuning solutions ). If you are into ID'ing drugs and metabolites in urine, sensitivity and specificity requirements should determine your choice. i.e. do you need High sensitivity since you may be sample limited or need to achieve extremely low levels of detection ? do you need MS/MS or will in source CID suffice? What is the price difference and is it justifiable based on the requirements of your investigation? I would also suggest sending an identical test sample to your prospective vendors in order for you to make some assessment of full spectrum quality and reporting capabilities... You also may want to look at other products and references for the Agilent 1100 LC/MSD at www.agilent.com/chem ****************************************************************************** From: "Rich Yelton" Date: Thu, 25 Jan 2001 03:53:35 GMT Subject: Re: filament burnout Organization: Excite@Home - The Leader in Broadband http://home.com/faster Make sure that a solvent delay of around 4 mins. is set in your method. The filament and multiplier must be OFF when the solvent front elutes to prevent premature filament failure and multiplier arcing. Best of Luck, -- Richard O. Yelton Spectratek Mass Spectrometry Services Phone:859-341-6599 Fax: 859-341-6598 E-Mail: ryelton@massspecrepair.com Web: http://www.massspecrepair.com ****************************************************************************** From: Jens Glastrup Date: Thu, 25 Jan 2001 12:48:15 +0100 Subject: Re: filament burnout Organization: The Danish National Museum Do you have an air leak somewhere in your system? ****************************************************************************** From: "M Sweeney - MSMS Consulting" Date: Thu, 25 Jan 2001 18:21:35 GMT Subject: Re: Parent ion scan possible by Traps MS/MS ? Organization: EarthLink Inc. -- http://www.EarthLink.net OK so I got a question on the method I posted...I know there are a few holes in the explanation...here's an attempt to patch one. Someone asked "Ok so how do you run the sample/method you created- exactly?" basically you set up a sample list with the file name you choose...then you pick the exp method you created earlier also...then you just start the infusion/nano-sample using the tune view..to get it spraying...once it is spraying you exit tune...go to the sample list you set up (one element perhaps) then run the sample...the issue that gets most people is that the thing won't start acquiring data...that is where this comes in... ************************************************************ *START Bill Haddon's instructions* ************************************************************ To run a sample on the LCQ using Syringe Pump Infusion and a Method File (triple play for ex) ************************************************************ Xcalibur ROADMAP SEQUENCE SETUP -- Actions -- Run this sample | run this sequence (Alt A s or Alt A h) RUN SEQUENCE box "Change Instruments" Button Remove LC and Autosampler Designate LCQ MS as Start Instrument ************************************************************ *END Bill Haddon's instructions* ************************************************************ basically you set the inst up to not wait for a contact closure or AS injection or whatever. It just starts when you start it. Matt Sweeney mattsweeney@earthlink.net Mass Spec Consulting Training/Operations/Consulting/Method Development LC/MS Pharmacokinetics, Peptides, Proteins, Metabolism, Maintenance Classes, Specialist in Finnigan Equipment and Software ****************************************************************************** From: "Craig Just" Date: Thu, 25 Jan 2001 10:58:49 -0600 Subject: LC/MS of explosives Organization: The University of Iowa Hello, Has anyone worked with LC/MS (or even MS/MS) of explosives compounds (RDX, TNT, HMX) and their metabolites? RDX, in particular, doesn't seem to be very amenable to electrspray since it doesn't really care to form an ion in solution. I'm looking to identify and quantify at fairly low levels in a green plant extract. Craig Just Department of Civil and Environmental Engineering The University of Iowa ****************************************************************************** From: "Justin Withers" Date: Thu, 25 Jan 2001 18:47:07 -0800 Subject: Re: LC/MS of explosives Organization: Posted via Supernews, http://www.supernews.com Do a lit. search for my colleague, Bruno Casetta. He did some work a few years ago, certainly on RDX and TNT. Don't recall what ion source, sorry. Regards, Justin "Craig Just" wrote in message news:94psn6$o3g$1@news-int.gatech.edu... } Hello, } } Has anyone worked with LC/MS (or even MS/MS) of explosives compounds (RDX, } TNT, HMX) and their metabolites? RDX, in particular, doesn't seem to be } very amenable to electrspray since it doesn't really care to form an ion in } solution. I'm looking to identify and quantify at fairly low levels in a } green plant extract. } } Craig Just } Department of Civil and Environmental Engineering } The University of Iowa } } } } ****************************************************************************** From: "Rich Yelton" Date: Fri, 26 Jan 2001 04:50:56 GMT Subject: Re: LC/MS of explosives Organization: Excite@Home - The Leader in Broadband http://home.com/faster Since CI/MS works so well for RDX you might want to try APCI MS. -- Richard O. Yelton Spectratek Mass Spectrometry Services Phone:859-341-6599 Fax: 859-341-6598 E-Mail: ryelton@massspecrepair.com Web: http://www.massspecrepair.com ****************************************************************************** From: Tony Hassett Date: Fri, 26 Jan 2001 11:08:46 +0200 Subject: HP 5988 Organization: University of Pretoria We have an HP 5988 quadrupole MS and one of our post grad. students inadvertently loosened the magnets on the source yoke while cleaning the source. It seems that these magnets need to be aligned in some way or other since the trap current is now too low and we cannot get proper spectra. There is a small arrow on each magnet, each facing in the same direction. Should these two arrows be aligned and does anyone know how they should be aligned in relation to the source. Regards TonyH ****************************************************************************** From: Amanda Palumbo Date: Fri, 26 Jan 2001 07:36:29 -0800 (PST) Subject: unknown peptide derivative Organization: * Hi, I was hoping for help identifying the strucure of a molecule by it's mass spectra. Peaks are: 70(100%), 389(73%), 42(69%), 168(35%), 55(7%), 84(4%), 97(3%), 11(3%), 210(3%, molecular ion?) It is a product of the tri peptide, valine-proline-leucine, reacted with tetramethyl ammoiniumhydroxide. The expected products of this reaction are the three individual amino acids with 2 methyl groups attached to the N ( or 1 for proline) and O-CH3 attached to the C=O end. The reaction is expected hydrolize peptides and then methylate the N and OH groups. I think this is an incomplete reaction product consisting of two of the amino acids and some degree of methylation, but nothing I come up with is consistent with both the reaction and the spectra. Any help anyone can provide would be very much appreciated. __________________________________________________ Do You Yahoo!? Yahoo! Auctions - Buy the things you want at great prices. http://auctions.yahoo.com/ ****************************************************************************** From: "Rich Yelton" Date: Fri, 26 Jan 2001 17:22:45 GMT Subject: Re: HP 5988 Organization: Excite@Home - The Leader in Broadband http://home.com/faster The proper orientation of the magnets that focus the filament electron beam is that they should be facing North to South. i.e the pole pieces should attract when correctly positioned around the filament/target path........ -- Richard O. Yelton Spectratek Mass Spectrometry Services Phone:859-341-6599 Fax: 859-341-6598 E-Mail: ryelton@massspecrepair.com Web: http://www.massspecrepair.com ****************************************************************************** From: Skoog Date: Fri, 26 Jan 2001 17:31:07 -0000 Subject: Re: unknown peptide derivative Organization: University College London Any chance of posting the spectra? "Amanda Palumbo" wrote in message news:94s98g$bte$1@news-int.gatech.edu... } Hi, } I was hoping for help identifying the strucure of a } molecule by it's mass spectra. } } Peaks are: } 70(100%), 389(73%), 42(69%), 168(35%), 55(7%), 84(4%), } 97(3%), 11(3%), 210(3%, molecular ion?) } } It is a product of the tri peptide, } valine-proline-leucine, reacted with tetramethyl } ammoiniumhydroxide. The expected products of this } reaction are the three individual amino acids with 2 } methyl groups attached to the N ( or 1 for proline) } and O-CH3 attached to the C=O end. The reaction is } expected hydrolize peptides and then methylate the N } and OH groups. } I think this is an incomplete reaction product } consisting of two of the amino acids and some degree } of methylation, but nothing I come up with is } consistent with both the reaction and the spectra. } Any help anyone can provide would be very much } appreciated. } } } } __________________________________________________ } Do You Yahoo!? } Yahoo! Auctions - Buy the things you want at great prices. } http://auctions.yahoo.com/ } } ****************************************************************************** From: diego88@my-deja.com Date: Sat, 27 Jan 2001 19:16:20 GMT Subject: Norcocaine Organization: Deja.com I am having a hard time finding the most abundant ions of norcaine using MTBSTFA as a derivative. Any help? Sent via Deja.com http://www.deja.com/ ****************************************************************************** From: Daniel Boismenu Date: Fri, 26 Jan 2001 23:59:25 GMT Subject: Re: LC/MS of explosives Organization: McGill University Mass Spectrometry Unit Greetings Craig, Last December, while I was attending the Lake Louise Tandem Mass Spectrometry Workshop (Alberta, Canada), there was a conference on RDX detection given by Richard Sleeman from Mass Spec Analytical Ltd. He told me that he would add 1% dichloromethane in the mobile phase in order to get the Cl adduct to RDX. You could then try it in electrospray in negative mode. Best Regards, Daniel Boismenu, Ph.D. Assistant Director McGill University Mass Spectrometry Unit 1130 Pine ave West Montréal, Qc Canada, H3A 1A3 tel (514)398-3661 fax (514)398-2488 email dboism1@po-box.mcgill.ca Craig Just wrote: } Hello, } } Has anyone worked with LC/MS (or even MS/MS) of explosives compounds (RDX, } TNT, HMX) and their metabolites? RDX, in particular, doesn't seem to be } very amenable to electrspray since it doesn't really care to form an ion in } solution. I'm looking to identify and quantify at fairly low levels in a } green plant extract. } } Craig Just } Department of Civil and Environmental Engineering } The University of Iowa ****************************************************************************** From: "pete" Date: Thu, 25 Jan 2001 11:05:53 -0500 Subject: Basic Internal standard questions.. Organization: Posted via Supernews, http://www.supernews.com Pretty green on a Elan 6100. Looking to troubleshoot sudden increase in IS recoveries. They started to climb to almost 200%. Any thoughts why? Thanks. ****************************************************************************** From: Kayce Date: Mon, 29 Jan 2001 22:57:36 GMT Subject: Sio2-Caso4 compound cocktail Organization: Deja.com Hi: To identify and quantify the elements in a chemical cocktail containing Sio2-Caso4 in addition to several minor components, ICP mass spectroscopy was recommendded to me. Can somebody provide info on the working principles, approx. cost of an ICP mass spec, vendors, universities/labs near New Mexico who might have it. Thanks in advance. Kayce Sent via Deja.com http://www.deja.com/ ****************************************************************************** From: Simon Date: Tue, 30 Jan 2001 07:01:58 GMT Subject: Re: unknown peptide derivative Organization: TIN Hello, ave you try to use the freewere program lutefisk to predict the structure of your peptide? Simon. Amanda Palumbo ha scritto: } Hi, } I was hoping for help identifying the strucure of a } molecule by it's mass spectra. } } Peaks are: } 70(100%), 389(73%), 42(69%), 168(35%), 55(7%), 84(4%), } 97(3%), 11(3%), 210(3%, molecular ion?) } } It is a product of the tri peptide, } valine-proline-leucine, reacted with tetramethyl } ammoiniumhydroxide. The expected products of this } reaction are the three individual amino acids with 2 } methyl groups attached to the N ( or 1 for proline) } and O-CH3 attached to the C=O end. The reaction is } expected hydrolize peptides and then methylate the N } and OH groups. } I think this is an incomplete reaction product } consisting of two of the amino acids and some degree } of methylation, but nothing I come up with is } consistent with both the reaction and the spectra. } Any help anyone can provide would be very much } appreciated. } } __________________________________________________ } Do You Yahoo!? } Yahoo! Auctions - Buy the things you want at great prices. } http://auctions.yahoo.com/ ****************************************************************************** From: Derek Bradley Date: Tue, 30 Jan 2001 16:50:18 +0000 Subject: MS: Protein MS References Organization: * Hi Guys, Does anyone know of good references/reviews regarding the MS analysis of proteins particularly with reference to MALDI and electrospray techniques. Thanks, Derek Bradley Dept. of Medicine UCL ****************************************************************************** From: wilfred_tang@yahoo.com Date: Wed, 31 Jan 2001 02:30:16 GMT Subject: Literature on peak detection and peak integration Organization: Deja.com I am interested in peak detection and peak integration. Given a spectrum (that is, a series of (x,y) data), I would like to answer the following questions: What is the background? Where are peaks located? For a given peak, what are the boundaries of the peak? (Once the boundaries of the peak are determined, integration is trivial.) What is the literature regarding this topic? I would think that this is a well-studied problem, but I’m not sure where to look for references. Thanks, Wilfred Tang wilfred_tang@yahoo.com Sent via Deja.com http://www.deja.com/ ****************************************************************************** From: Skoog Date: Wed, 31 Jan 2001 09:22:58 -0000 Subject: Re: unknown peptide derivative Organization: University College London Do you have a URL where I could download Lutefisk ? "Simon" wrote in message news:956g24$s68$1@news-int.gatech.edu... } Hello, ave you try to use the freewere program lutefisk to predict the } structure of your peptide? } } Simon. } } Amanda Palumbo ha scritto: } } } Hi, } } I was hoping for help identifying the strucure of a } } molecule by it's mass spectra. } } } } Peaks a