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Supercritical fluid extraction and negative ion electrospray liquid chromatography tandem mass spectrometry analysis of phenobarbital, butalbital, pentobarbital and thiopental in human serum

1998; Wiley; Volume: 12; Issue: 13 Linguagem: Inglês

10.1002/(sici)1097-0231(19980715)12

1097-0231

J. Christopher Spell, Karthik Srinivasan, James T. Stewart, Michael G. Bartlett,

Analytical chemistry methods development

Rapid Communications in Mass SpectrometryVolume 12, Issue 13 p. 890-894 Research Article Supercritical fluid extraction and negative ion electrospray liquid chromatography tandem mass spectrometry analysis of phenobarbital, butalbital, pentobarbital and thiopental in human serum J. Christopher Spell, J. Christopher Spell Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, GA 30602-2352, USASearch for more papers by this authorKarthik Srinivasan, Karthik Srinivasan Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, GA 30602-2352, USASearch for more papers by this authorJames T. Stewart, James T. Stewart Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, GA 30602-2352, USASearch for more papers by this authorMichael G. Bartlett, Corresponding Author Michael G. Bartlett Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, GA 30602-2352, USADepartment of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, GA 30602-2352, USASearch for more papers by this author J. Christopher Spell, J. Christopher Spell Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, GA 30602-2352, USASearch for more papers by this authorKarthik Srinivasan, Karthik Srinivasan Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, GA 30602-2352, USASearch for more papers by this authorJames T. Stewart, James T. Stewart Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, GA 30602-2352, USASearch for more papers by this authorMichael G. Bartlett, Corresponding Author Michael G. Bartlett Department of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, GA 30602-2352, USADepartment of Pharmaceutical and Biomedical Sciences, College of Pharmacy, The University of Georgia, Athens, GA 30602-2352, USASearch for more papers by this author First published: 04 December 1998 https://doi.org/10.1002/(SICI)1097-0231(19980715)12:13 3.0.CO;2-XCitations: 30AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinked InRedditWechat Abstract Four commonly used barbiturates (phenobarbital, butalbital, pentobarbital and thiopental) were analyzed in human serum using supercritical fluid extraction (SFE) and negative ionization LC/ESI-MS/MS. Barbital was used as the internal standard. Carbon dioxide SFE was performed at 40 °C and 500 atm, with a total extraction time of 35 min. The analytes were collected off-line in a liquid trap containing absolute methanol. Samples were then concentrated by vacuum centrifugation. The high performance liquid chromatography separation utilized gradient elution with a total analysis time of 21 min. The precursor and major product ions for the four barbiturates were monitored on a triple quadrupole mass spectrometer with negative ion electrospray ionization (ESI) in the multiple reaction monitoring mode as follows: (1) thiopental (m/z 241.20 → 58.00), (2) phenobarbital (m/z 231.10 → 188.0), (3) pentobarbital (m/z 225.10 → 181.90) and (4) butalbital (m/z 222.80 → 179.90). In the case of phenobarbital, pentobarbital and butalbital, the most abundant product ion arises from the loss of 43 u (HCNO loss). However, in the case of thiopental, the most abundant product ion was observed at m/z 58.0 (the [M − 183]− ion, or NCS−). Mechanisms for the formation of the collision induced dissociation reaction products of these barbiturates are proposed. © 1998 John Wiley & Sons, Ltd. Citing Literature Volume12, Issue1315 July 1998Pages 890-894 RelatedInformation