Premium
Optimization of short‐column gas chromatography/electron ionization mass spectrometry conditions for the determination of underivatized anabolic steroids
Author(s) -
Rossi StacyAnn,
Johnson Jodie V.,
Yost Richard A.
Publication year - 1992
Publication title -
biological mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 1052-9306
DOI - 10.1002/bms.1200210903
Subject(s) - chromatography , chemistry , mass spectrometry , electron ionization , gas chromatography , analytical chemistry (journal) , fragmentation (computing) , gas chromatography–mass spectrometry , mass spectrum , direct electron ionization liquid chromatography–mass spectrometry interface , chemical ionization , resolution (logic) , ionization , ion , computer science , organic chemistry , artificial intelligence , operating system
A gas chromatographic/mass spectrometric method based on the use of short capillary gas chromatograph columns (3‐5 m) and electron ionization mass spectrometry has been optimized and evaluated for the determination of underivatized anabolic steroids. The short‐column gas chromatographic/mass spectrometric method was shown to result in short analysis times and to require minimal sample preparation, but suffered from some loss in sensitivity and chromatographic resolution compared with conventional gas chromatographic/mass spectrometric techniques for derivatized steroids. Therefore, short‐column gas chromatographic conditions were optimized to maximize the sample transfer efficiency (sensitivity) from the gas chromatograph into the ion source of the mass spectrometer, while maintaining chromatographic integrity and minimizing thermal decomposition. Mass spectrometric conditions were optimized to maximize ionization efficiency with respect to the intensity of the molcular ion and degree of fragmentation such that positive identication of each steroid could be made based on the resulting mass spectra. Under optimized conditons, we have shown that underivatized anabolic steroids spiked into urine samples can be determined at low‐nanogram levels using short‐column chromatography/full‐scan electron ionization mass spectrometry.