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Quantitative gas chromatographic/mass spectrometric analysis of morphine glucuronides in human plasma by negative ion chemical ionization mass spectrometry
Author(s) -
Leis Hans Jörg,
Fauler Günter,
Raspotnig Günther,
Windischhofer Werner
Publication year - 2002
Publication title -
journal of mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 1076-5174
DOI - 10.1002/jms.294
Subject(s) - chemistry , chromatography , mass spectrometry , selected ion monitoring , chemical ionization , detection limit , gas chromatography–mass spectrometry , glucuronide , gas chromatography , metabolite , solid phase extraction , morphine , quantitative analysis (chemistry) , ionization , ion , organic chemistry , medicine , biochemistry , pharmacology
Abstract A sensitive and specific method for the determination of morphine glucuronides in human plasma is presented. Morphine glucuronides, namely morphine‐6‐glucuronide (M6G) and morphine‐3‐glucuronide (M3G), were extracted from plasma by solid‐phase extraction on C 18 cartridges at pH 9.3 and derivatized to their pentafluorobenzyl ester trimethylsilyl ether derivatives. The compounds were measured by gas chromatography/negative ion chemical ionization mass spectrometry without any further purification. Using this detection mode, a diagnostic useful fragment ion at m/z 748 was obtained at high relative abundance for both target compounds. [ 2 H 3 ]‐labeled morphine glucuronides were used as internal standards. Calibration graphs were calculated by polynomial fit within a range of 10–1280 and 15–1920 nmol l −1 for the 6‐ and 3‐glucuronide, respectively. At the limit of quantitation (LOQ), the inter‐assay precision was 2.21% (M3G) and 2.23% (M6G) and the GC/MS assay variability was 1.8% (M3G) and 0.9% (M6G). The accuracy at the LOQ showed deviations of +4.92% (M3G) and +1.5% (M6G). The sample recovery after solid‐phase extraction was 84.7% for both M3G and M6G. The method is rugged, rapid and robust and has been applied to the batch analysis of morphine glucuronides during pharmacokinetic profiling of the drugs. Copyright © 2002 John Wiley & Sons, Ltd.