采用负离子化学电离气相色谱/质谱联用和串联质谱法测定四种合成代谢类固醇代谢物。

Determination of four anabolic steroid metabolites by gas chromatography/mass spectrometry with negative ion chemical ionization and tandem mass spectrometry.

作者信息

Choi M H, Chung B C, Kim M, Choi J, Kim Y

机构信息

Doping Control Centre, Korea Institute of Science and Technology, Cheongryang, Seoul, Korea.

出版信息

Rapid Commun Mass Spectrom. 1998;12(22):1749-55. doi: 10.1002/(SICI)1097-0231(19981130)12:22<1749::AID-RCM395>3.0.CO;2-S.

DOI:10.1002/(SICI)1097-0231(19981130)12:22<1749::AID-RCM395>3.0.CO;2-S

PMID:9853384

Abstract

A gas chromatography/mass spectrometry method is described which uses negative ion chemical ionization and tandem mass spectrometry for the determination of anabolic steroid metabolites. Four anabolic steroid metabolites to be derivatized by Pentafluoropropionic anhydride (PFPA) were determined using gas chromatography/mass spectrometry (GC/MS) with negative chemical ionization (NCI) and NCI/MS/MS. The repeatability and reproducibility of this procedure were in the range of 5.3-9.7% and 6.1-10.2%, respectively. This method of derivatization with PFPA for NCI and NCI/MS/MS was useful to determine four metabolites of nandrolone, dromostanolone, methenolone and boldenone. The derivatized metabolites of boldenone could be detected to 2 ppb and the other three steroids could be detected to 25 ppb in urine at a signal-to-noise ratio of S/N = 3.

摘要

描述了一种气相色谱/质谱法，该方法使用负离子化学电离和串联质谱来测定合成代谢类固醇代谢物。使用气相色谱/质谱（GC/MS）结合负离子化学电离（NCI）和NCI/MS/MS测定了四种将用五氟丙酸酐（PFPA）进行衍生化的合成代谢类固醇代谢物。该方法的重复性和再现性分别在5.3 - 9.7%和6.1 - 10.2%的范围内。这种用PFPA进行衍生化用于NCI和NCI/MS/MS的方法对于测定诺龙、屈他雄酮、美睾酮和勃地酮的四种代谢物很有用。在信噪比S/N = 3时，尿液中勃地酮的衍生化代谢物可检测到2 ppb，其他三种类固醇可检测到25 ppb。