采用气相色谱-质谱联用技术测定尿液中诺龙及其代谢物。

The determination of nandrolone and its metabolites in urine by gas chromatography-mass spectrometry.

作者信息

Ozer D, Temìzer A

机构信息

Department of Analytical Chemistry, Faculty of Pharmacy, Hacettepe University, Ankara, Turkey.

出版信息

Eur J Drug Metab Pharmacokinet. 1997 Oct-Dec;22(4):421-5. doi: 10.1007/BF03190980.

DOI:10.1007/BF03190980

PMID:9512944

Abstract

The determination of nandrolone and its major metabolites in urine of a healthy volunteer is typically performed by fused-silica capillary column gas chromatography with electron impact quadropole mass spectrometry. Two well-known urinary metabolites of nandrolone, 19-norandrosterone and 19-norethiocholanolone, were isolated by XAD-2 adsorption from urine, eluted with methanol and separated into unconjugated and conjugated fractions. The conjugated fraction was hydrolyzed with beta-glucuronidase from Escherichia coli and the samples derivatized with MSTFA/ammonium iodide/dithioerythritol. Ion fragmentograms of the bis-trimethylsilyl derivatives of nandrolone and its metabolites displayed molecular ions of M+ = 420 and M(+) -15 = 405. Extraction yield and the minimum detection limit of nandrolone in urine were identified. Finally, excretion rates of nandrolone and its metabolites in urine were determined.

摘要

健康志愿者尿液中诺龙及其主要代谢产物的测定通常采用熔融石英毛细管柱气相色谱法结合电子轰击四极杆质谱法进行。通过XAD - 2吸附从尿液中分离出诺龙的两种著名尿液代谢产物，即19 - 去甲雄酮和19 - 去甲硫代胆烷醇酮，用甲醇洗脱并分离为未结合和结合部分。结合部分用来自大肠杆菌的β - 葡萄糖醛酸酶水解，样品用MSTFA/碘化铵/二硫赤藓糖醇衍生化。诺龙及其代谢产物的双三甲基硅烷基衍生物的离子碎片图显示分子离子为M+ = 420和M(+) - 15 = 405。确定了尿液中诺龙的提取率和最低检测限。最后，测定了尿液中诺龙及其代谢产物的排泄率。