Extending the detection window of diazepam by directly analyzing its glucuronide metabolites in human urine using liquid chromatography-tandem mass spectrometry

被引：16
作者：
Wang, Xin [1 ,2 ]
Wang, Rong [2 ]
Zhang, Yurong [2 ]
Liang, Chen [2 ]
Ye, Haiying [2 ]
Cao, Fangqi [2 ]
Rao, Yulan [3 ]
机构：
[1] Shanghai Inst Pharmaceut Ind, State Key Lab New Drug & Pharmaceut Proc, Shanghai 200040, Peoples R China
[2] Shanghai Inst Forens Sci, Shanghai Key Lab Crime Scene Evidence, Shanghai 200083, Peoples R China
[3] Fudan Univ, Sch Basic Med Sci, Dept Forens Med, Shanghai 200032, Peoples R China
来源：
JOURNAL OF CHROMATOGRAPHY A | 2012年 / 1268卷
关键词：
Diazepam; Glucuronide metabolites; Human urine; Detection window; SPE; LC-MS/MS; GAS-CHROMATOGRAPHY; BENZODIAZEPINES; EXTRACTION; OXAZEPAM; BLOOD; 1,4-BENZODIAZEPINES; VALIDATION; PLASMA; SERUM;
D O I：
10.1016/j.chroma.2012.10.012
中图分类号：
Q5 [生物化学];
学科分类号：
071010 ; 081704 ;
摘要：
A method for the simultaneous direct analysis of diazepam oxazepam glucuronide, temazepam glucuronide, oxazepam, nordiazepam, and temazepam in human urine was developed and validated. Urine sample was purified by solid phase extraction (SPE), and the analysis was achieved using a liquid chromatography-tandem mass spectrometry (LC-MS/MS) system equipped with an electrospray ionization source (ESI). Multiple reaction monitoring (MRM) mode was used to analyze the target compounds. Extraction recoveries were 65-122% for all the analytes. The method showed acceptable intra-assay and inter-assay precision (both relative standard deviation (RSD) <= 11.2%) for quality control (QC) samples. The limits of detections (LODs) were in the range of 0.1-2 ng/mL. The present assay was applied to analyze the urine obtained from three volunteers after oral administration of a single dose 5 mg of diazepam. The results showed that, the detection periods of oxazepam glucuronide and temazepam glucuronide were much longer than diazepam and other metabolites. (C) 2012 Elsevier B.V. All rights reserved.
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收藏
页码：29 / 34
页数：6
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