Direct determination of diazepam and its glucuronide metabolites in human whole blood by 渭Elution solid-phase extraction and liquid chromatography-tandem mass spectrometry

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• 作者：Rong Wang ; Xin Wang ; Chen Liang ; Chunfang Ni ; Lingjuan Xiong ; Yulan Rao ; Yurong Zhang
• 关键词：Diazepam ; Diazepam glucuronides ; 96-Well 渭Elution plate solid-phase extraction ; Human whole blood ; LC&ndash ; MS/MS
• 刊名：Forensic Science International
• 出版年：10 December, 2013
• 年：2013
• 卷：233
• 期：1-3
• 页码：304-311
• 全文大小：1367 K

文摘

A 渭Elution solid-phase extraction (SPE) liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for simultaneous determination of diazepam, nordiazepam, oxazepam, oxazepam glucuronide, temazepam and temazepam glucuronide in human whole blood is presented. 200 渭L of whole blood samples were loaded onto a Waters Oasis HLB 96-well 渭Elution SPE plate using 75 渭L of methanol as the elution solvent, and the eluents were injected into an Eclipse XDB C18 column. No hydrolysis, solvent transfer, evaporation or reconstitution was involved in the sample preparation procedures. Tandem mass spectrometric detection with Turbo Ion Spray was conducted via multiple reaction monitoring (MRM) under positive ionization mode. The method was validated and proved to be accurate (accuracy within 93-108%), precise (intra-day RSD < 9.9% and inter-day RSD < 7.2%) and sensitive with limits of detection (LOD) in the range of 0.05-0.25 ng/mL for all the compounds. Extraction recoveries were in the range of 31-80% for all the analytes. This method demonstrated to be reproducible and reliable. The applicability of the method was demonstrated by analysis of several forensic cases involving diazepam and its metabolites.