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An atmospheric pressure chemical ionisation liquid chromatographic–tandem mass spectrometry method for the analysis of benzodiazepines in urine
Journal of Chromatography B ( IF 3 ) Pub Date : 2017-08-24 , DOI: 10.1016/j.jchromb.2017.08.023
S. Dunlop , K. Hayes , P. Leavy , D. Cusack , R. Maguire

The objective of this work was to establish an analytical method for the analysis of 7 Benzodiazepines (diazepam, oxazepam, temazepam, nordiazepam, desalkylflurazepam, alprazolam and α-hydroxyalprazolam) in urine specimens taken from drivers suspected of driving under the influence of drugs. The specimen, calibrator and control preparation involved hydrolysis of conjugated benzodiazepines using β-glucuronidase in sodium acetate buffer, with incubation at 60 °C for 2 h. Specimens were then centrifuged, before being diluted 1 in 5 (total dilution 1 in 10), with 10% acetonitrile in water. Specimens were analysed using a Shimadzu Prominence UPLC coupled to an AB Sciex 4000 QTrap LC–MS-MS. The chromatographic column was a Shim-pack XR ODS 2.2 μm. 3.0 × 50 mm column and the mobile phase was a binary gradient system comprising of mobile phase A which was an ammonium formate/formic acid buffer dissolved in water and mobile phase B which was an ammonium formate/formic acid buffer dissolved in Acetonitrile. APCI was selected as the ionisation technique and the MS was operated in MRM mode, monitoring 2 transitions per analyte. The validation of the method is described. The method was found to be linear, accurate and precise (within day and between day) for diazepam, oxazepam, temazepam, nordiazepam, desalkylflurazepam, alprazolam and α-hydroxyalprazolam. The results of 480 cases are reviewed and show that alprazolam use was found in 35% of cases. Use of benzodiazepines resulting in oxazepam, nordiazepam or temazepam were found ca. 70% of cases analysed.



中文翻译:

大气压化学电离液相色谱-串联质谱法分析尿中苯二氮卓类药物

这项工作的目的是建立一种分析方法,以分析从怀疑受药物影响驾驶的驾驶员尿液样本中的7种苯二氮卓类药物(地西p,奥沙西m,替马西m,去甲地西,、去烷基氟拉西epa,阿普唑仑和α-羟基阿普唑仑)。标本,校准品和对照品包括在乙酸钠缓冲液中使用β-葡萄糖醛酸苷酶水解共轭苯并二氮杂ze,并在60°C下孵育2小时。然后将样品离心,然后用10%的乙腈水溶液稀释至1:5(总稀释度:1:10)。使用Shimadzu Prominence UPLC和AB Sciex 4000 QTrap LC-MS-MS进行样品分析。色谱柱为Shim-pack XR ODS 2.2μm。3。0×50 mm色谱柱,流动相为二元梯度系统,该系统由流动相A和流动相B组成,流动相A为溶于水的甲酸铵/甲酸缓冲液,流动相B为溶于乙腈的甲酸铵/甲酸缓冲液。选择了APCI作为电离技术,MS在MRM模式下运行,每个分析物监测2个离子对。描述了该方法的有效性。已发现该方法对于地西epa,奥沙西m,替马西m,去甲西p,去烷基氟拉西m,阿普唑仑和α-羟基阿普唑仑是线性的,准确的和精确的(一天之内和一天之间)。审查了480例病例的结果,结果表明35%的病例中使用了阿普唑仑。大约在2000年发现使用苯二氮卓类药物导致奥沙西m,去甲西ze或替马西m。已分析70%的案例。

更新日期:2017-08-24
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