冯雪伊,陈航,沈敏,向平
单位
1.中国刑事警察学院法化学系
2.司法部司法鉴定科学技术研究所 上海市法医学重点实验室基金项目:国家级科研院所公益项目(GY2016Z-1)；国家自然科学基金面上项目(81273340)；上海市法医学重点实验室项目(14DZ2270800)
中文摘要:采用微波辅助提取(MAE)与液相色谱-串联质谱(LC-MS/MS)技术，建立了同时测定人体指甲中14种抗精神失常及安眠镇静类物质的分析方法。指甲经冷冻研磨后加入内标溶液，用微波辅助提取。以Allure PFPP苯基柱分离，甲醇(含20mmol/L乙酸铵)-乙酸铵(20mmol/L)进行梯度洗脱，采用二级质谱多反应监测模式(MRM)检测14种抗精神失常和安眠镇静类物质及其代谢物。目标物在对应含量范围内均线性良好(r2≥0.990)；检出限为0.1~50pg/mg；大多数目标物的定量下限为100pg/mg；日内精密度和日间精密度均不大于7.8%；准确度在±10.16%范围内。对7例服用部分抗精神失常及安眠镇静类药物的患者指甲进行分析，目标物检出情况与用药情况相符。该方法样品处理简便、高效、快速且分析准确、灵敏度高、选择性好，可用于人体指甲中pg/mg级抗精神失常及安眠镇静类物质的定性定量分析。
中文关键词:微波辅助提取(MAE) 液相色谱-串联质谱(LC-MS/MS) 指甲 抗精神失常及安眠镇静类物质
Simultaneous Determination of 14 Antipsychotic and Sedative Substances in Human Nails Using Microwave-assisted Extraction Combined with Liquid Chromatography-Tandem Mass Spectrometry
Abstract:A method based on microwave-assisted extraction combined with liquid chromatography-tandem mass spectrometry(MAE/LC-MS/MS) was established for the simultaneous determination of 14 antipsychotic and sedative substances in human nails.About 20 mg of decontaminated and pulverized nail samples was microwave-assistedly extracted for twice in the presence of clozapine-d4 used as the internal standard, and the supernatant was determined by LC-MS/MS using the Allure PFPP column with a mobile phase of methanol(containing 20mmol/L ammonium acetate)-20mmol/L ammonium acetate buffer. Multiple reaction monitoring(MRM) mode was used to analyze 14 antipsychotic and sedative substances. Good linearities(r2≥0.990) over the corresponding range were obtained for all the analytes.The limits of detection(LOD) were in the range of 0.1-50pg/mg and the limits of quantitation(LOQ) were 100pg/mg for most of the analytes.The deviations of intra- and inter-RSD were not more than 7.8%.Accuracies were within ±10.16%.Positive results were obtained from 7 authentic nail samples,which were in good accordance with the drug administration of the corresponding antipsychotic and sedative substances.The developed method presents a simplified,efficient and rapid procedure for sample preparation,and shows high sensitivity and selectivity,which is suitable for the simultaneous analysis of 14 antipsychotic and sedative substances at pg/mg levels in nail samples.
Key Words:microwave-assisted extraction(MAE) liquid chromatography-tandem mass spectrometry(LC-MS/MS) nails antipsychotic and sedative substances
引用本文：冯雪伊,陈航,沈敏,向平.微波辅助提取/液相色谱-串联质谱法同时测定人体指甲中14种抗精神失常及安眠镇静类物质[J].分析测试学报,2016,35(10):1233-1340.
