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  

Simultaneous Determination of 14 Antipsychotic and Sedative Substances in Human Nails Using Microwave-assisted Extraction Combined with Liquid Chromatography-Tandem Mass Spectrometry

作　　者：冯雪伊 陈航[2] 沈敏[2] 向平[2] 

机构地区：[1]中国刑事警察学院法化学系,辽宁沈阳110854 [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,上海200063

出　　处：《分析测试学报》2016年第10期1233-1240,共8页Journal of Instrumental Analysis

基　　金：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)

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20 mmol/L乙酸铵)-乙酸铵(20 mmol/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(r^2≥0.990);检出限为0.1~50 pg/mg;大多数目标物的定量下限为100 pg/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。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 pulver- ized 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 20 mmol/L ammonium acetate） -20 mmol/L am- monium acetate buffer. Multiple reaction monitoring（MRM） mode was used to analyze 14 antipsy- chotic and sedative substances. Good linearities （ re I〉0. 990） over the corresponding range were ob- tained for all the analytes. The limits of detection （LOD） were in the range of 0. 1 - 50 pg/mg and the limits of quantitation（LOQ） were 100 pg/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 ob- tained 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 simpli- fied, 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.

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 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]