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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
  • ISSN号:1004-4957
  • 期刊名称:《分析测试学报》
  • 分类:O657.63[理学—分析化学;理学—化学] TQ460.72[医药卫生—药物分析学;化学工程—制药化工]
  • 作者机构:[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
  • 相关基金: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)
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。

英文摘要:

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.

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期刊信息
  • 《分析测试学报》
  • 北大核心期刊(2011版)
  • 主管单位:广东省科学技术厅
  • 主办单位:中国分析测试协会 中国广州分析测试中心
  • 主编:陈小明
  • 地址:广州市先烈中路100号34栋B201中国广州分析测试中心内
  • 邮编:510070
  • 邮箱:fxcsxb@china.com
  • 电话:020- 37656606
  • 国际标准刊号:ISSN:1004-4957
  • 国内统一刊号:ISSN:44-1318/TH
  • 邮发代号:46-104
  • 获奖情况:
  • 获广东省第一、二届优秀期刊奖
  • 国内外数据库收录:
  • 俄罗斯文摘杂志,美国化学文摘(网络版),日本日本科学技术振兴机构数据库,中国中国科技核心期刊,中国北大核心期刊(2004版),中国北大核心期刊(2008版),中国北大核心期刊(2011版),中国北大核心期刊(2014版),英国英国皇家化学学会文摘,中国北大核心期刊(2000版)
  • 被引量:25362