超高效液相色谱-串联质谱法测定生物样品中常见毒品
UHPLC-MS/MS Determination of Common Narcotic Drugs in Biological Samples
摘 要
提出了高效液相色谱-串联质谱法测定血液、尿液和唾液中甲基苯丙胺、吗啡和O6-单乙酰吗啡含量的方法。试样中蛋白用乙腈沉淀后离心分离除去,所得滤液用于高效液相色谱-串联质谱分析。3种毒品的峰面积与质量浓度分别在1~500 μg·L-1(甲基苯丙胺)和1~1 000 μg·L-1(吗啡和O6-单乙酰吗啡)范围内呈线性,方法的检出限(3S/N)在0.2~0.5 μg·L-1之间。在空白血液、尿液和唾液样品中添加3个水平混合标准溶液,测得3种毒品的回收率在62.4%~106.3%之间,日内与日间相对标准偏差(n=6)分别在3.4%~17.4%,6.1%~17.8%之间。
毒品
生物样品
UHPLC-MS/MS
Narcotic drugs
Biological samples
Abstract
A method of UHPLC-MS/MS for the determination of 3 common narcotic drugs, i.e., methamphetamine, morphine and 6-acetylmorphine, in blood, urine and saliva was proposed. Protein in sample was precipitated with acetonitrile and the filtrate obtained after centrifugation was analyzed by UHPLC-MS/MS. Linear relationships between values of peak area and mass concentration of the 3 drugs were kept in the ranges of 1-500 μg·L-1 for methamphetamine and 1-1 000 μg·L-1 for morphine and 6-acetylmorphine, with detection limits (3S/N) in the range of 0.2-0.5 μg·L-1. Recovery and precision of the method were tested by addition of mixed standard of the 3 drugs at 3 concentration levels of 10, 20, 50 μg·L-1, giving values of recovery in the range of 62.4%-106.3%. Values of intraday and interday relative standard deviation (n=6) found were in the ranges of 3.4%-17.4% and 6.1%-17.8% respectively.
中图分类号 O657.63
所属栏目 工作简报
基金项目 中央高校基本科研业务费专项资金资助(YX11013)
收稿日期 2012/5/27
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备注陈跃(1983-),男,山东临沂人,博士研究生,主要从事毒物、毒品分析工作。
引用该论文: CHEN Yue,LIN Lei-xiang,ZHANG Yun-feng,YU Zhong-shan,ZHU Jun,ZOU Ji-xin,YUE Yue. UHPLC-MS/MS Determination of Common Narcotic Drugs in Biological Samples[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(10): 1154～1157
陈跃,林雷祥,张云峰,于忠山,朱军,邹积鑫,岳玥. 超高效液相色谱-串联质谱法测定生物样品中常见毒品[J]. 理化检验－化学分册, 2012, 48(10): 1154～1157
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【3】邸玉敏,朱军,常靖,等.GC/MS、GC/NPD法检测血液中氯胺酮［J］.刑事技术, 2010(3):11-14.
【4】李雯佳,廖林川,陈礼莉,等.GC法检测血液和尿液中甲基苯丙胺和咖啡因［J］.中国法医学杂志, 2009,24(1):11-14.
【5】孟品佳,张吉林.毛细管区带电泳定量分析苯丙胺类毒品［J］.中国人民公安大学学报:自然科学版, 2006(1):5-7.
【6】孟梁,王燕燕,孟品佳,等.分散液相微萃取-毛细管电泳法同时检测唾液中的8种毒品［J］.分析化学, 2011,39(7):1077-1082.
【7】KUDO K, ISHIDA T, HARA K, et al. Simultaneous determination of 13 amphetamine related drugs in human whole blood using an enhanced polymer column and gas chromatography-mass spectrometry［J］. J Chromatogra B, 2007(855):115-120.
【8】PETERS F T, SCHAEFER S, STAACK R F, et al. Screening for and validated quantification of amphetamines and of amphetamine- and piperazine-derived designer drugs in human blood plasma by gas chromatographymass spectrometry［J］. J Mass Spectrom, 2003,38:659-676.
【9】王燕燕,孟品佳.固相萃取SPE-GC/MS法检测人血中的鸦片类毒品［J］.应用化学, 2009,26(12):1495-1497.
【10】DRESEN S, FERREIROS N, GNANN H, et al. Detection and identification of 700 drugs by multi-target screening with a 3200 Q TRAP LC-MSMS system and library searching［J］. Anal Bioanal Chem, 2010,396:2425-2434.
【11】CONCHEIRO M, CASTRO A, QUINTELA O, et al. Determination of illicit and medicinal drugs and their metabolites in oral fluid and preserved oral fluid by liquid chromatography-tandem mass spectrometry［J］. Anal Bioanal Chem, 2008,391:2329-2338.
【12】CONCHEIRO M, GRAY T R, SHAKLEYA D M, et al. High-throughput simultaneous analysis of buprenorphine,methadone, cocaine, opiates, nicotine, and metabolites in oral fluid by liquid chromatography tandem mass spectrometry［J］. Anal Bioanal Chem, 2010,398:915-924.
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