液相色谱-串联质谱法测定头发中11种阿片类生物碱  

Simultaneous determination of 11 opiates in hair by liquid chromatography-tandem mass spectrometry

作　　者：孙英英[1,2] 向平[2] 沈敏[2] 

机构地区：[1]苏州大学基础医学与生物科学学院法医学系,江苏苏州215123 [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：《药学学报》2011年第12期1501-1506,共6页Acta Pharmaceutica Sinica

基　　金：国家自然科学基金资助项目(20975070);国家科研院所公益项目(GY0903)

摘　　要：建立头发中海洛因、吗啡、单乙酰吗啡等11种阿片类生物碱的液相色谱-串联质谱测定方法,并考察海洛因滥用者头发中阿片类组分的存在情况。头发经冷冻研磨后加入硼酸缓冲液超声30 min,用氯仿-异丙醇(9∶1)提取。用Allure PFP丙基柱,以乙腈-乙酸铵(0.1%甲酸)梯度洗脱分离,采用二级质谱多反应监测模式(MRM)检测11种阿片类生物碱。头发中海洛因、吗啡、单乙酰吗啡等11种阿片类生物碱在对应质量浓度范围内线性良好(r>0.996 0);检测限(LOD)均小于0.05 ng.mg-1;回收率范围为47.2%～110%;日内精密度和日间精密度均小于14%。21例海洛因滥用者头发中均检出了海洛因、单乙酰吗啡、吗啡、可待因、乙酰可待因、氢可酮等主要组分。所建方法灵敏度高、选择性好,适用于同时分析头发中海洛因等11种阿片类生物碱组分,可有效鉴别海洛因滥用与阿片类药物或食品的摄取。The paper reports the establishment of a liquid chromatography-tandem mass spectrometry（LC-MS/MS） for simultaneous analysis of 11 opiates in hair samples,and the study of presence of opiates in the hair of active heroin addicts.About 20 mg of decontaminated and pulverized hair sample was hydrolyzed with buffer solution for 30 min,in the presence of morphine-d3 and acetylmorphine-d6 used as internal standards,and then extracted with the mixture of dichlormethane and isopropanol,separated by the Allure PFP propyl column with a mobile phase consisting of acetonitrile and 20 mmol-L-1 ammonium acetate buffer,and then analyzed by LC-MS/MS.Multiple reaction monitoring（MRM） mode was used to analyze 11 opiates.Eleven opiates showed a fairly good linearity over the corresponding range（r 0.996 0）.The detection limits were less than 0.05 ng-mg-1.The recoveries were between 47.2% and 110%,and the deviations of intra-and inter-day precision were less than 14%.Heroin,acetylmorphine,morphine,codeine,acetylcodeine and hydrocodone were detected in hair samples of 21 herion addicts.The developed method shows high sensitivity and selectivity,and is suitable for the simultaneous analysis of 11opiates in hair samples and identify legal and illegal use of opiates.

关 键 词：头发 阿片类生物碱 LC-MS/MS 

分 类 号：R917[医药卫生—药物分析学]