Sun Ying-Ying, Xiang Ping, Shen Min
Department of Forensic Medicine, Institute of Preclinical Medicine and Biological Science, Soochow University, Suzhou 215123, China.
Yao Xue Xue Bao. 2011 Dec;46(12):1501-6.
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 11 opiates in hair samples and identify legal and illegal use of opiates.
本文报道了一种用于同时分析毛发样本中11种阿片类药物的液相色谱-串联质谱法（LC-MS/MS），以及对活跃海洛因成瘾者毛发中阿片类药物存在情况的研究。将约20mg经过净化和粉碎的毛发样本在作为内标的吗啡-d3和乙酰吗啡-d6存在下，用缓冲溶液水解30分钟，然后用二氯甲烷和异丙醇的混合物萃取，通过Allure PFP丙基柱分离，流动相由乙腈和20mmol L(-1)醋酸铵缓冲液组成，然后用LC-MS/MS进行分析。采用多反应监测（MRM）模式分析11种阿片类药物。11种阿片类药物在相应范围内呈现出相当好的线性关系（r > 0.996 0）。检测限小于0.05 ng mg(-1)。回收率在47.2%至110%之间，日内和日间精密度偏差小于14%。在21名海洛因成瘾者的毛发样本中检测到了海洛因、乙酰吗啡、吗啡、可待因、乙酰可待因和氢可酮。所建立的方法具有高灵敏度和选择性，适用于毛发样本中11种阿片类药物的同时分析，并可鉴别阿片类药物的合法和非法使用情况。
