液-质联用法对人血浆中吗啡类、氯胺酮和苯丙胺类9种毒品的定性定量检测

摘要

目的:建立同时测定人血浆中吗啡、6-单乙酰吗啡、可待因、海洛因、氯胺酮、3,4-甲二氧基苯异丙胺、3,4-亚甲二氧基甲基安非他明、苯丙胺、甲基苯丙胺的定性定量检测方法.方法:血浆经10％三氯乙酸直接沉淀后进样分析.色谱柱为ACQUITY UPLC HSS C18柱,流动相为含0.01％甲酸的水溶液-0.01％甲酸的甲醇溶液,流速为0.3 mL· min-1,电喷雾离子源,用多反应监测,正离子分段扫描分析.结果:可用保留时间、特征碎片离子、分子离子峰丰度比为指标来定性鉴别血浆中9种化合物.另外,吗啡、可待因、海洛因、氯胺酮、6-单乙酰吗啡、3,4-甲二氧基苯异丙胺、3,4-亚甲二氧基甲基安非他明、苯丙胺、甲基苯丙胺血药浓度分别在5.00× 10-3～5.00(r=0.9934),1.00× 10-2～10.00(r=0.9905),1.00×10-2～10.00(r=0.9929),2.50×10-～ 2.50(r =0.9960),5.00× 10-3～ 5.00 (r=0.9925),5.00× 10-4～ 5.00(r=0.9910),5.00× 10-4～5.00(r=0.9924),5.00×10-4～5.00(r=0.9920),5.00× 10-4～5.00 (r=0.9900) μg· mL-1内,线性关系均良好;最低检测限分别为1.00、1.00、1.00、0.50、0.50、0.10、0.10、0.10、0.10 ng·mL-1.日内、日间精密度(RSD)均＜18％;提取回收率均＞60％,RSD均＜15％.结论:该方法灵敏、快速、准确、专属性强,可用于吗啡类、氯胺酮和苯丙胺类9种毒品化合物的定性筛查和定量检测研究.%Objective To develop the method for simultaneous identification and quantification of morphine,6-monoactylmorphine,codeine,heroin,ketamine,3,4-Methylenedioxyamphetamine (MDA),3,4-methylenedioxymethamphetamine (MDMA),amphetamine and methylamphetamine in human plasma.Methods UPLC-MS/MS was adopted to analyze plasma with protein precipitated using 10％ trichloroacetic acid.Plasma samples were separated on ACQUITY UPLC HSS C18 column with aqueous solution (0.01％ formic acid)-methanol (0.01％ formic acid) as the mobile phase,and at a flow rate of 0.3 mL·min-1.The multiple reaction monitoring (MRM) mode was performed combined with the positive ion mode for quantification in four sections.Results The retention time,the characteristic fragment ions,and the relative abundance ratio of the molecular ion peak could be used to identify these nine compounds sensitively.The liner calibration curve of morphine,codeine,heroin,ketamine,6-monoacetylmorphine,MDA,MDMA,amphetamine and methamphetamine were obtained in the concentration range of 5.00×10-3～5.00 (r=0.9934),1.00× 10-2～ 10.00 (r=0.9905),1.00× 10-2～ 10.00 (r=0.9929),2.50× 10-3 ～2.50 (r=0.9960),5.00× 10-3 ～ 5.00 (r=0.9925),5.00× 10-4 ～ 5.00 (r=0.9910),5.00× 10-4 ～ 5.00 (r=0.9924),5.00× 10-4 ～ 5.00 (r=0.9920) and 5.00×10-4～5.00 μg·mL-1 (r=0.9900) respectively.The lowest detection limit was 1.00,1.00,1.00,0.50,0.50,0.10,0.10,0.10 and 0.10 ng· mL-1 respectively.The relative standard deviation (RSD) of the inter-day and intra-day were less than 18％.The relative recovery was more than 60％,and the RSD were less than 15％.Conclusion The method is accurate,sensitive and suitable for identification and quantification of 9 drugs of opiates,ketamine and amphetamines in human plasma.