气相色谱-质谱联用法检测不同成瘾程度吸毒人员毛发样本研究  

Study on hair concentration of amphetamines of drug abusers by gas chromatography-mass spectrometry

作　　者：倪四阳[1] 武峰[1] 王淑民[1] 宋思玥 赵秀丽[1] 周延明 NI Si-yang;WU Feng;WANG Shu-min;SONG Si-yue;ZHAO Xiu-li;ZHOU Yan-ming(Clinical Trials for Human Used Drug,Beijing Tongren Hospital,Capital Medical University,Beijing 100730,China;The Ankang Hospital of Heilongjiang Public Security Agency,Harbin 150078,Heilongjiang Province,China)

机构地区：[1]首都医科大学附属北京同仁医院国家药物临床试验机构,北京100730 [2]黑龙江公安厅安康医院,黑龙江哈尔滨150078

出　　处：《中国临床药理学杂志》2020年第16期2497-2500,共4页The Chinese Journal of Clinical Pharmacology

基　　金：国家科技支撑计划基金资助项目(2011BAK04B08)。

摘　　要：目的建立可同时快速测定人毛发样品中苯丙胺、甲基苯丙胺、3,4-亚甲基二氧基苯丙胺和3,4-亚甲基二氧甲基苯丙胺的方法。方法以NaOH溶液水解毛发,经三氟乙酸酐酰化处理,进样气相色谱-质谱联用系统(GC-MS)分析,色谱柱:HP-5 MS(30 m×0.25 mm i.d.×0.25μm),流动相:氦气,流速:1.00 mL·min-1,柱温:80℃维持2 min,以30℃·min-1增加到180℃,再以10℃·min-1增加到210℃,再以30℃·min-1增加到280℃,维持10 min,进样阀、离子源和四级杆温度分别为280℃,230℃和200℃,进样量:1μL,电子轰击电离,用单反应监测模式,定量分析离子分别为m/z 118 (苯丙胺)、m/z 154 (甲基苯丙胺)、m/z 162 (3,4-亚甲基二氧基苯丙胺)、m/z 162 (3,4-亚甲基二氧甲基苯丙胺)、m/z 176(4-苯基丁氨)。结果苯丙胺标准曲线方程为y=3.36e+000x+6.08e-002(r=0.999),线性范围为1.5~150 ng·mg-1;甲基苯丙胺标准曲线方程为y=3.38e+000x+9.35e-002(r=0.999),线性范围为1.5~150 ng·mg-1;3,4-亚甲基二氧基苯丙胺标准曲线方程为y=2.49e+000x+2.44e-002(r=0.998),线性范围为1.5~150 ng·mg-1;3,4-亚甲基二氧甲基苯丙胺标准曲线方程为y=2.90e+000x+6.38e-002(r=0.999),线性范围为1.5~150 ng·mg-1。批内、批间精密度均在1.97%~9.18%,准确度在94.28%~107.78%,提取回收率均大于85.00%,稳定性好。结论本方法样本处理简便,灵敏度高,专属性强,适用于上述四种化合物的毛发样本浓度测定。Objective To develop a rapid method for determining of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, and 3,4-methylenedioxymethamphetamine simultaneously in human hair samples. Methods The hair samples were treated by sodium hydroxide solution, and acylated by trifluoroacetic anhydride, and then determined by gas chromatography-mass spectrometry. The column was HP-5 MS(30 m×0.25 mm i.d. ×0.25 μm), and the mobile phase was helium. The flow rate was 1 mL·min-1, and the column temperature gradient were 80 ℃ for 2 min, increased to 180 ℃ at 30 ℃·min-1, then increased to 210 ℃ at 10 ℃·min-1, then increased to 280 ℃ at 30 ℃·min-1, and maintained for another 10 min. The temperature of the ion source, the quadrupole, and the injector port were 280 ℃, 230 ℃, and 200 ℃, respectively. The injection volume was 1 μL, and the electron impact source was used. The single ion monitoring mode was used to quantitatively analyze the ions as m/z 118(amphetamine),m/z 154(methamphetamine),m/z 162(3,4-methylenedioxyamphetamine),and m/z 162(3,4-methylenedioxymethamphetamine). Results The standard curve of amphetamine was y = 3. 36 e+000 x + 6. 08 e-002(r =0. 999),the linear range was 1. 5-150 ng·mg-1. The standard curve of methamphetamine was y = 3. 38 e+000 x +9. 35 e-002(r = 0. 999), the linear range was 1. 5-150 ng · mg-1. The standard curve of 3,4-methylenedioxyamphetamine was y = 2. 49 e+000 x + 2. 44 e-002(r = 0. 999),the linear range was 1. 5-150 ng·mg-1.And the standard curve of 3,4-methylenedioxymethamphetamine was y = 2. 90 e+000 x + 6. 38 e-002(r = 0. 999),the linear range was 1. 5 ~ 150 ng·mg-1. The intra-day and inter-day precisions were between 1. 97% and 9. 18%.The accuracy was between 94. 28% and 107. 78%,and the average extraction recoveries of the four analytes were greater than 85. 00%,and the stability was good. Conclusion The method was simple,sensitive as well as specific,which can be applied for the determination of Amphetamines of hair samples of drug abusers.

关 键 词：气相色谱-质谱联用 毛发 甲基苯丙胺 成瘾 

分 类 号：R97[医药卫生—药品]