HS-SPME-GC/MS法检测尿液及毛发中苯丙胺类毒品

目的采用顶空固相微萃取（HS-SPME）、GC/MS分析方法,对生物样品中苯丙胺（AM）、甲基苯丙胺（MAM）、3,4-亚甲二氧基苯丙胺（MDA）和3,4-亚甲二氧基甲基苯丙胺（MDMA）4种苯丙胺类毒品进行定性定量分析。方法在碱性和饱和盐处理状态下,采用100μm聚二甲基硅氧烷（PDMS）萃取纤维,于顶空瓶中进行生物样品AM、MAM、MDA、MDMA 4种毒品萃取,以2-甲基苯乙胺为内标,经气-质联用选择离子检测（GC/MS/SIM）模式进行定性定量分析。对HS-SPME条件优化,对方法的精密度、准确度和检出限进行测定。结果 AM、MAM、MDA、MDMA 4种毒品尿液中的最低检出限为5ng/mL,毛发中的最低检出限为0.5ng/mg。尿液中线性关系范围为0.05μg/mL~5μg/mL,r〉0.991,回收率为82%~108%,RSD为2.6%~6.1%（n=5）;毛发中线性关系范围为5ng/mg~500ng/mg,r〉0.992,回收率为80%~113%,RSD（%）为1.4%~6.8%（n=5）。结论 HS-SPME-GC/MS各项定量参数符合分析要求。该方法简单、灵活、经济、快速、无溶剂,适用于生物检材中该类毒品的分析。

Application of headspace solid-phase microextraction and gas chromatography-mass spectrometry in determination of amphetamines in urine and hair samples

Objective A method was developed for qualitative and quantitative analyses of amphetamine（ AM）, methamphetamine（ MAM）, 3, 4-methylenedioxyamphetamine（ MDA） and 3, 4-methylenedioxymethamphetamine（ MDMA） by headspace solid-phase microextraction and gas chromatographymass spectrometry（ HS-SPME-GC / MS）. Methods Alkalized and saturated with sodium chloride prior to SPME,the analytes were absorbed onto 100 μm polydimethylsiloxane（ PDMS） fiber. With methylphenethylamine used as an internal standard,the analytes were determined by gas chromatography-mass spectrometry with selected ion monitoring（ GC / MS / SIM）. The conditions for HS-SPME were optimized and the precision,accuracy and limit of detection（ LOD） of the method were determined. Results The LOD, recovery,RSD% of the method were 5ng / mL,82% ~ 108%,2. 6% ~ 6. 1%（ n = 5） and 0. 5ng / mg,80% ~ 113%,1. 4% ~ 6. 8%（ n = 5） for urine and hair samples,respectively. The linear calibration curves were obtained in concentration ranges of 0. 05 ~ 5μg / mL（ r ＆gt; 0. 991） for urine samples,and 5 ~ 500ng / mg（ r ＆gt; 0. 992） for hair samples. Conclusion The HS-SPME-GC / MS method could be applied for analyses of amphetamines in biological samples,as it is simple,flexible,economic,fast and solvent-free.