GC-MS和LC-MS/MS法测定毛发中的6种苯丙胺类药物

    The Determination of 6 Amphetamine Drugs in Hair Samples by GC-MS and LC-MS/MS

    • 摘要: 建立毛发样本中6种苯丙胺类药物的GC-MS和LC-MS/MS分析检测方法。选择合适的人体毛发,浸泡在药物-二甲基亚砜溶液中制备含6种苯丙胺类药物的毛发样本,采用单因素变量法优化样品前处理过程,利用GC-MS和LC-MS/MS法对制备的毛发样本进行定量分析。以甲基苯丙胺-D5为内标,采用工作曲线法进行定量分析。实验结果显示,制备的毛发样本中6种苯丙胺类药物的最佳前处理方法为:提取溶剂0.01 mol·L−1 HCl,液料比100:1(mL·g−1),提取温度40 ℃,提取时间50 min。GC-MS中,6种苯丙胺类药物在0.5~5.0 ng·mg−1浓度范围内线性关系良好,r2>0.999,检测限为0.04~0.08 ng·mg−1,回收率≥85.46%,RSDs≤ 3.6%(n=9);LC-MS/MS中,6种苯丙胺类药物在0.06~0.50 ng·mg−1浓度范围内线性关系良好,r2>0.999,检测限低至0.05~5.0 pg·mg−1,回收率在86.50%~111.9%范围内,RSDs≤ 4.2%(n=9)。这两种方法应用于毛发中苯丙胺类药物的检测,灵敏度高、准确度好、专属性强,可作为毛发中苯丙胺类药物基体标准物质的定值方法,用于标准物质的研制,应用于法医滥用药物检测和实验室质量控制领域。

       

      Abstract: A method was developed for the analytical determination of six amphetamine drugs in hair samples by GC-MS and LC-MS/MS. The hair samples were prepared by immersing in the drug-dimethyl sulfoxide solution including target analytes. The sample pretreatment process was optimized using the one-way variable method, and the prepared hair samples were quantified using GC-MS and LC-MS/MS methods. The working curve method was used for quantitative analysis with methamphetamine-D5 as the internal standard. The results showed that the optimal pretreatment methods for the six amphetamine drugs in the prepared hair samples were: 0.01 mol·L−1 HCl, liquid-material ratio 100:1 (mL·g−1), extraction temperature 40 ℃, extraction time 50 min. In GC-MS, the linear range of 6 amphetamine drugs was 0.5 ~ 5.0 ng·mg−1, r2>0.999. The detection limits of the method were 0.04~0.08 ng·mg−1, and the recovery rates were greater than 85.46%, RSDs≤3.6% (n=9). In LC-MS/MS, the 6 amphetamine drugs showed a good linear relationship within the concentration range of 0.06~0.50 ng·mg−1, r2>0.999. The detection limits were 0.05~5.0 pg·mg−1and the recovery of appended contrast in the blank sample ranged from 86.50% to 111.9%, RSDs≤4.2% (n=9). The established methods were used for the detection of amphetamine drugs in human hair, with high sensitivity, good accuracy, and strong specificity. These two methods can be used as the certification method of the reference material of the amphetamine drug in human hair, which could be applied for drug abuse testing and laboratory quality control in the forensic field.

       

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