毛发中甲基苯丙胺、苯丙胺、6-单乙酰吗啡及吗啡的检测阈值评估
Evaluation of the cut-off value of methamphetamine,amphetamine,6-monoacetylmorphine, and morphine in hair
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摘要: 建立并优化快速检测甲基苯丙胺、苯丙胺、6-单乙酰吗啡及吗啡在毛发中含量的超高效液相色谱-质谱（UPLC-MS/MS）方法，对吸毒者与毒品实验室技术人员毛发中目标物的浓度进行考察并进行阈值评估。将清洗后的毛发样品经甲醇-水（7∶3）在3 000 r/min条件下研磨提取100 s后调节进样体积为甲醇-水（1∶1）使用UPLC-MS/MS分析。色谱柱为Waters Acquity BEH C18（2.1 mm × 100 mm，1.7 μm），流动相为5 mmol/L甲酸铵-0.1%甲酸水溶液及乙腈，0.4 mL/min梯度洗脱。质谱采用ESI+离子源，MRM多反应监测，测定4种目标物的定性离子对和定量离子对。优化后的方法定量限低，提取率较优化前更高。各目标物在0.01 ~ 5 ng/mg（除苯丙胺为0.01 ~ 4 ng/mg）范围内线性关系良好（R2 ≥ 0.999 6），定量限均为0.01 ng/mg，检出限范围为0.001 ~ 0.008 ng/mg；准确度、精密度基质效应和回收率均符合方法学要求。根据接受者操作特征（ROC）曲线、Youden指数、执法成本和执法力度等综合考量，得出4种目标物的参考阈值为甲基苯丙胺 ≥ 0.1 ng/mg；苯丙胺 ≥ 0.025 ng/mg； 6-单乙酰吗啡 ≥ 0.05 ng/mg； 吗啡 ≥ 0.05 ng/mg。本实验建立的方法可快速、高效、准确地测定甲基苯丙胺、苯丙胺、6-单乙酰吗啡及吗啡的含量。本研究为公安系统今后制定涉毒人员毛发样品检测规范的检测阈值提供了参考。
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关键词:
- 毒品 /
- 毛发检测 /
- 前处理优化 /
- 检测阈值评估 /
- 超高效液相色谱-质谱联用技术
Abstract: A rapid determination of methamphetamine, amphetamine, 6-monoacetylmorphine, and morphine in hair samples by UPLC-MS/MS was established and optimized.The concentration of target compounds in the hair of drug abusers and drug laboratory technicians was investigated and the cut-off value was evaluated.After cleaned hair was extracted by grinding with methanol-water (7∶3) at 3 000 r/min for 100 s, the final solution after adjusting the volume to methanol-water (1∶1) was analyzed by UPLC-MS/MS.The analytes were gradient eluted on a Waters Acquity BEH C18 (2.1 mm × 100 mm, 1.7 μm) column with 5 mmol/L ammonium formate-0.1% formic acid aqueous solution and acetonitrile as mobile phase at a flow rate of 0.4 mL/min. The ESI+ ion source and multiple reaction monitoring (MRM) were used to select the qualitative and quantitative ion pairs of the four target compounds. All analytes showed good linearity (R2 ≥ 0.999 6) in the range of 0.01-5 ng/mg (except amphetamine in 0.01-4 ng/mg), limit of the quantitation was 0.01 ng/mg, and the limit of detection was 0.001-0.008 ng/mg.The accuracy, precision, matrix effect, and recovery all met the requirements of biological sample methodology.According to the comprehensive consideration of the receiver operating characteristic (ROC) curve, Youden index, law enforcement cost and intensity, the reference cut-off values were methamphetamine ≥ 0.1 ng/mg; amphetamine ≥ 0.025 ng/mg; 6-monoacetylmorphine ≥ 0.05 ng/mg; morphine ≥ 0.05 ng/mg.The method established in our research can quickly and accurately detect the contents of methamphetamine, amphetamine, 6-monoacetylmorphine, and morphine in hair.This study provides some reference for the public security system to make more rational cut-off values in the norm of drug-related personnel hair samples detection in the future.-
Keywords:
- drug /
- hair testing /
- pretreatment optimization /
- cut-off value evaluation /
- UPLC-MS/MS
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