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使用液相色谱-串联质谱法同时测定毛发中的哌醋甲酯和利他林酸。

Simultaneous determination of methylphenidate and ritalinic acid in hair using LC-MS/MS.

作者信息

Jang Moonhee, Kim Jihyun, Shin Ilchung, Kang Seojin, Choi Hyeyoung, Yang Wonkyung

机构信息

National Forensic Service, 139 Jiyang-ro, Yangcheon-Gu, Seoul 158-707, Republic of Korea.

National Forensic Service, 139 Jiyang-ro, Yangcheon-Gu, Seoul 158-707, Republic of Korea.

出版信息

Forensic Sci Int. 2019 Jan;294:183-188. doi: 10.1016/j.forsciint.2018.11.021. Epub 2018 Nov 29.

DOI:10.1016/j.forsciint.2018.11.021
PMID:30530155
Abstract

Methylphenidate (MPH) is one of the most commonly prescribed stimulants for attention deficit hyperactivity disorder and its abuse is on the rise with its growing availability. Some analytical methods have been reported for the detection of MPH in hair. However, the concentration range of MPH as well as its metabolite, ritalinic acid (RA) in the hair of MPH abuse cases has not been reported. In this study, a sensitive and reliable liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous determination of MPH and RA in hair. Sample preparation was carried out by a simple methanol extraction using 10mg of hair. Limits of detection for MPH and RA in hair were 0.5pg/mg and 1pg/mg, respectively, and the limits of quantification (LOQs) were 1pg/mg for both the analytes. Validation results showed good linearity in the range of 1-100pg/mg with acceptable precision and accuracy. The developed method was applied to real hair samples obtained from ten drug users who obtained MPH illegally without a prescription. MPH concentrations in the hair samples ranged from 1.0pg/mg to 265.0pg/mg, and RA was present at concentrations <LOQ-76.3pg/mg. In this study, hair analysis and background findings revealed that most subjects have abused illicit substances (methamphetamine, Δ-tetrahydrocannabinol, zolpidem etc.) other than MPH. The low picogram range of LODs for MPH and RA in hair was achieved with the present method and the results from real sample analysis would provide useful information related to MPH abuse under forensic settings.

摘要

哌甲酯(MPH)是治疗注意力缺陷多动障碍最常用的处方兴奋剂之一,随着其可获得性的增加,其滥用情况也在上升。已经报道了一些检测头发中MPH的分析方法。然而,MPH滥用案例中头发中MPH及其代谢物利他林酸(RA)的浓度范围尚未见报道。本研究建立并验证了一种灵敏可靠的液相色谱-串联质谱法,用于同时测定头发中的MPH和RA。样品制备采用简单的甲醇萃取法,使用10mg头发。头发中MPH和RA的检测限分别为0.5pg/mg和1pg/mg,两种分析物的定量限(LOQ)均为1pg/mg。验证结果表明,在1-100pg/mg范围内具有良好的线性,精密度和准确度均可接受。所建立的方法应用于从10名非法获取无处方MPH的吸毒者处获得的实际头发样本。头发样本中MPH的浓度范围为1.0pg/mg至265.0pg/mg,RA的浓度<LOQ-76.3pg/mg。在本研究中,头发分析和背景调查结果显示,大多数受试者除了滥用MPH外,还滥用了其他非法物质(甲基苯丙胺、Δ-四氢大麻酚、唑吡坦等)。本方法实现了头发中MPH和RA的低皮克级检测限,实际样品分析结果将为法医环境下与MPH滥用相关的研究提供有用信息。

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