Choi Hyeyoung, Kim Suncheun, Ahn Suyoun, Chang Hyejin, Lee Sangki, Lee Yongmoon
Daejeon Institute, National Forensic Service , 1524 Yuseongdaero, Yuseong-gu, Daejeon 34054, Republic of Korea; College of Pharmacy, Chungbuk National University, 1 Chungdaero, Seowon-gu, Cheongju, Chungbuk 28356, Republic of Korea.
Drug & Forensic Toxicology Division, National Forensic Service, 10 Ipchunro, Wonjusi, Gangwondo 26460, Republic of Korea.
Forensic Sci Int. 2016 Feb;259:69-76. doi: 10.1016/j.forsciint.2015.12.016. Epub 2015 Dec 23.
Phenylalkylamine derivatives, such as methamphetamine (MA), 3,4-methylenedioxymethamphetamine (MDMA), phentermine, fenfluramine, phendimetrazine, amfepramone, and ketamine, are widely abused recreational or anorectic drugs in Korea, and their abuse has become a serious social problem. Hair is a useful specimen to prove chronic use and liquid chromatography-tandem mass spectrometry (LC-MS/MS) has recently become a more popular tool for hair analysis due to sensitivity and simplicity in sample preparation. In order to overcome limitations of standard reversed-phase column to separate low molecular weight amines, we adopted a multi-mode reversed-phase column, Scherzo SS-C18, which was composed of strong ionic ligands and C18 ligands, and used pH gradient elution to separate seven psychotropic phenylalkylamines and their metabolites. The essential validation parameters including selectivity, LOD, LLOQ, linearity, intra- and inter-assay precision and accuracy, recovery, and the matrix effect were satisfactory. The LODs ranged from 0.1ng/5mg hair (diethylnorephedrine, fenfluramine, ketamine, and MA) to 0.5ng/5mg hair (amfepramone, MDA, phendimetrazine, and phentermine). The LLOQs were 1ng/5mg hair for all analytes. The developed method was successfully applied to determination of phenylalkylamines in authentic hair samples analyzed previously by a routine gas chromatography/mass spectrometry (GC-MS) method. A good correlation was observed between the two methods, with a slope near one.
苯烷基胺衍生物，如甲基苯丙胺（MA）、3,4-亚甲基二氧基甲基苯丙胺（摇头丸）、芬特明、芬氟拉明、苯双甲吗啉、安非拉酮和氯胺酮，在韩国是广泛滥用的娱乐性或食欲抑制性药物，其滥用已成为一个严重的社会问题。毛发是证明长期使用情况的有用样本，液相色谱-串联质谱法（LC-MS/MS）由于样品制备的灵敏度和简便性，最近已成为毛发分析中更受欢迎的工具。为了克服标准反相柱分离低分子量胺类的局限性，我们采用了一种多模式反相柱Scherzo SS-C18，它由强离子配体和C18配体组成，并使用pH梯度洗脱来分离七种精神活性苯烷基胺及其代谢物。包括选择性、检测限（LOD）、定量下限（LLOQ）、线性、批内和批间精密度与准确度、回收率以及基质效应在内的基本验证参数均令人满意。检测限范围为0.1 ng/5mg毛发（二乙去甲麻黄碱、芬氟拉明、氯胺酮和甲基苯丙胺）至0.5 ng/5mg毛发（安非拉酮、3,4-亚甲基二氧基苯丙胺、苯双甲吗啉和芬特明）。所有分析物的定量下限均为1 ng/5mg毛发。所建立的方法成功应用于先前通过常规气相色谱/质谱法（GC-MS）分析的真实毛发样本中苯烷基胺的测定。两种方法之间观察到良好的相关性，斜率接近1。
