title: Development of an analytical method for simultaneous detection of psychotropic phenylalkylamines in hair by LC-MS/MS with a multi-mode reversed-phase column using pH gradient elution.
abstract: 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.
authors.affiliation: 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. Electronic address: hychoi22@korea.kr.
authors.forename: Hyeyoung
authors.initials: H
authors.lastname: Choi
authors.affiliation: Drug & Forensic Toxicology Division, National Forensic Service, 10 Ipchunro, Wonjusi, Gangwondo 26460, Republic of Korea. Electronic address: nisi@korea.kr.
authors.forename: Suncheun
authors.initials: S
authors.lastname: Kim
authors.affiliation: Daejeon Institute, National Forensic Service , 1524 Yuseongdaero, Yuseong-gu, Daejeon 34054, Republic of Korea. Electronic address: aphroditesu@korea.kr.
authors.forename: Suyoun
authors.initials: S
authors.lastname: Ahn
authors.affiliation: Daejeon Institute, National Forensic Service , 1524 Yuseongdaero, Yuseong-gu, Daejeon 34054, Republic of Korea. Electronic address: changhj@korea.kr.
authors.forename: Hyejin
authors.initials: H
authors.lastname: Chang
authors.affiliation: Daejeon Institute, National Forensic Service , 1524 Yuseongdaero, Yuseong-gu, Daejeon 34054, Republic of Korea. Electronic address: skleedoc@korea.kr.
authors.forename: Sangki
authors.initials: S
authors.lastname: Lee
authors.affiliation: College of Pharmacy, Chungbuk National University, 1 Chungdaero, Seowon-gu, Cheongju, Chungbuk 28356, Republic of Korea. Electronic address: ymleefn@cbnu.ac.kr.
authors.forename: Yongmoon
authors.initials: Y
authors.lastname: Lee
mesh_terms: D000328:Adult; D002853:Chromatography, Liquid / Q000379:methods*; D056148:Chromatography, Reverse-Phase / Q000379:methods*; D005260:Female; D006197:Hair / Q000737:chemistry*; D006801:Humans; D006863:Hydrogen-Ion Concentration; D008297:Male; D008875:Middle Aged; D010627:Phenethylamines / Q000032:analysis*; D011619:Psychotropic Drugs / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D055815:Young Adult
chemical_list: D010627:Phenethylamines; D011619:Psychotropic Drugs
keywords: LC-MS/MS; Multi-mode reversed phase column; Psychotropic phenylalkylamines; pH gradient