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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.
Forensic Sci Int. 2016 Feb; 259:69-76.FS

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+Show Affiliations

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.Drug & Forensic Toxicology Division, National Forensic Service, 10 Ipchunro, Wonjusi, Gangwondo 26460, Republic of Korea. Electronic address: nisi@korea.kr.Daejeon Institute, National Forensic Service , 1524 Yuseongdaero, Yuseong-gu, Daejeon 34054, Republic of Korea. Electronic address: aphroditesu@korea.kr.Daejeon Institute, National Forensic Service , 1524 Yuseongdaero, Yuseong-gu, Daejeon 34054, Republic of Korea. Electronic address: changhj@korea.kr.Daejeon Institute, National Forensic Service , 1524 Yuseongdaero, Yuseong-gu, Daejeon 34054, Republic of Korea. Electronic address: skleedoc@korea.kr.College of Pharmacy, Chungbuk National University, 1 Chungdaero, Seowon-gu, Cheongju, Chungbuk 28356, Republic of Korea. Electronic address: ymleefn@cbnu.ac.kr.

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

26760907

Citation

Choi, Hyeyoung, et al. "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." Forensic Science International, vol. 259, 2016, pp. 69-76.
Choi H, Kim S, Ahn S, et al. 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. Forensic Sci Int. 2016;259:69-76.
Choi, H., Kim, S., Ahn, S., Chang, H., Lee, S., & Lee, Y. (2016). 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. Forensic Science International, 259, 69-76. https://doi.org/10.1016/j.forsciint.2015.12.016
Choi H, et al. 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. Forensic Sci Int. 2016;259:69-76. PubMed PMID: 26760907.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - 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. AU - Choi,Hyeyoung, AU - Kim,Suncheun, AU - Ahn,Suyoun, AU - Chang,Hyejin, AU - Lee,Sangki, AU - Lee,Yongmoon, Y1 - 2015/12/23/ PY - 2015/09/08/received PY - 2015/11/23/revised PY - 2015/12/11/accepted PY - 2016/1/14/entrez PY - 2016/1/14/pubmed PY - 2016/11/10/medline KW - LC-MS/MS KW - Multi-mode reversed phase column KW - Psychotropic phenylalkylamines KW - pH gradient SP - 69 EP - 76 JF - Forensic science international JO - Forensic Sci Int VL - 259 N2 - 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. SN - 1872-6283 UR - https://www.unboundmedicine.com/medline/citation/26760907/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_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0379-0738(15)00506-X DB - PRIME DP - Unbound Medicine ER -