Development and validation of a GC-MS method for determination of amphetamine-type stimulants and ketamine in human hair

A solid-phase extraction (SPE) followed by gas chromatography-mass spectrometry (GC-MS) method was developed and validated for determination of seven amphetamine-type stimulants (ATSs) including amphetamine (AM), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphet...

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Main Authors: Tran Viet Hung, Ha Minh Hien, Pham Quoc Chinh, Pham Thi Thu Ha, Nguyen Duc Nhu, Nguyen Duc Tuan
Format: Article
Language:English
Published: Faculty of Pharmacy, Mahidol University 2023-01-01
Series:Pharmaceutical Sciences Asia
Subjects:
Online Access:https://pharmacy.mahidol.ac.th/journal/_files/2023-50-1_4.pdf
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author Tran Viet Hung
Ha Minh Hien
Pham Quoc Chinh
Pham Thi Thu Ha
Nguyen Duc Nhu
Nguyen Duc Tuan
author_facet Tran Viet Hung
Ha Minh Hien
Pham Quoc Chinh
Pham Thi Thu Ha
Nguyen Duc Nhu
Nguyen Duc Tuan
author_sort Tran Viet Hung
collection DOAJ
description A solid-phase extraction (SPE) followed by gas chromatography-mass spectrometry (GC-MS) method was developed and validated for determination of seven amphetamine-type stimulants (ATSs) including amphetamine (AM), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylendioxyethylamphetamine (MDEA), para-methoxyamphetamine (PMA), 4-bromo-2,5- dimethoxyamphetamine (DOB), and ketamine (KET), norketamine (NKT) in human hair. Ten milligrams of human hair was washed by water and methanol followed by soaking in a solution of 1% hydrochloric acid in methanol for 18 hours. The analytes from the methanolic extract were isolated by a SPE procedure before being derivatized using heptafluorobutyric anhydride (HFBA) at 80°C for 40 minutes. The selected ion monitoring (SIM) method was used for the quantification of the derivatized compounds. The linear range was from 0.5-40 ng/mg for all of the analytes with the coefficient of determination (R2)>0.9971. The intra-day and inter-day accuracies were in the range of 93.63-112.40% and 94.70-110.20%, respectively. The intra-day and inter-day precision (RSD%) were in the range of 8.72 and 9.73, respectively. Limit of detection (LOD) and limit of quantitation (LOQ) for each analyte were less than 0.10 and 0.32 ng/mg, respectively. The recoveries were in the range of 75.18-89.30%. The GC-MS was used for the hair analysis on 51 subjects suspected to be ATSs and ketamine user. The average content of all the analytes was in the range of 1.14-12.70 ng/mg. On the basis of these results, the method was proved to be effective for identification and quantitation of
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spelling doaj.art-d73bb044989040de8e3f1b8d20138f8a2023-01-19T12:57:19ZengFaculty of Pharmacy, Mahidol UniversityPharmaceutical Sciences Asia2586-84702023-01-01501243310.29090/psa.2023.01.22.292Development and validation of a GC-MS method for determination of amphetamine-type stimulants and ketamine in human hairTran Viet Hung0Ha Minh Hien1Pham Quoc Chinh2Pham Thi Thu Ha3Nguyen Duc Nhu4Nguyen Duc Tuan5Institute of Drug Quality Control Ho Chi Minh City, Ho Chi Minh City, VietnamInstitute of Drug Quality Control Ho Chi Minh City, Ho Chi Minh City, VietnamNational Institute of Forensic Medicine, Hanoi City, VietnamNational Institute of Forensic Medicine, Hanoi City, VietnamNational Institute of Forensic Medicine, Hanoi City, VietnamFaculty of Pharmacy, University of Medicine and Pharmacy at Ho Chi Minh City, Ho Chi Minh City, VietnamA solid-phase extraction (SPE) followed by gas chromatography-mass spectrometry (GC-MS) method was developed and validated for determination of seven amphetamine-type stimulants (ATSs) including amphetamine (AM), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylendioxyethylamphetamine (MDEA), para-methoxyamphetamine (PMA), 4-bromo-2,5- dimethoxyamphetamine (DOB), and ketamine (KET), norketamine (NKT) in human hair. Ten milligrams of human hair was washed by water and methanol followed by soaking in a solution of 1% hydrochloric acid in methanol for 18 hours. The analytes from the methanolic extract were isolated by a SPE procedure before being derivatized using heptafluorobutyric anhydride (HFBA) at 80°C for 40 minutes. The selected ion monitoring (SIM) method was used for the quantification of the derivatized compounds. The linear range was from 0.5-40 ng/mg for all of the analytes with the coefficient of determination (R2)>0.9971. The intra-day and inter-day accuracies were in the range of 93.63-112.40% and 94.70-110.20%, respectively. The intra-day and inter-day precision (RSD%) were in the range of 8.72 and 9.73, respectively. Limit of detection (LOD) and limit of quantitation (LOQ) for each analyte were less than 0.10 and 0.32 ng/mg, respectively. The recoveries were in the range of 75.18-89.30%. The GC-MS was used for the hair analysis on 51 subjects suspected to be ATSs and ketamine user. The average content of all the analytes was in the range of 1.14-12.70 ng/mg. On the basis of these results, the method was proved to be effective for identification and quantitation ofhttps://pharmacy.mahidol.ac.th/journal/_files/2023-50-1_4.pdfamphetamine-type stimulantsketaminegc-mshair
spellingShingle Tran Viet Hung
Ha Minh Hien
Pham Quoc Chinh
Pham Thi Thu Ha
Nguyen Duc Nhu
Nguyen Duc Tuan
Development and validation of a GC-MS method for determination of amphetamine-type stimulants and ketamine in human hair
Pharmaceutical Sciences Asia
amphetamine-type stimulants
ketamine
gc-ms
hair
title Development and validation of a GC-MS method for determination of amphetamine-type stimulants and ketamine in human hair
title_full Development and validation of a GC-MS method for determination of amphetamine-type stimulants and ketamine in human hair
title_fullStr Development and validation of a GC-MS method for determination of amphetamine-type stimulants and ketamine in human hair
title_full_unstemmed Development and validation of a GC-MS method for determination of amphetamine-type stimulants and ketamine in human hair
title_short Development and validation of a GC-MS method for determination of amphetamine-type stimulants and ketamine in human hair
title_sort development and validation of a gc ms method for determination of amphetamine type stimulants and ketamine in human hair
topic amphetamine-type stimulants
ketamine
gc-ms
hair
url https://pharmacy.mahidol.ac.th/journal/_files/2023-50-1_4.pdf
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