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-2,5dimethoxyamphetamine (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 (R 2 )>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 above mentioned nine narcotics.
A cross sectional study was conducted at National Institute of forensic medicine of Vietnam on characteristics of deaths in custody through forensic medicine examination. Out of 125 deaths in custody were autopsied by the forensic medical specialist. The majority of the male sex is 94%. The deaths accounts for the largest number of people age group 41-50 (25.6%). Pathological causes accounts for 82.4% (103 cases), in which, tuberculosis accounts for the highest rate (19.42%), cardiovascular disease (17.48%), severe pneumonia (15.53%), multi-organ dysfunction syndrome and multi disease accounted for (15.53%), cerebrovascular accident (9.71%), cancer and HIV/AIDS (5.83%), cirrhosis ascites (4.85%), encephalitis, meningitis and gastrointestinal bleeding all accounted for (2.91%). Deaths are related to violent impacts, accounting for 14.4% (22 cases), of which hanging accounts for the most, others cause as trauma, drugs shock, poisoning, electricity shock with a small rate.
This article develops a combined solid phase extraction (SPE) and gas chromatography – mass spectrometry (GC-MS) procedure for determining amphetamine-type stimulants Amphetamine (AM) and Methamphetamine (MA) in human hair. Hair samples were incubated in methanol containing 1% hydrochloric acid in 18 hours and then subjected to SPE. The obtained extracts were evaporated to dryness, derivatized with heptafluorobutyric anhydride (HFBA) at 70 °C for 30 minutes prior to GC–MS analysis. Gas chromatography mass spectrometry was run on HP5-MS column (30 m × 0.25 mm × 0.25 µm) with detector MS 5975C. Experimentally, the proposed method proved sensitive, simple and time-saving, but quite accurate with a low limit of detection (LOD = 0.05ng/mg) and quantitation (LOQ = 0.15ng/mg). Keywords: SPE, GC – MS, hair samples, amphetamine, methamphetamine. References [1] Ming-Ren Fuh, Ti-Yu Wu and Tzuen-Yeuan Lin, Determination of amphetamine and methamphetamine in urine by solid phase extraction and ion-pair liquid chromatography–electrospray–tandem mass spectrometry Talanta, 68 (3) (2006), 987-991. https://doi.org/10.1016/j.talanta.2005.06.057[2] Naresh C. Jain, Thomas C. Sneath, and Robert D. Budd, Rapid Gas-Chomatographic Determination of Amphetamine and Methamphetamine in urine, Clinical Chemistry, 20 (11) (1974) 1460-1462. https://doi.org/10.1093/clinchem/20.11.1460.[3] Dong-liang Lin, Rea-Ming Yin, Ray H. Liu, Gas Chromatography-Mass Spectrometry (GC-MS) Analysis of Amphetamine, Methamphetamine, 3,4-Methylenedioxy- amphetamine and 3,4-Methylenedioxymethamphetamine in Human Hair and Hair Sections, Journal of Food and Drug Analysis, 13(2) (2005) 193-200. https://doi.org/10.38212/2224-6614.2526[4] María Jesús Tabernero, Maria Linda Felli, Ana María Bermejo, Marcello Chiarotti, Determination of ketamine and amphetamines in hair by LC/MS/MS, Anal Bioanal Chem, 395(2009), 2547–2557. https://doi.org/10.1007/s00216-009-3163-4.[5] D.V. Doan, D.Q. Huy, N.D. Hue, T.M. Tri, Determination of methamphetamine in urine samples by gas chromatography mass spectrometry combined with solid phase extraction technique, Journal of Science and Technology 47 (6) (2009) 53-58 (in Vietnamese).[6] Rodger L. Foltz, Allison F. Fentiman, Ruth B. Foltz, GC/MS Assays for Abused Drugs in Body Fluids, National Institute on Drug Abuse, Maryland, 1980.[7] AOAC, Appendix F: Guidelines for Standard Method Performance Requirements, AOAC official methods of analysis, Maryland, 2016.[8] Eunyoung Han, Martin P. Paulus, Marc Wittmann, Heesun Chung, Joon myong Song, Hair analysis and self-report of methamphetamine use by methamphetamine dependent individuals, Journal of Chromatography B, 879 (2011) 541–547. https://doi.org/10.1016/j.jchromb.2011.01.002.
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