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Simultaneous Determination of Amphetamine-Related New Psychoactive Substances in Urine by Gas Chromatography-Mass Spectrometry.
J Anal Toxicol. 2018 Nov 01; 42(9):605-616.JA

Abstract

Despite the efforts to prevent the spread of new psychoactive substances (NPS) such as synthetic amphetamine derivatives, it is apparent that newer types of NPS are still emerging on the market in recent years. Due to high potential for their abuse, reliable analytical methods are required to determine these substances in biological samples. The objective of this study was to develop and validate the gas chromatography-mass spectrometric (GC-MS) method for the simultaneous determination of 13 amphetamine-related NPS (amphetamine; AP, 4-fluoroamphetamine; 4FA, methamphamine; MA, 4-fluoromethamphetamine; 4FMA, 4-chloroamphetamine; 4CA, para-methoxyamphetamine; PMA, 4-chloromethamphetamine; 4CMA, 6-(2-aminopropyl)benzofuran; 6APB, 4-methylenedioxyamphetamine; MDA, para-methoxymethamphetamine; PMMA, 6-(2-methylaminopropyl)benzofuran; 6MAPB, 3,4-methylenedioxymethamphetamine; MDMA, 5,6-methylenedioxy-2-aminoindane; MDAI) in urine. The analytes were extracted at pH 7.4 by liquid-liquid extraction prior to their trifluoroacetyl derivatives and then analyzed by GC-MS. The validation parameters included selectivity, linearity, lower limits of quantification (LLOQ), intra and interday precision and accuracy, recovery and stability. The linear ranges were 2-100 ng/mL for AP, 4FA, 4FMA, 4CA, PMA, 6APB, MDA, and MDAI, 2-250 ng/mL for 4CMA, PMMA, and 6MAPB and 25-1,000 ng/mL for MA and MDMA, with acceptable coefficients of determination (r2 > 0.9963). The intra and interday precision were within 11.9 and 12.5%, while the intra and interday accuracies ranged from -10.6% to 13.0% and -11.0% to 6.8% for the nominal concentration at all studied levels, respectively. The LLOQs for each analyte were 2.0-25 ng/mL. The recoveries ranged from 69.3% to 96.4%. The short- and long-term variations of the analytes in urine were lower than 8.5 and 12.7%, indicating that the analytes are stable at least for 16 h at room temperature and for 7 days at 4°C, respectively. The applicability of the method was examined by analyzing urine samples from drug abusers and was determined to be effective for detecting multiple drug use.

Authors+Show Affiliations

Office of Forensic Science Planning, Supreme Prosecutors' Office, Seoul, Republic of Korea.Forensic Genetics & Chemistry Division, Supreme Prosecutors' Office, Seoul, Republic of Korea.Forensic Genetics & Chemistry Division, Supreme Prosecutors' Office, Seoul, Republic of Korea.Forensic Genetics & Chemistry Division, Supreme Prosecutors' Office, Seoul, Republic of Korea.

Pub Type(s)

Journal Article

Language

eng

PubMed ID

29982540

Citation

Kim, Jin Young, et al. "Simultaneous Determination of Amphetamine-Related New Psychoactive Substances in Urine By Gas Chromatography-Mass Spectrometry." Journal of Analytical Toxicology, vol. 42, no. 9, 2018, pp. 605-616.
Kim JY, Suh S, Park J, et al. Simultaneous Determination of Amphetamine-Related New Psychoactive Substances in Urine by Gas Chromatography-Mass Spectrometry. J Anal Toxicol. 2018;42(9):605-616.
Kim, J. Y., Suh, S., Park, J., & In, M. K. (2018). Simultaneous Determination of Amphetamine-Related New Psychoactive Substances in Urine by Gas Chromatography-Mass Spectrometry. Journal of Analytical Toxicology, 42(9), 605-616. https://doi.org/10.1093/jat/bky037
Kim JY, et al. Simultaneous Determination of Amphetamine-Related New Psychoactive Substances in Urine By Gas Chromatography-Mass Spectrometry. J Anal Toxicol. 2018 Nov 1;42(9):605-616. PubMed PMID: 29982540.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous Determination of Amphetamine-Related New Psychoactive Substances in Urine by Gas Chromatography-Mass Spectrometry. AU - Kim,Jin Young, AU - Suh,Sunglll, AU - Park,Jaehyeong, AU - In,Moon Kyo, PY - 2018/02/26/received PY - 2018/05/28/accepted PY - 2018/7/10/pubmed PY - 2019/2/14/medline PY - 2018/7/9/entrez SP - 605 EP - 616 JF - Journal of analytical toxicology JO - J Anal Toxicol VL - 42 IS - 9 N2 - Despite the efforts to prevent the spread of new psychoactive substances (NPS) such as synthetic amphetamine derivatives, it is apparent that newer types of NPS are still emerging on the market in recent years. Due to high potential for their abuse, reliable analytical methods are required to determine these substances in biological samples. The objective of this study was to develop and validate the gas chromatography-mass spectrometric (GC-MS) method for the simultaneous determination of 13 amphetamine-related NPS (amphetamine; AP, 4-fluoroamphetamine; 4FA, methamphamine; MA, 4-fluoromethamphetamine; 4FMA, 4-chloroamphetamine; 4CA, para-methoxyamphetamine; PMA, 4-chloromethamphetamine; 4CMA, 6-(2-aminopropyl)benzofuran; 6APB, 4-methylenedioxyamphetamine; MDA, para-methoxymethamphetamine; PMMA, 6-(2-methylaminopropyl)benzofuran; 6MAPB, 3,4-methylenedioxymethamphetamine; MDMA, 5,6-methylenedioxy-2-aminoindane; MDAI) in urine. The analytes were extracted at pH 7.4 by liquid-liquid extraction prior to their trifluoroacetyl derivatives and then analyzed by GC-MS. The validation parameters included selectivity, linearity, lower limits of quantification (LLOQ), intra and interday precision and accuracy, recovery and stability. The linear ranges were 2-100 ng/mL for AP, 4FA, 4FMA, 4CA, PMA, 6APB, MDA, and MDAI, 2-250 ng/mL for 4CMA, PMMA, and 6MAPB and 25-1,000 ng/mL for MA and MDMA, with acceptable coefficients of determination (r2 > 0.9963). The intra and interday precision were within 11.9 and 12.5%, while the intra and interday accuracies ranged from -10.6% to 13.0% and -11.0% to 6.8% for the nominal concentration at all studied levels, respectively. The LLOQs for each analyte were 2.0-25 ng/mL. The recoveries ranged from 69.3% to 96.4%. The short- and long-term variations of the analytes in urine were lower than 8.5 and 12.7%, indicating that the analytes are stable at least for 16 h at room temperature and for 7 days at 4°C, respectively. The applicability of the method was examined by analyzing urine samples from drug abusers and was determined to be effective for detecting multiple drug use. SN - 1945-2403 UR - https://www.unboundmedicine.com/medline/citation/29982540/Simultaneous_Determination_of_Amphetamine_Related_New_Psychoactive_Substances_in_Urine_by_Gas_Chromatography_Mass_Spectrometry_ L2 - https://academic.oup.com/jat/article-lookup/doi/10.1093/jat/bky037 DB - PRIME DP - Unbound Medicine ER -