Rapid Determination of Methamphetamine, Methylenedioxymethamphetamine, Methadone, Ketamine, Cocaine, and New Psychoactive Substances in Urine Samples Using Comprehensive Two-Dimensional Gas Chromatography
<b>Background/Objectives:</b> This study evaluates the applicability of a comprehensive two-dimensional gas chromatography−flame ionisation detection (GC×GC−FID) approach for the simultaneous determination of 12 underivatised psychoactive drugs, including new psychoactive substances, tha...
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2024-11-01
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| Series: | Metabolites |
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| Online Access: | https://www.mdpi.com/2218-1989/14/11/643 |
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| author | Doreen N. B. Chandra Siri Seng Yo Goh Ngee Sing Chong Philip J. Marriott Yong Foo Wong |
| author_facet | Doreen N. B. Chandra Siri Seng Yo Goh Ngee Sing Chong Philip J. Marriott Yong Foo Wong |
| author_sort | Doreen N. B. Chandra Siri |
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| description | <b>Background/Objectives:</b> This study evaluates the applicability of a comprehensive two-dimensional gas chromatography−flame ionisation detection (GC×GC−FID) approach for the simultaneous determination of 12 underivatised psychoactive drugs, including new psychoactive substances, that comprised of amphetamine, methamphetamine, mephedrone, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, α-pyrrolidinovalerophenone, <i>n</i>-ethylpentylone (ephylone), norketamine, ketamine, 3,4-methylenedioxypyrovalerone, methadone, and cocaine. <b>Methods:</b> Separation was effected using a non-polar first dimension (<sup>1</sup>D) and a polar second dimension (<sup>2</sup>D) column, demonstrating an improved separation of drug compounds compared to a polar/non-polar column configuration. Interference-free baseline separation of all psychoactive compounds in a urine matrix was achieved within 8 min. The GC×GC−FID method was validated according to the guidelines defined by Standard Practices for Method Validation in Forensic Toxicology. <b>Results:</b> The calibration curves for the 12 psychoactive drugs were well correlated (r<sup>2</sup> > 0.99) within the concentration ranges of 50–1500 ng mL<sup>−1</sup>. Detection limits of 10–20 ng mL<sup>−1</sup> were obtained, and good repeatability and reproducibility (CV < 11.4%) were attained for retention times and peak areas. Method recoveries for the small-scale solvent extraction procedure ranged from 96.9 to 114.5%, and bias was between −3.1% and 14.5%. <b>Conclusions:</b> The validated approach was successfully applied for the determination of these illicit compounds in spiked urine samples of different concentrations, highlighting its potential for rapid forensic drug screening. |
| format | Article |
| id | doaj-art-03d0f99c3c22466fba76a308c3188f97 |
| institution | Kabale University |
| issn | 2218-1989 |
| language | English |
| publishDate | 2024-11-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Metabolites |
| spelling | doaj-art-03d0f99c3c22466fba76a308c3188f972024-11-26T18:13:16ZengMDPI AGMetabolites2218-19892024-11-01141164310.3390/metabo14110643Rapid Determination of Methamphetamine, Methylenedioxymethamphetamine, Methadone, Ketamine, Cocaine, and New Psychoactive Substances in Urine Samples Using Comprehensive Two-Dimensional Gas ChromatographyDoreen N. B. Chandra Siri0Seng Yo Goh1Ngee Sing Chong2Philip J. Marriott3Yong Foo Wong4Center for Research on Multidimensional Separation Science, School of Chemical Sciences, Universiti Sains Malaysia, USM 11800, Penang, MalaysiaAgilent Technologies Sales (M) Sdn. Bhd., Unit 202 & 203, Level 2, Uptown 2, Jalan SS21/37, Damansara Uptown, Petaling Jaya 47400, Selangor, MalaysiaDepartment of Chemistry, Middle Tennessee State University, Murfreesboro, TN 37132, USAAustralian Centre for Research on Separation Science, School of Chemistry, Monash University, Wellington Road, Clayton Victoria 3800, AustraliaCenter for Research on Multidimensional Separation Science, School of Chemical Sciences, Universiti Sains Malaysia, USM 11800, Penang, Malaysia<b>Background/Objectives:</b> This study evaluates the applicability of a comprehensive two-dimensional gas chromatography−flame ionisation detection (GC×GC−FID) approach for the simultaneous determination of 12 underivatised psychoactive drugs, including new psychoactive substances, that comprised of amphetamine, methamphetamine, mephedrone, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, α-pyrrolidinovalerophenone, <i>n</i>-ethylpentylone (ephylone), norketamine, ketamine, 3,4-methylenedioxypyrovalerone, methadone, and cocaine. <b>Methods:</b> Separation was effected using a non-polar first dimension (<sup>1</sup>D) and a polar second dimension (<sup>2</sup>D) column, demonstrating an improved separation of drug compounds compared to a polar/non-polar column configuration. Interference-free baseline separation of all psychoactive compounds in a urine matrix was achieved within 8 min. The GC×GC−FID method was validated according to the guidelines defined by Standard Practices for Method Validation in Forensic Toxicology. <b>Results:</b> The calibration curves for the 12 psychoactive drugs were well correlated (r<sup>2</sup> > 0.99) within the concentration ranges of 50–1500 ng mL<sup>−1</sup>. Detection limits of 10–20 ng mL<sup>−1</sup> were obtained, and good repeatability and reproducibility (CV < 11.4%) were attained for retention times and peak areas. Method recoveries for the small-scale solvent extraction procedure ranged from 96.9 to 114.5%, and bias was between −3.1% and 14.5%. <b>Conclusions:</b> The validated approach was successfully applied for the determination of these illicit compounds in spiked urine samples of different concentrations, highlighting its potential for rapid forensic drug screening.https://www.mdpi.com/2218-1989/14/11/643new psychoactive substancescomprehensive two-dimensional gas chromatographymethamphetaminemephedroneα-pyrrolidinovalerophenoneecstasy |
| spellingShingle | Doreen N. B. Chandra Siri Seng Yo Goh Ngee Sing Chong Philip J. Marriott Yong Foo Wong Rapid Determination of Methamphetamine, Methylenedioxymethamphetamine, Methadone, Ketamine, Cocaine, and New Psychoactive Substances in Urine Samples Using Comprehensive Two-Dimensional Gas Chromatography Metabolites new psychoactive substances comprehensive two-dimensional gas chromatography methamphetamine mephedrone α-pyrrolidinovalerophenone ecstasy |
| title | Rapid Determination of Methamphetamine, Methylenedioxymethamphetamine, Methadone, Ketamine, Cocaine, and New Psychoactive Substances in Urine Samples Using Comprehensive Two-Dimensional Gas Chromatography |
| title_full | Rapid Determination of Methamphetamine, Methylenedioxymethamphetamine, Methadone, Ketamine, Cocaine, and New Psychoactive Substances in Urine Samples Using Comprehensive Two-Dimensional Gas Chromatography |
| title_fullStr | Rapid Determination of Methamphetamine, Methylenedioxymethamphetamine, Methadone, Ketamine, Cocaine, and New Psychoactive Substances in Urine Samples Using Comprehensive Two-Dimensional Gas Chromatography |
| title_full_unstemmed | Rapid Determination of Methamphetamine, Methylenedioxymethamphetamine, Methadone, Ketamine, Cocaine, and New Psychoactive Substances in Urine Samples Using Comprehensive Two-Dimensional Gas Chromatography |
| title_short | Rapid Determination of Methamphetamine, Methylenedioxymethamphetamine, Methadone, Ketamine, Cocaine, and New Psychoactive Substances in Urine Samples Using Comprehensive Two-Dimensional Gas Chromatography |
| title_sort | rapid determination of methamphetamine methylenedioxymethamphetamine methadone ketamine cocaine and new psychoactive substances in urine samples using comprehensive two dimensional gas chromatography |
| topic | new psychoactive substances comprehensive two-dimensional gas chromatography methamphetamine mephedrone α-pyrrolidinovalerophenone ecstasy |
| url | https://www.mdpi.com/2218-1989/14/11/643 |
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