Rapid Determination of Methamphetamine, Methylenedioxymethamphetamine, Methadone, Ketamine, Cocaine, and New Psychoactive Substances in Urine Samples Using Comprehensive Two-Dimensional Gas Chromatography

Abstract

Background/Objectives: 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, n-ethylpentylone (ephylone), norketamine, ketamine, 3,4-methylenedioxypyrovalerone, methadone, and cocaine. Methods: Separation was effected using a non-polar first dimension (1D) and a polar second dimension (2D) 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. Results: The calibration curves for the 12 psychoactive drugs were well correlated (r2 > 0.99) within the concentration ranges of 50–1500 ng mL−1. Detection limits of 10–20 ng mL−1 were obtained, and good repeatability and reproducibility (CV Conclusions: 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.

Keywords

• new psychoactive substances
• comprehensive two-dimensional gas chromatography
• methamphetamine
• mephedrone
• α-pyrrolidinovalerophenone
• ecstasy