Validated green phenyl reversed-phase LC method using ethanol to determine MDMA in seized ecstasy tablets
Leandro Oka Duarte, Bruno Ferreira, Gabriela R. Silva, Antônio José Ipólito, Marcelo Firmino de Oliveira
Abstract
3,4-Methylenedioxymethamphetamine (MDMA) is a popular illicit drug. Given its adverse effects, the growing abuse of MDMA worldwide, and the need for forensic chemistry methods that minimize environmental issues, here we report a green approach for quantitative MDMA analysis in ecstasy tablets based on phenyl reversed-phase liquid-chromatography coupled to a diode-array detector. Water with 0.1% formic acid (pH adjusted to 5.00 with ammonium hydroxide) and ethanol (85:15, v/v) was employed as the mobile phase. The method showed good analytical performance in terms of linearity (0.0031–0.1 mg mL−1, R2 = 0.9998), precision (1.26–7.79%), accuracy (93.5–107.7%), and recovery (96.6–100.6%). The limits of detection and quantification were 0.0007 and 0.0031 mg mL−1, respectively. The MDMA purity ranged from 14.7% to 35.1% (m/m). Additionally, greenness assessment using an eco-scale metric provided a score. The results indicated that the simultaneous use of ethanol and phenyl-bonded phase provides high selectivity and is suitable and reliable for routine analysis of seized ecstasy samples, constituting a powerful alternative to expensive mass spectrometer-based liquid chromatography and common reversed-phase columns.