Multi-parameter evaluation of sample preparation strategies for LC–MS/MS determination of classical drugs and synthetic cannabinoids in a surrogate aqueous matrix
Microchemical Journal, cilt.228, 2026 (SCI-Expanded, Scopus)
- Yayın Türü: Makale / Tam Makale
- Cilt numarası: 228
- Basım Tarihi: 2026
- Doi Numarası: 10.1016/j.microc.2026.118960
- Dergi Adı: Microchemical Journal
- Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus, BIOSIS, Chemical Abstracts Core, Chimica, Index Islamicus, Academic Search Ultimate (EBSCO), Engineering Source (EBSCO)
- Anahtar Kelimeler: Illicit drugs, LC–MS/MS, New psychoactive substances, Solid-phase extraction (SPE), Wastewater analysis
- Ankara Üniversitesi Adresli: Evet
Özet
The analytical determination of trace-level psychoactive drugs in aqueous matrices requires robust sample preparation strategies. This study presents a comprehensive, multi-parameter evaluation of sample preparation parameters for liquid chromatography–tandem mass spectrometry (LC–MS/MS) analysis of psychoactive drugs. To assess recovery-related performance and matrix-related implications without confounding environmental variables, an optimized surrogate matrix workflow was established. The recoveries and analytical behaviors of fifteen target compounds including amphetamine, methamphetamine, morphine, 6-monoacetylmorphine, codeine, MDMA, MDA, cocaine, benzoylecgonine, nicotine, cotinine, THC-COOH, and synthetic cannabinoids (4-fluoro MDMB-BUTICA,ADB-BUTINACA,MDMB-4en-PINACA) were evaluated. Reconstitution of evaporated eluates in 100% acetonitrile optimization consistently yielded recoveries for classical drugs within the acceptable range, although the overall differences among the tested reconstitution formulations were not statistically significant. Bond Elut SPE cartridges generally provided higher recoveries for classical drugs than HLB-based cartridges, except for methamphetamine and benzoylecgonine, with an average recovery increase of 17.2%. For the challenging synthetic cannabinoid class, mixed-mode polymeric Oasis MCX cartridges demonstrated the most reproducible and stable recovery profile (ranging from 81.2% to 89.0%), while final reconstitution in 100% acetonitrile enhanced their average recovery to 91.6% compared to the initial aqueous-organic mixtures. In contrast, final microfiltration prior to LC–MS/MS injection induced critical, analyte-dependent losses for classical compounds, decreasing the mean recovery significantly from 98.9% down to 80.9%, with severe retention observed particularly for cocaine, benzoylecgonine, cotinine, and THC-COOH. Ultimately, these findings establish a baseline method-optimization guide under controlled surrogate conditions, highlighting that while pre-analysis filtration and solvent selection significantly dictate extraction yields, full validation across authentic wastewater matrices with varying suspended solid loads remains mandatory prior to routine epidemiological scale-up.