Rapid SPE-LC–MS/MS Method for Detection and Quantification of MDMB-4en-PINACA and ADB-BUTINACA in Blood and Urine Using Solid-Phase Extraction

Çağılcı O. C., OCAK M., Ocak Ü. T.

Chromatographia, cilt.88, sa.11-12, ss.953-961, 2025 (SCI-Expanded, Scopus) identifier identifier

  • Yayın Türü: Makale / Tam Makale
  • Cilt numarası: 88 Sayı: 11-12
  • Basım Tarihi: 2025
  • Doi Numarası: 10.1007/s10337-025-04451-2
  • Dergi Adı: Chromatographia
  • Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus, Chemical Abstracts Core, Chimica, Compendex, EMBASE, DIALNET
  • Sayfa Sayıları: ss.953-961
  • Anahtar Kelimeler: ADB-BUTINACA, Blood, Detection method, MDMB-4en-PINACA, Solid-phase extraction, SPE-LC–MS/MS, Synthetic cannabinoid, Urine
  • Karadeniz Teknik Üniversitesi Adresli: Evet

Özet

MDMB-4en-PINACA (methyl-3,3-dimethyl-2-(1-(pent-4en-1-yl)-1H-indazole-3-carbox-amido)-butanoate) and ADB-BUTINACA (N-[1-amino-3,3-dimethyl-1-oxobutan-2-yl]-1-butyl-1H-indazole-3-carboxamide) are among the recently encountered synthetic cannabinoids (SCs). MDMB-4en-PINACA was first identified in 2017, while ADB-BUTINACA emerged in 2019. These substances were initially detected by the Trabzon Council of Forensic Medicine at the end of 2023 and have since become frequently observed in regional blood and urine analyses. Although some studies have addressed the detection of these compounds in biological matrices, existing sample preparation procedures are often time-consuming and labor-intensive. This study aimed to develop and validate a rapid and reliable LC–MS/MS method for the quantification of MDMB-4en-PINACA and ADB-BUTINACA using solid-phase extraction (SPE) for sample preparation. Among the three SPE columns evaluated, OASIS HLB demonstrated the lowest matrix effect and was selected as the most suitable under the tested conditions. The method showed good sensitivity and clear chromatographic separation of both analytes. The calibration curves were linear in the range of 1.0–50 ng/mL. The limits of detection (LOD) for ADB-BUTINACA were 0.60 ng/mL in blood and 0.63 ng/mL in urine, while for MDMB-4en-PINACA, the LODs were 1.29 ng/mL and 1.33 ng/mL, respectively. No metabolites of MDMB-4en-PINACA or ADB-BUTINACA were analyzed in this study due to the unavailability of certified reference standards. Selectivity was evaluated with respect to the parent compounds and potential endogenous interferences in the biological matrices. The validated method was successfully applied to 20 real-case samples obtained from the Trabzon Council of Forensic Medicine. These findings demonstrate that the developed SPE-LC–MS/MS method is suitable for routine forensic toxicology applications involving MDMB-4en-PINACA and ADB-BUTINACA.