Application of Homogeneous Liquid–Liquid Microextraction With Switchable Hydrophilicity Solvents to the Determination of MDMA, MDA and NBOMes in Postmortem Blood Samples

Abstract

Synthetic drugs for recreational purposes are in constant evolution and their consumption promote a significant increase in intoxication cases, resulting in damaging public health. The development of analytical methodologies to confirm the consumption of illicit drugs in biological matrices are required for control of these substances. This work exploited the development of an extraction method based on homogenous liquid-liquid microextraction with switchable hydrophilicity solvent as extraction phase (SHS-HLLME) for the determination of the synthetic drugs MDMA, MDA and NBOMes (25B, 25C and 25I) in postmortem blood, followed by liquid chromatography coupled to mass spectrometry in tandem (LC–MS/MS). The optimized sample preparation conditions consisted of using 250 µL of ZnSO4 10% and 50 µL of NaOH 1 mol/L in the protein precipitation step; N,N-dimethylcyclohexylamine (DMCHA) was used as switchable hydrophilicity solvent (SHS), 650 μL of a mixture of SHS:HCl 6 mol/L (1:1 v/v), 500 μL of whole blood, 500 μL of NaOH 10 mol/L and 1 min of extraction time. The proposed method was validated, providing determination coefficients higher than 0.99 for all analytes; LOD and LOQ ranged from 0.1 to 10 ng/mL; intra-run precision from 2.16 to 9.19%; inter-run precision from 2.39 to 9.59%; bias from 93.57 to 115.71%; and matrix effects from 28.94 to 51.54%. The developed method was successfully applied to four authentic postmortem blood samples from synthetic drugs users, and it was found to be reliable with good selectivity.

Green chemistry: Developments and perspectives for sample treatment in forensic methodologies

“…SHS‐HLLME was further employed for the determination of MDMA, MDA, and NBOMes in postmortem blood samples with detection by liquid chromatography–tandem mass spectrometry. LOD and LOQs were between 0.1 and 1 ng/mL and four real samples were analyzed, being positive for MDA and MDMA with concentrations ranging from 31.76 to 61.60 ng/mL and 6.91 to 68.20 ng/mL, respectively (Scheid et al, 2022).…”