Simultaneous determination of 10 new psychoactive piperazine derivatives in urine using ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction combined with gas chromatography-tandem mass spectrometry.

Abstract

With the rapid development of synthetic drugs, novel piperazine derivatives, as an increasingly important class of new psychoactive substances (NPS), have attracted global attention owing to their increasing demand in the illicit drug market. In this study, ten piperazine derivatives were analyzed in urine samples after pre-treatment with ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction (UA-LDS-DLLME) combined with gas chromatography-tandem mass spectrometry (GC-MS/MS). This simple approach involved the use of urine samples (1mL) adjusted to pH 12, which was added to 100 µL of n-hexane and subjected to ultrasonication for 3min to completely disperse the sample in the n-hexane solution. The resulting turbid suspension was centrifuged at 10,000rpm for 3min, and the supernatant was extracted and analyzed using GC-MS/MS. Under the optimized conditions presented in this study, the linear relationship between the analytes was good within 10-1500ng/mL, and the correlation coefficient (r) was between .9914 and .9983. The limit of detection (LOD) was 0.3-2ng/mL (S/N=3), and the lower limit of quantification (LLOQ) was 10ng/mL (S/N=10) with the recovery of the analytes of interest from the spiked samples being 76.3%-93.3%. This method has been used to analyze real-world samples; our study shows that the UA-LDS-DLLME approach can be used for rapid analysis while consuming minimal solvent for the simultaneous determination of a range of analytes. This method has the potential for use in clinical analyses and forensic toxicology.