Determination of synthetic cathinone α-pyrrolidinovalero-phenone and its metabolite in urine using solid-phase extraction and gas chromatography–mass spectrometry

Kai Wen Cheng, Chien Ming Hsieh, Huei Wen Chen, Pin Chieh Chi, Da Peng Yang, She Hung Chan, Ju Yu Chen, Hsaio Lin Hwa, Cheng Chung Fang, Te I. Weng, Pai Shan Chen

Research output: Contribution to journalArticle

Abstract

Rationale: The presence of α-pyrrolidinovalerophenone (α-PVP) and its metabolites in urine is evidence of the administration of α-PVP. A toxicological challenge is that the metabolites of α-PVP exhibit amphoteric properties, which make them unsuitable for detection using gas chromatography–mass spectrometry (GC/MS). In the study reported, proper derivatization and sample extraction were essential for improving the sensitivity for GC/MS analysis. Methods: An automated solid-phase extraction (SPE) method has been developed and optimized. The derivatization efficiency was tested using longer reaction time and the addition of polar pyridine into a mixture of N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) with 1% trimethylchlorosilane. Method validation, including linearity, limit of detection, precision, accuracy, and recovery, was evaluated using automatic SPE and GC/MS. Results: The results suggested that adding pyridine to BSTFA (1:1, v/v) significantly improved derivatization efficiency and precision. After optimization, the linear range was from 25 to 1000 ng mL−1 with R2 > 0.9950. The limit of detection was 5 ng mL−1 for α-PVP and 25 ng mL−1 for OH-α-PVP. The recovery for SPE was over 88%. The inter-day and intra-day precisions were less than 15%. A forensic sample has been found containing α-PVP (67.3 ng mL−1) and OH-α-PVP (560.2 ng mL−1). Conclusions: This study is the first to validate an auto-SPE-GC/MS method for the quantification and qualification of α-PVP and OH-α-PVP in urine. We have successfully improved the derivatization efficiency and developed a sensitive and semi-automatic approach. This approach is desirable for the detection of synthetic cathinone at trace levels in biological samples.

Original languageEnglish
Article numbere8579
JournalRapid Communications in Mass Spectrometry
Volume34
Issue numberS1
DOIs
Publication statusPublished - Apr 1 2020

ASJC Scopus subject areas

  • Analytical Chemistry
  • Spectroscopy
  • Organic Chemistry

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