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

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.

Influence of long-term storage temperatures and sodium fluoride preservation on the stability of synthetic cathinones and dihydro-metabolites in human whole blood

“…From an analytical perspective, given the extreme instability of numerous parent cathinones, specifically those featuring halogenated groups, the detection of these instability products and metabolites in the blood might be useful biomarkers and would greatly increase the detection windows for suspected SCt use. Indeed, dihydro-metabolites continue to be detected in forensic caseworks either in the presence or absence of parent drug [22][23][24][25].…”

Rapid Screening of New Psychoactive Substances Using pDART-QqQ-MS

“…Over the past decade, regulatory challenges and health risk concerns related to NPSs have dramatically risen due to their widespread proliferation. Traditionally, the quantitative confirmation of NPSs in biological matrices has been carried out using hyphenated mass spectrometry with chromatography techniques in forensic laboratories. − These approaches not only provide the sensitivity and accuracy necessary for screening analysis of many NPSs, but they have also led to the publication of methodologies for measuring specific emerging drug classes and a broad spectrum of drugs from different classes.…”

Rapid detection of nine synthetic cathinones in blood and urine by direct analysis in real‐time‐tandem mass spectrometry

“…New psychoactive substances of synthetic cathinone are a kind of controlled drugs with strong excitatory and hallucinogenic effects. [1][2][3] The earliest cathinone designer drugs, methcathinone and 4-methyl methcathinone, were accidentally synthesized by scientists in the 1920s. 4 These two substances were initially used as antidepressantspecific medicines, but gradually flowed into the drug market.…”