China State Institute of Pharmaceutical Industry, State Key Laboratory of New Drug and Pharmaceutical Process, Shanghai 200040, China.
Shanghai Key Laboratory of Crime Scene Evidence, Shanghai Institute of Forensic Science, Shanghai 200083, China.
Anal Methods. 2021 Nov 4;13(42):5048-5055. doi: 10.1039/d1ay01280k.
For the rapid quantitation of three synthetic cathinones, namely 1-(4-chlorophenyl)-2-(1-pyrrolidinyl)pentan-1-one (4-Cl-α-PVP), 1-(4-methylphenyl)-2-(methylamino)pentan-1-one (4-MPD), and 1-(5,6,7,8-tetrahydronaphthalen-2-yl)-2-(1-pyrrolidinyl)pentan-1-one (β-TH-naphyrone), in urine, a new method was established using magnetic dispersive solid-phase extraction (MDSPE) combined with direct analysis in real time and high-resolution mass spectrometry (DART-HRMS). Methcathinone-D3 and proadifen (SKF525A) were used as the internal standards. Hydrophobic magnetic adsorbents were used and consisted of hydrophobic functional group (divinylbenzene) and hydrophilic functional group (vinylpyrrolidone) at a ratio of 3 : 1, and NaHPO//NaOH buffer (0.2 M, pH 7) was used in MDSPE. Detection was conducted by DART-HRMS in less than 1 min. For 4-Cl-α-PVP, 4-MPD and β-TH-Naphyrone, the limits of detection were 0.1 ng mL, 0.05 ng mL and 0.1 ng mL, and the linear ranges were 0.5-100 ng mL, 0.2-100 ng mL and 0.2-100 ng mL, respectively. The correlation coefficients were all greater than 0.99. The precision and deviation of accuracy were all within ±15%, and the stability of the samples was high under various conditions. The method was successfully applied to detect 4-Cl-α-PVP, 4-MPD and β-TH-naphyrone in rat urine after subcutaneous administration. In summary, a fast and convenient detection method was established, providing new and effective technical support for the rapid quantitation of three synthetic cathinones (4-Cl-α-PVP, 4-MPD and β-TH-Naphyrone) for forensic purposes.
为了快速定量检测三种合成卡西酮,即 1-(4-氯苯基)-2-(1-吡咯烷基)戊-1-酮(4-Cl-α-PVP)、1-(4-甲基苯基)-2-(甲基氨基)戊-1-酮(4-MPD)和 1-(5,6,7,8-四氢萘-2-基)-2-(1-吡咯烷基)戊-1-酮(β-TH-naphyrone),本研究建立了一种新的尿液分析方法,该方法结合了磁分散固相萃取(MDSPE)和实时直接分析高分辨质谱(DART-HRMS)。Methcathinone-D3 和 proadifen(SKF525A)被用作内标。所使用的疏水磁性吸附剂由疏水性官能团(二乙烯基苯)和亲水性官能团(乙烯基吡咯烷酮)以 3:1 的比例组成,在 MDSPE 中使用 NaHPO//NaOH 缓冲液(0.2 M,pH 7)。通过 DART-HRMS 在不到 1 分钟的时间内进行检测。对于 4-Cl-α-PVP、4-MPD 和 β-TH-Naphyrone,检测限分别为 0.1 ng mL、0.05 ng mL 和 0.1 ng mL,线性范围分别为 0.5-100 ng mL、0.2-100 ng mL 和 0.2-100 ng mL,相关系数均大于 0.99。精密度和准确度偏差均在±15%以内,且在各种条件下样品稳定性较高。该方法成功应用于皮下给予大鼠尿液中 4-Cl-α-PVP、4-MPD 和 β-TH-naphyrone 的检测。综上所述,建立了一种快速便捷的检测方法,为法医目的快速定量检测三种合成卡西酮(4-Cl-α-PVP、4-MPD 和 β-TH-Naphyrone)提供了新的有效技术支持。