Hong Wei-Yin, Ko Ya-Chun, Lin Mei-Chih, Wang Po-Yu, Chen Yu-Pen, Chiueh Lih-Ching, Shih Daniel Yang-Chih, Chou Hsiu-Kuan, Cheng Hwei-Fang
Food and Drug Administration, Ministry of Health and Welfare, Taipei, Taiwan.
Food and Drug Administration, Ministry of Health and Welfare, Taipei, Taiwan
J Anal Toxicol. 2016 Jan-Feb;40(1):12-6. doi: 10.1093/jat/bkv108. Epub 2015 Sep 25.
In recent years, the abuse of synthetic cathinones has increased considerably. This study proposes a method, based on gas chromatography/mass spectrometry (GC-MS), to analyze and quantify six synthetic cathinones in urine samples: mephedrone (4-MMC), methylone (bk-MDMA), butylone, ethylone, pentylone and methylenedioxypyrovalerone (MDPV). In our procedure, the urine samples undergo solid-phase extraction (SPE) and derivatization prior to injection into the GC-MS device. Separation is performed using a HP-5MS capillary column. The use of selective ion monitoring (SIM mode) makes it is good sensitivity in this method, and the entire analysis process is within 18 min. In addition, the proposed method maintains linearity in the calibration curve from 50 to 2,000 ng/mL (r(2) > 0.995). The limit of detection of this method is 5 ng/mL, with the exception of MDPV (20 ng/mL); the limit of quantification is 20 ng/mL, with the exception of MDPV (50 ng/mL). In testing, the extraction performance of SPE was between 82.34 and 104.46%. Precision and accuracy results were satisfactory <15%. The proposed method was applied to six real urine samples, one of which was found to contain 4-MMC and bk-MDMA. Our results demonstrate the efficacy of the proposed method in the identification of synthetic cathinones in urine, with regard to the limits of detection and quantification. This method is highly repeatable and accurate.
近年来，合成卡西酮的滥用现象显著增加。本研究提出了一种基于气相色谱/质谱联用（GC-MS）的方法，用于分析和定量尿液样本中的六种合成卡西酮：甲麻黄碱（4-MMC）、亚甲基二氧甲基苯丙胺（bk-MDMA）、丁酮、乙酮、戊酮和亚甲基二氧吡咯戊酮（MDPV）。在我们的实验过程中，尿液样本在注入GC-MS设备之前要经过固相萃取（SPE）和衍生化处理。使用HP-5MS毛细管柱进行分离。采用选择性离子监测（SIM模式）使得该方法具有良好的灵敏度，整个分析过程在18分钟内完成。此外，所提出的方法在校准曲线50至2000 ng/mL范围内保持线性（r(2) > 0.995）。该方法的检测限为5 ng/mL，但MDPV除外（20 ng/mL）；定量限为20 ng/mL，但MDPV除外（50 ng/mL）。在测试中，SPE的萃取性能在82.34%至104.46%之间。精密度和准确度结果令人满意，<15%。所提出的方法应用于六个实际尿液样本，其中一个被发现含有4-MMC和bk-MDMA。我们的结果证明了所提出的方法在尿液中合成卡西酮鉴定方面在检测限和定量限方面的有效性。该方法具有高度的可重复性和准确性。
