Department of Forensic Medicine, Hjelt Institute, University of Helsinki, Helsinki, Finland.
Ther Drug Monit. 2011 Apr;33(2):257-63. doi: 10.1097/FTD.0b013e318208b693.
A gas chromatography-mass spectrometry (GCMS) procedure was developed for the quantitative analysis of the new designer drug methylenedioxypyrovalerone (MDPV) in urine together with the common stimulants amphetamine, methamphetamine, and methylenedioxymethamphetamine (MDMA). The procedure involved electron ionization (EI) GCMS in the selected ion monitoring (SIM) mode after liquid-liquid extraction with toluene and derivatization with heptafluorobutyric acid anhydride. All MDPV findings were confirmed by positive chemical ionization GCMS in SIM mode. Positive chemical ionization-GCMS allowed the protonated molecule M+H+ m/z 276 to be used as a target ion with 3 abundant fragments as qualifier ions. By electron ionization-GCMS, the limit of quantification (LOQ) for MDPV was 0.02 mg/L; and for amphetamine, methamphetamine, and MDMA, the LOQ was 0.05 mg/L. The method was applied to monitoring urine samples from opioid-dependent patients undergoing opioid substitution treatment. Nine of the 34 urine samples (26%) analyzed were MDPV positive by the GCMS procedure. The positive samples were obtained from 2 female and 7 male patients with a mean age of 31 years. The median (range) MDPV concentration was 0.16 mg/L (0.04-3.9 mg/L) based on the 7 samples for which a numeric value was obtained, whereas the concentration was below the LOQ but above the limit of detection in 2 samples. The method revealed amphetamine in approximately 40% of the cases, and there was no statistical difference between the MDPV-positive and MDPV-negative groups. Urine amphetamine concentrations were on average 10 times higher than those of MDPV. The opioid-dependent patients used MDPV mainly as a substitute for amphetamine, judging from the laboratory findings of this study and the information from our patients.
建立了一种气相色谱-质谱联用（GCMS）方法，用于尿液中新设计药物甲叉二氧吡咯戊酮（MDPV）与常见兴奋剂安非他命、甲基苯丙胺和 3,4-亚甲二氧基甲基苯丙胺（MDMA）的定量分析。该方法涉及电子电离（EI）GCMS 在选择离子监测（SIM）模式下，经甲苯液-液萃取和七氟丁酰基酐衍生化处理。所有 MDPV 检测结果均通过正化学电离 GCMS 在 SIM 模式下得到确认。正化学电离-GCMS 允许将质子化分子 M+H+ m/z 276 用作目标离子，将 3 个丰富的片段用作定性离子。通过电子电离-GCMS，MDPV 的定量限（LOQ）为 0.02mg/L；而对于安非他命、甲基苯丙胺和 MDMA，LOQ 为 0.05mg/L。该方法应用于监测接受阿片类药物替代治疗的阿片类药物依赖患者的尿液样本。通过 GCMS 程序分析的 34 个尿液样本中有 9 个（26%）为 MDPV 阳性。阳性样本来自 2 名女性和 7 名男性患者，平均年龄为 31 岁。根据 7 个可获得数值的样本，中位数（范围）MDPV 浓度为 0.16mg/L（0.04-3.9mg/L），而在 2 个样本中浓度低于 LOQ 但高于检测限。该方法发现大约 40%的情况下存在安非他命，并且 MDPV 阳性组和 MDPV 阴性组之间没有统计学差异。尿液中安非他命的浓度平均是 MDPV 浓度的 10 倍。从本研究的实验室结果和我们患者的信息来看，阿片类药物依赖患者主要将 MDPV 用作安非他命的替代品。
