Mohamed Khaled M, Bakdash Abdulsallam
The Department of Forensic Chemistry, The College of Forensic Sciences, Naif Arab University for Security Sciences, Riyadh, Saudi Arabia.
Anal Chem Insights. 2017 Aug 24;12:1177390117727533. doi: 10.1177/1177390117727533. eCollection 2017.
The heptafluorobutyric anhydride (HFBA), pentafluoropropionic anhydride (PFPA), and trifluoroacetic anhydride (TFAA) are compared as derivatizing reagents to use as the optimal method for the analysis of 10 amphetamines and cathinones in oral fluid. The target compounds were amphetamine (AMP), methamphetamine (MA), 4-methylamphetamine, 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxy--ethylamphetamine (MDEA), cathinone (CAT), methcathinone, mephedrone, and ephedrine. Amphetamine-D, MA-D, MDA-D, MDMA-D, and MDEA-D use as internal standards (IS). The analytes and IS were extracted from 0.5 mL of oral fluid by ethyl acetate in the presence of NaOH (0.1 N) as the base and then the dried extracts were derivatized with HFBA, PFPA, or TFAA at 70°C for 30 minutes. The limits of quantification based on signal-to-noise ratios ≥10 were ranged between 2.5 and 10 ng/mL. The calibration graphs were linear in the range of 5 or 10 to 1000 ng/mL for all analytes. Based on sensitivity, the PFPA is proved to be the best for derivatization of the target compounds prior to gas chromatography-mass spectrometry analysis.
比较了七氟丁酸酐（HFBA）、五氟丙酸酐（PFPA）和三氟乙酸酐（TFAA）作为衍生试剂，以确定其作为分析口腔液中10种苯丙胺类和卡西酮类药物的最佳方法。目标化合物为苯丙胺（AMP）、甲基苯丙胺（MA）、4-甲基苯丙胺、3,4-亚甲基二氧基苯丙胺（MDA）、3,4-亚甲基二氧基甲基苯丙胺（MDMA）、3,4-亚甲基二氧基乙基苯丙胺（MDEA）、卡西酮（CAT）、甲基卡西酮、甲氧麻黄酮和麻黄碱。使用苯丙胺-D、MA-D、MDA-D、MDMA-D和MDEA-D作为内标（IS）。在0.1 N NaOH作为碱的存在下，用乙酸乙酯从0.5 mL口腔液中提取分析物和内标，然后将干燥的提取物在70°C下用HFBA、PFPA或TFAA衍生化30分钟。基于信噪比≥10的定量限在2.5至10 ng/mL之间。所有分析物的校准曲线在5或10至1000 ng/mL范围内呈线性。基于灵敏度，证明PFPA是在气相色谱-质谱分析之前对目标化合物进行衍生化的最佳试剂。
