气相色谱-质谱联用分析口服液中苯丙胺相关药物3种衍生化方法的比较

Analytical Chemistry Insights Pub Date : 2017-08-24 eCollection Date: 2017-01-01 DOI:10.1177/1177390117727533
Khaled M Mohamed, Abdulsallam Bakdash
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引用次数: 13

摘要

以七氟丁酸酐(HFBA)、五氟丙酸酐(PFPA)和三氟乙酸酐(TFAA)为衍生化试剂,对口服液中10种安非他明和卡西酮的分析方法进行了比较。目标化合物为安非他明(AMP)、甲基苯丙胺(MA)、4-甲基安非他明、3,4-亚甲基二氧基安非他明(MDA)、3,4-亚甲基二氧基- n -乙基安非他明(MDMA)、3,4-亚甲基二氧基- n -乙基安非他明(MDEA)、卡西酮(CAT)、甲卡西酮、甲氧基酮和麻黄碱。安非他明- d5、MA-D5、MDA-D5、MDMA-D5和MDEA-D5用作内标(IS)。在NaOH (0.1 N)存在下,用乙酸乙酯从0.5 mL口服液中提取分析物和IS,然后用HFBA、PFPA或TFAA在70°C下衍生30分钟。信噪比≥10的定量限在2.5 ~ 10 ng/mL之间。所有分析物的校准图在5或10至1000 ng/mL范围内呈线性。基于灵敏度,PFPA被证明是气相色谱-质谱分析前目标化合物衍生化的最佳方法。
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Comparison of 3 Derivatization Methods for the Analysis of Amphetamine-Related Drugs in Oral Fluid by Gas Chromatography-Mass Spectrometry.

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-N-ethylamphetamine (MDEA), cathinone (CAT), methcathinone, mephedrone, and ephedrine. Amphetamine-D5, MA-D5, MDA-D5, MDMA-D5, and MDEA-D5 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.

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