A simple and rapid pipette-tip solid-phase extraction (PT-SPE) procedure with derivatization prior to gas chromatography triple quadrupole mass spectrometry analysis is developed for the simultaneous determination of amphetamine (AMP), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA) and 3,4-methylenedioxymethamphetamine (MDMA) in urine samples. The PT-SPE procedure using self-made sorbent could extract drugs within 6 min from 100-μL urine samples, requiring low solvent-consumption (<2.0 mL). Besides, the self-made pipette tip could be reused at least five times. Under optimized conditions, the recoveries of four amphetamines at spiked levels (low, medium and high) ranged from 87.7 to 110.4%, with relative standard deviations < 9.5%. The limit of detections and limit of quantifications for AMP, MA, MDA and MDMA were in the range of 2.52–8.25 ng⋅mL⁻¹ and 8.4–27.5 ng⋅mL⁻¹, respectively. Validation results show that the proposed method is suitable for the quantitation of amphetamines and has been successfully applied in the urine samples of suspected drug abusers.

中文翻译：

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自制移液器提示固相萃取，然后进行GC-MS / MS快速分析尿液中的四种苯丙胺。

建立了一种简单，快速的移液管尖端固相萃取（PT-SPE）方法，在气相色谱三重四极杆质谱分析之前先进行衍生化，可同时测定苯丙胺（AMP），甲基苯丙胺（MA），3,4-亚甲基二氧基苯丙胺（MDA）和3,4-亚甲二氧基甲基苯丙胺（MDMA）尿液样本中。使用自制吸附剂的PT-SPE程序可在6分钟内从100μL尿液样品中提取药物，要求低溶剂消耗量（<2.0 mL）。此外，自制移液器吸头可重复使用至少五次。在优化条件下，四种安非他明在加标水平（低，中和高）下的回收率在87.7％至110.4％之间，相对标准偏差<9.5％。AMP，MA，^-1和8.4-27.5 ng·mL ^-1。验证结果表明，该方法适用于安非他命的定量，并已成功应用于可疑药物滥用者的尿液样品中。