Determination of amphetamine-type stimulants (ATSs) and synthetic cathinones in urine using solid phase micro-extraction fibre tips and gas chromatography-mass spectrometry,Analytical Methods

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Determination of amphetamine-type stimulants (ATSs) and synthetic cathinones in urine using solid phase micro-extraction fibre tips and gas chromatography-mass spectrometry
Analytical Methods ( IF 2.7 ) Pub Date : 2018-03-06 00:00:00 , DOI: 10.1039/c8ay00041g
Khalid A. Alsenedi _{1,

2,

3,

4,

5} , Calum Morrison _{1,

2,

3,

4,

5}

Affiliation

In recent years, an increasing number of stimulant drugs and new psychoactive substances (NPSs) have caused concern in scientific communities and therefore innovative methods to extract compounds from complex biological samples are required. This work is aimed at developing and validating a clean, convenient and straightforward extraction procedure with microliter amounts of organic solvent using Solid Phase Micro-Extraction tips (SPME tips) and analysis using Gas Chromatography-Mass Spectrometry (GC-MS) in human urine samples. Another aim is to evaluate three different types of SPME fibre tips C18, C18-SCX (mixed mode) and PDMS-DVB. The quantification method examined the different classes of stimulant compounds included Amphetamine-Type Stimulants (ATSs) (amphetamine, methamphetamine, para-methoxyamphetamine (PMA), and (±)-3,4-methylenedioxymethamphetamine (MDMA)) and synthetic cathinones (mephedrone, buphedrine (buphedrone ephedrine metabolite), 4-methylephedrine (mephedrone metabolite), and pentylone). The method was developed with respect to several areas of the experimental design including pH, ionic strength, addition of salts, vial dimensions, analytes and derivatisation, type of solvents, solvent volume, extraction and desorption time, agitation speeds in the extraction and desorption steps and matrix volume. The optimised method was validated for eight compounds using the SPME PDMS/DVB fibre tips with satisfactory linearity and selectivity ranging between 50 and 2000 ng mL⁻¹, and limits of detection (LODs) and low limits of quantification (LLOQs) ranging between (5–25) and (25–100) ng mL⁻¹ respectively. Within-run and between-run accuracy and precision were <15%. The method was applied to real human urine samples indicating its suitability for common stimulant drugs and provided clean chromatograms with no interfering peaks. The assessment of green analytical chemistry for the method used was discussed and compared with Solid Phase Extraction (SPE). According to the results obtained we recommend the method for use in routine laboratories carrying out drug/forensic analysis for confirmation tests of the studied compounds.

中文翻译：

固相微萃取纤维尖端和气相色谱-质谱法测定尿液中的苯丙胺类兴奋剂（ATS）和合成卡西酮

近年来，越来越多的刺激药物和新型精神活性物质（NPS）引起了科学界的关注，因此需要创新的方法从复杂的生物样品中提取化合物。这项工作旨在开发和验证使用固相微萃取针尖（SPME针尖）和使用气相色谱-质谱法（GC-MS）对人尿液样品进行分析的微升有机溶剂的清洁，便捷和直接提取程序。另一个目标是评估三种不同类型的SPME光纤头C18，C18-SCX（混合模式）和PDMS-DVB。定量方法检查了不同类别的兴奋剂化合物，包括苯丙胺类兴奋剂（ATS）（苯丙胺，甲基苯丙胺，对苯二酚-甲氧基苯丙胺（PMA）和（±）-3,4-亚甲基二氧基甲基苯丙胺（MDMA））和合成的卡西酮（甲氧麻黄酮，甲氧麻黄碱（甲氧麻黄碱麻黄碱代谢物），4-甲氧麻黄碱（甲氧麻黄碱代谢物）和戊酮。该方法是针对实验设计的几个领域开发的，包括pH值，离子强度，盐的添加，小瓶尺寸，分析物和衍生化，溶剂类型，溶剂体积，萃取和解吸时间，萃取和解吸步骤中的搅拌速度和基质体积。使用SPME PDMS / DVB光纤头对优化的方法进行了八种化合物的验证，其线性和选择性介于50到2000 ng mL ^-1之间，检测限（LOD）和定量下限（LLOQ）分别在（5–25）ngng ^-1和（25–100）ng mL ^-1之间。批内和批间准确性和精密度均<15％。该方法已应用于实际的人类尿液样品，表明它适用于常见的刺激性药物，并提供了干净的色谱图，没有干扰峰。讨论了对所用方法的绿色分析化学评估，并将其与固相萃取（SPE）进行了比较。根据获得的结果，我们推荐用于常规实验室进行药物/法医分析的方法，以对所研究的化合物进行确认测试。

更新日期：2018-03-06

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