Department of Experimental and Clinical Toxicology, Institute of Experimental and Clinical Pharmacology and Toxicology, Center for Molecular Signaling (PZMS), Saarland University, Homburg, Germany.
Drug Test Anal. 2024 Sep;16(9):893-902. doi: 10.1002/dta.3608. Epub 2023 Nov 27.
Sewage-based epidemiology using influent wastewater is used to estimate the consumption trends of (illicit) drugs over a short or long period of time in a subpopulation. The current study aimed to develop two separate methods for the quantitative analysis of selected drugs of abuse (DOA) and cognitive enhancers in influent wastewater using reversed-phase (RP) or hydrophilic interaction liquid chromatography (HILIC) coupled to high-resolution tandem mass spectrometry (LC-HRMS/MS). The performance of RP and HILIC column was evaluated. A simple solid phase extraction was used for sample preparation. Short runtimes of 10 and 15 min on the RP and the HILIC column, respectively, allowed sufficient throughput. A six-point calibration was used for quantification with calibration ranges between 10 and 100 ng/L for all analytes except for benzoylecgonine (BZE, 30-300 ng/L). Method validation was performed according to ICH guideline M10. Analytes such as amphetamine (AMPH), BZE, cocaethylene (CE), cocaine (COC), ethyl sulfate, 4-hydroxy-3-methoxymethamphetamine, 3,4-methylenedioxymethamphetamine (MDMA), methamphetamine, methylphenidate (MPH), and ritalinic acid (RA) were included in method development and validation. Two different column types were necessary for sufficient chromatographic resolution. The analytical setup allowed detection of all other analytes at concentration levels between 1 ng/L for methylphenidate to 10 ng/L for amphetamine. A method for the detection and quantification of DOA, cognitive enhancers, and their biomarkers in wastewater was successfully developed and validated. Moreover, six proof-of-concept samples were analyzed in which AMPH, BZE, COC, MDMA, MPH, and RA were identified and further quantified.
基于污水的流行病学使用进水废水来估计亚人群在短或长时间内（非法）药物的消费趋势。本研究旨在开发两种单独的方法，用于使用反相（RP）或亲水相互作用液相色谱（HILIC）结合高分辨串联质谱（LC-HRMS/MS）定量分析选定的滥用药物（DOA）和认知增强剂在进水废水中。评估了 RP 和 HILIC 柱的性能。简单的固相萃取用于样品制备。RP 和 HILIC 柱的短运行时间分别为 10 和 15 分钟，允许足够的通量。使用六点校准进行定量，所有分析物的校准范围为 10 至 100 ng/L，除苯甲酰古柯碱（BZE）外为 30-300 ng/L。方法验证按照 ICH 指南 M10 进行。分析物如苯丙胺（AMPH）、BZE、可卡因乙基酯（CE）、可卡因（COC）、乙基硫酸盐、4-羟基-3-甲氧基甲卡西酮、3,4-亚甲基二氧甲基苯丙胺（MDMA）、甲基苯丙胺、哌醋甲酯（MPH）和利他林酸（RA）均包含在方法开发和验证中。需要两种不同的柱类型才能实现足够的色谱分辨率。该分析设置允许在 1ng/L 到 10ng/L 之间的浓度水平检测到所有其他分析物，从哌醋甲酯的甲基苯丙胺到 10ng/L。成功开发并验证了一种用于检测和定量废水中 DOA、认知增强剂及其生物标志物的方法。此外，还分析了六个概念验证样本，其中鉴定并进一步定量了 AMPH、BZE、COC、MDMA、MPH 和 RA。
