Quantitative determination of amphetamine-type stimulants in sewage and urine by hybrid monolithic column solid-phase microextraction coupled with UPLC-QTRAP MS/MS

• Published in: Talanta (Oxford) 2024-03, Vol.269, p.125437-125437, Article 125437
• Main Authors: Zhao, Ling-yu, Qin, Mian, Wu, Guo-ping, Zhou, Yi-tong, Zhu, Jia-xuan, Peng, Hao
• Format: Article
• Language: English
• Subjects: Amphetamine; Hybrid monolithic column; Sewage; Solid-phase microextraction; UPLC-QTRAP MS/MS; Urine
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2023.125437

A needle-solid-phase microextraction (SPME) method based on hybrid monolithic column (HMC) was proposed for simultaneous separation and extraction of seven amphetamine-type stimulants (ATSs) (amphetamine, methamphetamine, cathinone, methcathinone, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, and 3,4-methylenedioxyethylamphetamine), combining with ultra-performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometer (UPLC-QTRAP MS/MS). Thiol functionalized HMC (T-HMC) showed high extraction efficiency and excellent elution results towards target analytes, among three kinds of single/bi-functionalized HMCs. Various parameters of SPME operation and analytical performance were investigated systematically. The adsorption mechanism of T-HMC to ATSs was also discussed and explained as a mixed mode of electrostatic and hydrophobic interactions. Under the optimum experimental conditions, the proposed T-HMC needle-SPME-UPLC-QTRAP MS/MS method was rapid and convenient with good accuracy, low sample consumption, high sensitivity and strong anti-interference ability. This method was successfully applied to quantitative determination of seven trace ATSs in complex sewage and urine samples. In view of abundant types of HMCs, the needle-SPME based on functional HMC also had the potential to selectively separating and enriching other tract new psychoactive substances in complex matrices, and could provide a reliable tool for drug monitoring, especially in applications for forensic analysis and drug abuse. [Display omitted] •Quantitative determination of trace amphetamine-type stimulants in sewage and urine.•A needle-SPME method based on hybrid monolithic column was proposed.•Three functionalized hybrid monolithic columns were investigated and compared.•Thiol hybrid monolithic column showed excellent extraction and elution efficiency.•The adsorption mechanism was explained as electrostatic and hydrophobic interactions.