Abstract:
An automated microextraction by packed sorbent followed by liquid chromatography-tandem mass spectrometry (MEPS-LC-MS/MS) method was developed for the determination of four endocrine disruptors-parabens, benzophenones, and synthetic phenolic antioxidants-in wastewater samples. The method utilizes a lab-made repackable MEPS device and a multi-syringe robotic platform that provides flexibility to test small quantities (2 mg) of multiple extraction phases and enables high-throughput capabilities for efficient method development. The overall performance of the MEPS procedure, including the investigation of influencing variables and the optimization of operational parameters for the robotic platform, was comprehensively studied through univariate and multivariate experiments. Under optimized conditions, the target analytes were effectively extracted from a small sample volume of 1.5 mL, with competitive detectability and analytical confidence. The limits of detection ranged from 0.15 to 0.30 ng L-1, and the intra-day and inter-day relative standard deviations were between 3 and 21%. The method\'s applicability was successfully demonstrated by determining methylparaben, propylparaben, butylated hydroxyanisole, and oxybenzone in wastewater samples collected from the São Carlos (SP, Brazil) river. Overall, the developed method proved to be a fast, sensitive, reliable, and environmentally friendly analytical tool for water quality monitoring.
摘要:
建立了一种通过填充吸附剂然后进行液相色谱-串联质谱(MEPS-LC-MS/MS)的自动微萃取方法,用于测定四种内分泌干扰物-对羟基苯甲酸酯。二苯甲酮,和合成的酚类抗氧化剂-在废水样品中。该方法利用实验室制造的可重新包装的MEPS装置和多注射器机器人平台,该平台提供了测试少量(2mg)多个提取阶段的灵活性,并实现了高效方法开发的高通量能力。MEPS程序的整体性能,包括影响变量的调查和机器人平台运行参数的优化,通过单变量和多变量实验进行了全面研究。在优化条件下,从1.5mL的少量样品中有效提取目标分析物,具有竞争力的可检测性和分析信心。检测限范围为0.15至0.30ngL-1,日内和日间相对标准偏差在3%至21%之间。通过测定对羟基苯甲酸甲酯成功证明了该方法的适用性,对羟基苯甲酸丙酯,丁基羟基茴香醚,和从圣卡洛斯收集的废水样品中的氧苯酮(SP,巴西)河。总的来说,开发的方法被证明是一种快速的,敏感,可靠,和环保的水质监测分析工具。