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采用超高效液相色谱-串联质谱法对环境和废水中的个人护理产品和药物进行多类别的测定。

Multi-class determination of personal care products and pharmaceuticals in environmental and wastewater samples by ultra-high performance liquid-chromatography-tandem mass spectrometry.

机构信息

Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellón, Spain.

出版信息

Talanta. 2012 Sep 15;99:1011-23. doi: 10.1016/j.talanta.2012.07.091. Epub 2012 Aug 8.

Abstract

In this work, a multi-class method for the simultaneous determination of 17 emerging contaminants, including pharmaceuticals and personal care products, has been developed. Target analytes were two anti-inflammatories, a lipid regulator agent, two angiotensin II antagonists, two antiepileptic drugs and a diuretic. Among personal care products, four preservatives and five UV filters were included. The method is based on solid-phase extraction (SPE) using Oasis HLB cartridges followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Up to three simultaneous transitions per compound were acquired to assure a reliable identification. A detailed study of the extraction process efficiency and matrix effects was carried out in surface water and effluent wastewater. The use of isotope-labeled internal standards (ILIS) was tested to compensate both potential SPE losses during sample extraction and signal suppression/enhancement observed, especially in EWW. Satisfactory correction in all water samples was only ensured when the own analyte ILIS was used. The use of analogues ILIS was a rather useful approach for correction in the majority of the samples tested when analyte ILIS was unavailable. The method was successfully validated in five different surface water (SW) samples and five effluent wastewater (EWW) samples spiked at two concentration levels (0.05 and 0.5 μg/L in SW; 0.1 and 0.5 μg/L in EWW). The developed method was applied to the analysis of 22 samples (SW and EWW) from the Spanish Mediterranean area and 51 reservoir water samples from Colombia. Personal care products were frequently detected, with the highest concentrations corresponding to benzophenone and benzophenone-4 (samples from Spain), and methylparaben (samples from Colombia). Several pharmaceuticals were detected in the Spanish samples, where irbesartan and valsartan - two Angiotensin II antagonists that are not commonly monitored in the aquatic environment - were the compounds most frequently detected.

摘要

在这项工作中,开发了一种用于同时测定 17 种新兴污染物的多类方法,包括药物和个人护理产品。目标分析物包括两种消炎药、一种脂质调节剂、两种血管紧张素 II 拮抗剂、两种抗癫痫药和一种利尿剂。在个人护理产品中,包括四种防腐剂和五种紫外线过滤器。该方法基于固相萃取(SPE),使用 Oasis HLB 小柱,然后进行超高效液相色谱-串联质谱(UHPLC-MS/MS)分析。每个化合物最多可同时采集三个转换,以确保可靠的鉴定。在地表水和废水处理厂废水中对萃取过程效率和基质效应进行了详细研究。测试了使用同位素标记内标物(ILIS)的方法,以补偿样品萃取过程中的潜在 SPE 损失和信号抑制/增强,特别是在 EWW 中。只有当使用自身分析物的 ILIS 时,才能确保在所有水样中进行令人满意的校正。当无法获得分析物 ILIS 时,使用类似物 ILIS 是一种在大多数测试样本中进行校正的非常有用的方法。该方法在五个不同的地表水(SW)样品和五个废水处理厂废水(EWW)样品中进行了成功验证,在两个浓度水平(SW 为 0.05 和 0.5 μg/L;EWW 为 0.1 和 0.5 μg/L)下进行了加标。该方法应用于西班牙地中海地区 22 个地表水和哥伦比亚 51 个水库水样的分析。经常检测到个人护理产品,浓度最高的是二苯甲酮和二苯甲酮-4(来自西班牙的样品)和对羟基苯甲酸甲酯(来自哥伦比亚的样品)。在西班牙的样品中检测到几种药物,其中厄贝沙坦和缬沙坦——两种在水生环境中不常监测的血管紧张素 II 拮抗剂——是最常检测到的化合物。

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