Departamento de Química Analítica, Escuela Politécnica Superior, Universidad de Sevilla, C/ Virgen de África, 7, 41011, Sevilla, Spain.
Anal Bioanal Chem. 2019 Oct;411(25):6625-6635. doi: 10.1007/s00216-019-02035-2. Epub 2019 Jul 27.
The presence of parabens and pharmaceuticals on the aquatic environment has been widely evaluated in the last years. Nevertheless, there is scarce information about the occurrence of their metabolites and/or degradation products in spite of the fact that they can be more toxic or more concentrated than their parent compounds. One of the main drawbacks for their monitoring is the lack of simple and reliable analytical methods for their routine determination. In this work, an analytical method has been developed and validated for the simultaneous extraction and determination of the main metabolites of the pharmaceuticals diclofenac, ibuprofen, sulfamethoxazole, carbamazepine and caffeine and of the parabens methylparaben and propylparaben and their parent compounds in wastewater and tap water samples. Sample extraction was carried out by conventional solid-phase extraction with OASIS HLB cartridges. Analytical determination was carried out by liquid chromatography-tandem mass spectrometry with electrospray ionization. Average accuracy was in the range from 66 to 120% in wastewater and from 86 to 120% in tap water. Precision, expressed as relative standard deviation, was lower than 17% for all the compounds. Method quantification limits were in the range from 1.0 to 33 ng L in wastewater and from 0.5 to 28 ng L in tap water. The method was applied to wastewater and tap water samples. None of the target compounds was detected in tap water whereas all of them were detected in wastewater. Concentrations of the metabolites were similar or higher than those of the parent compounds. Graphical abstract.
近年来,人们广泛评估了防腐剂和药物在水生环境中的存在情况。尽管它们可能比其母体化合物更具毒性或更浓缩,但关于它们的代谢物和/或降解产物的发生情况,信息却很少。对它们进行监测的主要缺点之一是缺乏用于常规测定的简单可靠的分析方法。在这项工作中,开发并验证了一种分析方法,用于同时提取和测定废水和自来水中主要药物(如双氯芬酸、布洛芬、磺胺甲恶唑、卡马西平和咖啡因)以及防腐剂(如甲基对羟基苯甲酸酯和对羟基苯甲酸丙酯)及其母体化合物的代谢物。样品提取采用常规固相萃取法,使用 OASIS HLB 小柱。分析测定采用电喷雾电离液相色谱-串联质谱法。在废水中,平均准确度在 66%至 120%之间,在自来水中,平均准确度在 86%至 120%之间。所有化合物的精密度(以相对标准偏差表示)均低于 17%。方法定量限在废水中为 1.0 至 33ng/L,在自来水中为 0.5 至 28ng/L。该方法应用于废水和自来水样品。自来水中未检测到目标化合物,而废水中均检测到。代谢物的浓度与母体化合物的浓度相似或更高。