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采用超高效液相色谱-串联质谱法测定污水污泥中的药物、类固醇激素和内分泌干扰性个人护理产品。

Determination of pharmaceuticals, steroid hormones, and endocrine-disrupting personal care products in sewage sludge by ultra-high-performance liquid chromatography-tandem mass spectrometry.

机构信息

State key Laboratory of Organic Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou, 510640, China.

出版信息

Anal Bioanal Chem. 2011 Jan;399(2):891-902. doi: 10.1007/s00216-010-4295-2. Epub 2010 Oct 28.

Abstract

A sensitive method has been developed and validated for the determination of diverse groups of pharmaceuticals, steroid hormones, and hormone-like personal care products in sewage sludge. Samples were extracted by ultrasonic-assisted extraction followed by solid-phase extraction cleanup. For determination of estrogens and hormone-like phenolic compounds, sample extracts were further derivatized with dansyl chloride and purified with silica gel column chromatography to improve the analytical sensitivity. The chemicals were determined by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) in multiple-reaction monitoring mode. Recoveries ranged mostly from 63% to 119% with relative standard deviations within 15%. Method quantification limits were 0.1-3 ng g(-1) dry weight (dw) for sewage sludge. The method was applied to a preliminary investigation of pharmaceuticals and personal care products (PPCPs) in sewage sludge and sediment in the Pearl River Delta, South China. Triclosan, triclocarban, 2-phenylphenol, bisphenol A, and parabens were ubiquitously detected at 3.6-5088.2 ng g(-1) dw in sludge and 0.29-113.1 ng g(-1) dw in sediment samples, respectively. Estrone, carbamazepine, metoprolol, and propranolol were also frequently quantified in the sludge and sediment samples. The dewatering process caused no significant losses of these PPCPs in sewage sludge.

摘要

已开发并验证了一种灵敏的方法,用于测定污水污泥中的各种药物、甾体激素和类激素个人护理产品。样品通过超声辅助提取,然后固相萃取净化进行提取。为了测定雌激素和类激素酚类化合物,样品提取物用丹磺酰氯衍生,并通过硅胶柱色谱进一步纯化,以提高分析灵敏度。采用超高效液相色谱-串联质谱法(UHPLC-MS/MS)在多反应监测模式下测定这些化学品。回收率大多在 63%至 119%之间,相对标准偏差在 15%以内。该方法对污水污泥和沉积物中药物和个人护理产品(PPCPs)的初步调查具有定量限为 0.1-3ng/g(dw)。该方法应用于中国南方珠江三角洲污水污泥和沉积物中药物和个人护理产品(PPCPs)的初步调查。三氯生、三氯卡班、2-苯酚、双酚 A 和对羟基苯甲酸酯在污泥中的浓度为 3.6-5088.2ng/g(dw),在沉积物中的浓度为 0.29-113.1ng/g(dw)。雌酮、卡马西平、美托洛尔和普萘洛尔也经常在污泥和沉积物样品中定量。脱水过程不会导致这些 PPCPs 在污水污泥中明显损失。

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