Multi-residue analytical method for human pharmaceuticals and synthetic hormones in river water and sewage effluents by solid-phase extraction and liquid chromatography-tandem mass spectrometry
Multi-residue analytical method for human pharmaceuticals and synthetic hormones in river water and sewage effluents by solid-phase extraction and liquid chromatography-tandem mass spectrometry
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DOI：
10.1016/j.chroma.2010.08.033
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发表时间：
2010-10-29
影响因子：
4.1
通讯作者：
Surif, Salmijah
中科院分区：
文献类型：
--
作者：
Al-Odaini, Najat Ahmed;Zakaria, Mohamad Pauzi;Surif, Salmijah
环境立法未涵盖的人类药物和合成激素等污染物已日益成为重要的新兴水生污染物。本文报道了一种灵敏、选择性多残留方法的开发，用于同时测定和定量水样中不同治疗类别的 23 种药物和合成激素。目标药物包括抗糖尿病药、抗高血压药、降血脂药、β2-肾上腺素受体激动剂、抗组胺药、镇痛药和性激素。所开发的方法基于固相萃取 (SPE)，然后使用液相色谱-电喷雾电离-串联质谱 (LC-ESI-MS/MS) 进行仪器分析，总运行时间为 30 分钟。将河水样品 (150 mL) 和（污水处理厂）STP 废水 (100 mL) 调节至 pH 2，装入 MCX（3 cm(3)，60 mg）柱中，并用四种不同的试剂进行洗脱，以获得最大回收率。通过使用八个同位素标记的内标 (IS.) 实现定量，可有效校正样品制备过程中的损失和 LC-ESI-MS/MS 分析过程中的基质效应。所有基质中的大多数目标分析物均获得了高于 70% 的良好回收率。方法检测限 (MDL) 范围为 0.2 至 281 ng/L。所开发的方法用于测定各种样品中目标分析物的水平，包括河水和 STP 废水。在检测的新兴污染物中，氯噻嗪的浓度最高，STP出水中的浓度高达865纳克/升，河水中的浓度高达182纳克/升。 (c) 2010 Elsevier B.V. 保留所有权利。
Pollutants such as human pharmaceuticals and synthetic hormones that are not covered by environmental legislation have increasingly become important emerging aquatic contaminants. This paper reports the development of a sensitive and selective multi-residue method for simultaneous determination and quantification of 23 pharmaceuticals and synthetic hormones from different therapeutic classes in water samples. Target pharmaceuticals include anti-diabetic, antihypertensive, hypolipidemic agents, beta 2-adrenergic receptor agonist, antihistamine, analgesic and sex hormones. The developed method is based on solid phase extraction (SPE) followed by instrumental analysis using liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) with 30 min total run time. River water samples (150 mL) and (sewage treatment plant) STP effluents (100 mL) adjusted to pH 2, were loaded into MCX (3 cm(3), 60 mg) cartridge and eluted with four different reagents for maximum recovery. Quantification was achieved by using eight isotopically labeled internal standards (IS.) that effectively correct for losses during sample preparation and matrix effects during LC-ESI-MS/MS analysis. Good recoveries higher than 70% were obtained for most of target analytes in all matrices. Method detection limit (MDL) ranged from 0.2 to 281 ng/L. The developed method was applied to determine the levels of target analytes in various samples, including river water and STP effluents. Among the tested emerging pollutants, chlorothiazide was found at the highest level, with concentrations reaching up to 865 ng/L in STP effluent, and 182 ng/L in river water. (c) 2010 Elsevier B.V. All rights reserved.