Poirier Larabie S, Houde M, Gagnon C
Aquatic Contaminants Research Division, Science and Water Technology Directorate, Environment and Climate Change Canada, 105 McGill Street, Montréal, Québec, H2Y 2E7, Canada.
Aquatic Contaminants Research Division, Science and Water Technology Directorate, Environment and Climate Change Canada, 105 McGill Street, Montréal, Québec, H2Y 2E7, Canada.
J Chromatogr A. 2017 Nov 3;1522:48-55. doi: 10.1016/j.chroma.2017.09.055. Epub 2017 Sep 27.
Aquatic systems near major urban centers are constantly contaminated with effluent from wastewater treatment plants. Pharmaceuticals are part of the contamination and several classes of drugs have been detected in surface waters in the last decade. To better understand the impact of those pharmaceuticals in ecosystems, the exposure to aquatic species needs to be investigated. This study presents a new simple and rugged quantitative method for the determination of several classes of drugs using 100μL of plasma from fish environmentally exposed to a major but highly diluted urban effluent. Six common drugs (i.e., diclofenac, ibuprofen, naproxen, salbutamol, sulfamethoxazole and trimethoprim) and one major metabolite (2-hydroxy-ibuprofen), present in significant amount in impacted waterways have been selected for the development and validation of the method. First, all drugs were extracted using cation exchange solid phase extraction (SPE) and eluted with two solvent mixtures. Then, the extracts were analyzed using a reverse-phase analytical column Waters CORTECS C+ (150×2.1mm, 2.7μm) within 14min. MS/MS was performed with an electrospray (ESI) interface in positive ion mode, with multiple reaction monitoring (MRM) experiment acquiring two product ions per drugs. Quantification has been made with standard curves for each analyte using isotopically labeled internal standards. This method has high sensitivity with limits of quantification of 1ngmL for each drug, except for ibuprofen and its metabolite 2-hydroxy-ibuprofen at 2ngmL. The precision of the method was below 11%, the accuracy between 94 and 105% and overall recovery between 94 and 111% for all drugs, with high selectivity. Application of the method to plasma samples from wild northern pike inhabiting the St. Lawrence River collected over a three-year period showed the presence of naproxen, diclofenac, trimethoprim and salbutamol at very low concentrations (around 1ngmL).
主要城市中心附近的水生系统不断受到来自污水处理厂废水的污染。药品是污染物的一部分，在过去十年中，地表水中已检测到几类药物。为了更好地了解这些药物对生态系统的影响，需要研究其对水生物种的暴露情况。本研究提出了一种新的简单且耐用的定量方法，用于使用100μL来自环境暴露于主要但高度稀释的城市废水的鱼类血浆来测定几类药物。已选择六种常见药物（即双氯芬酸、布洛芬、萘普生、沙丁胺醇、磺胺甲恶唑和甲氧苄啶）和一种主要代谢物（2-羟基布洛芬），这些物质在受影响的水道中含量较高，用于该方法的开发和验证。首先，使用阳离子交换固相萃取（SPE）提取所有药物，并用两种溶剂混合物洗脱。然后，使用反相分析柱Waters CORTECS C+（150×2.1mm，2.7μm）在14分钟内对提取物进行分析。采用电喷雾（ESI）接口在正离子模式下进行MS/MS，通过多反应监测（MRM）实验为每种药物获取两个产物离子。使用同位素标记的内标物为每种分析物绘制标准曲线进行定量。该方法具有高灵敏度，每种药物的定量限为1ng/mL，布洛芬及其代谢物2-羟基布洛芬除外，其定量限为2ng/mL。该方法的精密度低于11%，准确度在94%至105%之间，所有药物的总回收率在94%至111%之间，具有高选择性。将该方法应用于在三年期间收集的栖息于圣劳伦斯河的野生北美狗鱼的血浆样本，结果显示萘普生、双氯芬酸、甲氧苄啶和沙丁胺醇的浓度非常低（约1ng/mL）。
