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A very fast and simple method for the determination of sulfonamide residues in seawaters

机译:一种快速,简单的海水中磺酰胺残留量测定方法

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摘要

The development of simple and reproducible analytical methods for the determination of new organic pollutants like pharmaceuticals and personal care products in seawaters is of the highest priority. In the present study, a new analytical method based on offline solid phase extraction and liquid chromatography with standard UV detection (SPE-HPLC-UV) was developed to determine the presence of sulfonamides in seawaters. Special attention was paid to the sample preparation step. Different variables affecting the extraction process, such as seawater salinity and the humic acid content were studied. As a result, the presented SPE procedure for the extraction of sulfonamides from seawaters is also applicable to other techniques like LC-MS and LC-MS/MS. This method was optimized and fully validated for its performance parameters. It has very good selectivity, linearity (R~2 > 0.995), precision (RSD < 5%), accuracy (76.7-115.4%), as well as low limits of detection (LOD, 167 ng L~(-1)) and quantification (LOQ, 500 ng L~(-1)). This SPE procedure proved to be very effective (absolute recovery >75%), even in highly saline waters and in the presence of humic acids.
机译:开发测定海水中新有机污染物(如药物和个人护理产品)的简单且可重现的分析方法是当务之急。在本研究中,开发了一种新的分析方法,该方法基于离线固相萃取和具有标准UV检测的液相色谱(SPE-HPLC-UV),以确定海水中是否存在磺酰胺。特别注意样品制备步骤。研究了影响提取过程的不同变量,例如海水盐度和腐殖酸含量。结果,所提出的从海水中萃取磺酰胺的SPE方法也适用于其他技术,例如LC-MS和LC-MS / MS。该方法已经过优化,并对其性能参数进行了充分验证。它具有很好的选择性,线性(R〜2> 0.995),精度(RSD <5%),精度(76.7-115.4%)和低检测限(LOD,167 ng L〜(-1))定量(LOQ,500 ng L〜(-1))。该SPE程序被证明是非常有效的(绝对回收率> 75%),即使在高盐度水和腐殖酸存在下也是如此。

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