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Application of fully automated online solid phase extraction-liquid chromatography-electrospray-tandem mass spectrometry for the determination of sulfonamides and their acetylated metabolites in groundwater

机译:全自动在线固相萃取-液相色谱-电喷雾串联质谱法在地下水中磺胺类及其乙酰化代谢产物测定中的应用

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摘要

The present study describes an automated methodology based on a liquid chromatography-electrospray, tandem mass spectrometry method combined with online solid phase extraction (online SPE-LC-ESI-MS/MS) for the simultaneous analysis of 16 sulfonamides (SAs) and five of their acetylated metabolites in groundwater. The evaluation of the degree of SA pollution in groundwater was made through the analysis of a total of 39 samples taken in seven groundwater bodies of Catalonia (Spain). Recovery values obtained ranged from 34.3% (N ~4-acetylsulfadiazine) to 134.4% (sulfabenzamide). The method limits of detection for all the analytes were 0.09-11 ng L~(-1). Sulfamethoxazole was the SA detected more frequently (56.4% of the samples), with an average concentration of 2.3 ng L~(-1), followed by sulfadimethoxine, present in 54% of the samples with an average concentration of 0.2 ng L~(-1). It should be highlighted that the acetylated metabolites were ubiquitous in the different samples, with frequencies of detection up to 36% and maximum concentrations of 18 ng L~(-1) (N ~4- acetylsulfamerazine).
机译:本研究描述了一种基于液相色谱-电喷雾,串联质谱联用在线固相萃取(在线SPE-LC-ESI-MS / MS)的自动化方法学,用于同时分析16种磺酰胺(SA)和5种磺胺类药物。它们在地下水中的乙酰化代谢产物。通过分析在加泰罗尼亚(西班牙)的七个地下水体中采集的总共39个样品,对地下水中SA污染的程度进行了评估。获得的回收率范围从34.3%(N〜4-乙酰磺胺嘧啶)到134.4%(磺胺苯甲酰胺)。所有分析物的检出限为0.09-11 ng L〜(-1)。磺胺甲恶唑是最常见的SA(56.4%样品),平均浓度为2.3 ng L〜(-1),其次是54%样品中磺胺二甲肟,平均浓度为0.2 ng L〜(-1)。 -1)。应当强调的是,乙酰化代谢产物在不同样品中无处不在,检测频率高达36%,最大浓度为18 ng L〜(-1)(N〜4-乙酰磺胺嘧啶)。

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