Department of Environmental Chemistry, IDAEA-CSIC, Jordi Girona 18-26, 08034 Barcelona, Spain.
J Chromatogr A. 2013 Feb 1;1275:32-40. doi: 10.1016/j.chroma.2012.12.004. Epub 2012 Dec 19.
The present study describes the development, validation and a practical application of a fully automated analytical method based on pressurized liquid extraction (PLE) followed by solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) for the simultaneous determination of 22 sulfonamides, including five acetylated metabolites, in sewage sludge and soil samples. Both matrix matched calibration curves and standard calibration curves were built in order to evaluate the potential matrix effects during analysis, and different internal standards were used to compensate these effects during quantification. The recovery efficiencies were found to be 60-130% for the majority of the sulfonamides in both matrices and at two spike levels. The intra-day and inter-day precisions, expressed by the relative standard deviation (RSD), were below 23%. The method limits of detection (MLODs) achieved were in the range 0.03-2.23 ng g(-1) for sewage sludge and 0.01-4.19 ng g(-1) for soil samples. The methodology was applied to evaluate the occurrence of the target sulfonamides in several sewage sludge and soil samples taken in different wastewater treatment plants (WWTPs) and agricultural areas. Results confirmed the wide presence of sulfonamides in both matrices, being sulfathiazole and sulfamethazine the sulfonamides most frequently detected in sewage sludge and soil samples, respectively. Maximum concentrations corresponded to sulfamethazine in both cases (139.2 ng g(-1) and 8.53 ng g(-1) for sewage sludge and soils respectively). Levels were generally lower in soils. Three of the five acetylated metabolites were detected in sewage sludge and two of them in soils, at concentrations not higher than 9.81 ng g(-1).
本研究描述了一种完全自动化的分析方法的开发、验证和实际应用，该方法基于加压液体萃取（PLE），随后进行固相萃取-液相色谱-串联质谱（SPE-LC-MS/MS），用于同时测定污水污泥和土壤样品中的 22 种磺胺类药物，包括 5 种乙酰化代谢物。为了评估分析过程中的潜在基质效应，建立了基质匹配校准曲线和标准校准曲线，并使用不同的内标物在定量时补偿这些效应。在两种基质和两个加标水平下，大多数磺胺类药物的回收率为 60-130%。日内和日间精密度（RSD）表示，均低于 23%。在污水污泥中，方法检出限（MLOD）范围为 0.03-2.23ng g(-1)，在土壤样品中为 0.01-4.19ng g(-1)。该方法应用于评估在不同污水处理厂（WWTP）和农业区采集的几种污水污泥和土壤样品中目标磺胺类药物的发生情况。结果证实磺胺类药物在这两种基质中广泛存在，污水污泥和土壤样品中分别最常检测到磺胺噻唑和磺胺甲噁嗪。在这两种情况下，最大浓度均对应于磺胺甲噁嗪（污水污泥分别为 139.2ng g(-1)和 8.53ng g(-1)，土壤分别为 8.53ng g(-1)）。土壤中的水平通常较低。在污水污泥中检测到 5 种乙酰化代谢物中的 3 种，在土壤中检测到 2 种，浓度不高于 9.81ng g(-1)。
