Extraction and determination of sulfonamides, macrolides, and trimethoprim in sewage sludge
Extraction and determination of sulfonamides, macrolides, and trimethoprim in sewage sludge
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DOI：
10.1016/j.chroma.2005.05.051
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发表时间：
2005-09-02
影响因子：
4.1
通讯作者：
Ternes, TA
中科院分区：
文献类型：
--
作者：
Göbel, A;Thomsen, A;Ternes, TA
建立了加压液萃取(PLE)测定城市污泥中磺胺类、大环内酯类抗菌剂和甲氧苄啶的方法。水/甲醇(50：50，v/v)是最有效的萃取剂。选择100摄氏度的温度和100巴的压力进行提取。每次5分钟的两次循环有效地从活性污泥中提取了所有被研究分析物的至少97%的可提取总量。方法的定量限(S/N=10)为3~41mUg/kg干重，相对回收率为78~142%。此外，还考察了pH值和不同的LC/MS/MS体系对绝对回收率的影响。在所调查的抗菌剂中，在城市污水污泥样品中检出了磺胺吡啶、磺胺甲恶唑、甲氧匹林、阿奇霉素、克拉霉素和罗红霉素。活性污泥中的浓度高达197微克/千克干重。相比之下，磺胺类药物的超声溶剂萃取法结果明显较低，而大环内酯类药物的超声溶剂萃取法结果有下降的趋势。(C)2005 Elsevier B.V.保留所有权利。
Pressurized liquid extraction (PLE) was optimized and validated for the determination of sulfonamide and macrolide antimicrobials and trimethoprim in sewage sludge samples. A mixture of water/methanol (50:50, v/v) was found as the most efficient extraction solvent. A temperature of 100 degrees C and a pressure of 100 bar were chosen for extraction. Two cycles of 5 min each efficiently extracted at least 97% of the total extractable amount of all studied analytes from activated sludge. The limits of quantification (S/N= 10) varied between 3 and 41 mu g/kg dry weight (dw) and the relative recoveries ranged between 78 and 142%. Additionally, the influence of pH and different LC/MS/MS systems on the absolute recoveries was assessed. Of the investigated antimicrobials sulfapyridin, sulfamethoxazole, trimethoprim, azithromycin, clarithromycin and roxithromycin were detected in municipal sewage sludge samples. Concentrations in activated sludge ranged up to 197 mu g/kg dw. In comparison, results obtained by ultrasonic solvent extraction were significantly lower for sulfonamides and in tendency lower for macrolides. (c) 2005 Elsevier B.V. All rights reserved.