Nieto Antonio, Borrull Francesc, Marcé Rosa Maria, Pocurull Eva
Department of Analytical Chemistry and Organic Chemistry, University Rovira i Virgili, Sescelades Campus, Marcel.lí Domingo s/n, Tarragona 43007, Spain.
J Chromatogr A. 2007 Dec 7;1174(1-2):125-31. doi: 10.1016/j.chroma.2007.09.068. Epub 2007 Oct 6.
A method for the quantitative determination of three macrolides, five sulfonamides, ranitidine, omeprazole and trimethoprim in sewage sludge samples was developed by using pressurized liquid extraction and high-performance liquid chromatography-electrospray ionization mass spectrometry. The extraction solvent and such operational parameters as temperature, pressure, extraction time and purge time were optimized in pressurized liquid extraction. The experimental conditions were: an extraction solvent of water (pH 3):methanol (1:1, v/v), a temperature of 80 degrees C, a pressure of 1500 psi, a sample weight of 5 g, an extraction time of 5 min, one cycle, a flush volume of 60% and a purge time of 120 s. All recoveries were over 74%, except those for ranitidine whose value was 54%. The repeatability and reproducibility between days expressed as relative standard deviation (n = 3) were lower than 11% and 15%, respectively. The limit of detection values ranged from 2 to 11 microg/kg dry weight (d.w.). The method was applied to determine the pharmaceuticals in sewage sludge from two domestic sewage treatment plants. Roxithromycin and tylosin were determined in the samples and tylosin showed the highest value (4.0 mg/kg d.w.).
采用加压液体萃取和高效液相色谱 - 电喷雾电离质谱联用技术,建立了一种测定污水污泥样品中三种大环内酯类、五种磺胺类、雷尼替丁、奥美拉唑和甲氧苄啶的定量方法。在加压液体萃取过程中,对萃取溶剂以及温度、压力、萃取时间和吹扫时间等操作参数进行了优化。实验条件为:萃取溶剂为水(pH 3):甲醇(1:1,v/v),温度80℃,压力1500 psi,样品重量5 g,萃取时间5 min,一个循环,冲洗体积60%,吹扫时间120 s。除雷尼替丁回收率为54%外,其余回收率均超过74%。以相对标准偏差(n = 3)表示的日内重复性和日间重现性分别低于11%和15%。检测限范围为2至11 μg/kg干重(d.w.)。该方法用于测定两家生活污水处理厂污水污泥中的药物。样品中检测到罗红霉素和泰乐菌素,泰乐菌素含量最高(4.0 mg/kg d.w.)。