Nieto Antonio, Borrull Francesc, Pocurull Eva, Marcé Rosa Maria
Departament de Química Analítica i Química Orgànica, Universitat Rovira i Virgili, Tarragona, Spain.
J Sep Sci. 2007 May;30(7):979-84. doi: 10.1002/jssc.200600360.
A method for the quantitative determination of ten pharmaceuticals in sewage sludge was developed by using pressurized liquid extraction (PLE) and HPLC-MS with ESI (HPLC-(ESI)MS). The PLE was optimized with regard to solvents and operational parameters, such as temperature, pressure, extraction time, and purge time. The optimum conditions were: 50 mM phosphoric acid/methanol (1:1 v/v) as the extraction solvent, temperature of 100 degrees C, pressure of 100 bar, extraction time 15 min, 2 cycles, flush volume 150% and purge time 300 s. All recoveries for pharmaceuticals were over 68% except for salicylic acid. The repetitivity and reproducibility between days expressed as RSD was lower than 8% for repetitivity and 10% for reproducibility. The LOD of all compounds was lower than 10 microg/kg of dry weight of sewage sludge. The method was applied to determine the pharmaceuticals in sewage sludge from two domestic sewage treatment plants (STPs). The samples were collected every three months between February 2004 and June 2005. Some pharmaceuticals were determined in the samples and naproxen showed the highest value (242 microg/kg of dry weight).
建立了一种采用加压液体萃取(PLE)和电喷雾电离高效液相色谱-质谱联用(HPLC-(ESI)MS)定量测定污水污泥中10种药物的方法。对PLE的溶剂及温度、压力、萃取时间和吹扫时间等操作参数进行了优化。最佳条件为:以50 mM磷酸/甲醇(1:1 v/v)作为萃取溶剂,温度100℃,压力100 bar,萃取时间15 min,2个循环,冲洗体积150%,吹扫时间300 s。除水杨酸外,所有药物的回收率均超过68%。以相对标准偏差(RSD)表示的日内重复性和日间重现性,重复性低于8%,重现性低于10%。所有化合物的检测限均低于10 μg/kg干重的污水污泥。该方法用于测定两家生活污水处理厂(STP)污水污泥中的药物。在2004年2月至2005年6月期间每三个月采集一次样品。在样品中测定了一些药物,萘普生含量最高(242 μg/kg干重)。