Department of Analytical Chemistry, Faculty of Chemical Engineering and Technology, University of Zagreb, Zagreb, Croatia.
J Sep Sci. 2013 Sep;36(18):3042-9. doi: 10.1002/jssc.201300486. Epub 2013 Aug 12.
This paper describes the development, optimization, and validation of a method for the determination of five pharmaceuticals from different therapeutic classes (antibiotics, anthelmintics, glucocorticoides) in water samples. Water samples were prepared using SPE and extracts were analyzed by HPLC with diode-array detection. The efficiency of 11 different SPE cartridges to extract the investigated compounds from water was tested in preliminary experiments. Then, the pH of the water sample, elution solvent, and sorbent mass were optimized. Except for optimization of the SPE procedure, selection of the optimal HPLC column with different stationary phases from different manufacturers has been performed. The developed method was validated using spring water samples spiked with appropriate concentrations of pharmaceuticals. Good linearity was obtained in the range of 2.4-200 μg/L, depending on the pharmaceutical with the correlation coefficients >0.9930 in all cases, except for ciprofloxacin (0.9866). Also, the method has revealed that low LODs (0.7-3.9 μg/L), good precision (intra- and interday) with RSD below 17% and recoveries above 98% for all pharmaceuticals. The method has been successfully applied to the analysis of production wastewater samples from the pharmaceutical industry.
本文描述了一种从水样中测定五种不同治疗类别的药物（抗生素、驱虫药、糖皮质激素）的方法的开发、优化和验证。水样采用 SPE 进行预处理，提取物采用 HPLC 二极管阵列检测进行分析。在初步实验中测试了 11 种不同 SPE 小柱从水中萃取目标化合物的效率。然后，优化了水样的 pH 值、洗脱溶剂和吸附剂质量。除了 SPE 步骤的优化外，还对不同制造商的不同固定相的最佳 HPLC 柱进行了选择。采用加标不同浓度药物的泉水样品对所建立的方法进行了验证。除环丙沙星（0.9866）外，所有药物的线性范围均在 2.4-200μg/L 之间，相关系数均大于 0.9930。此外，该方法还具有较低的检出限（0.7-3.9μg/L）、良好的精密度（日内和日间），RSD 低于 17%，所有药物的回收率均高于 98%。该方法已成功应用于制药工业生产废水中药物的分析。
