1University of Zagreb Faculty of Chemical Engineering and Technology, Department of Analytical Chemistry, 10000 Zagreb, Croatia.
2University of Zagreb Faculty of Pharmacy and Biochemistry, Department of Pharmaceutical Analysis, 10000 Zagreb, Croatia.
Acta Pharm. 2023 Dec 26;73(4):515-535. doi: 10.2478/acph-2023-0041. Print 2023 Dec 1.
Solid-phase extraction (SPE) coupled with capillary electrophoresis (CE) for the determination of macrolide antibiotics (azithromycin, clarithromycin, roxithromycin, tylosin) and tiamulin in water samples was described in this article. These compounds were extracted with different types of sorbents ( Oasis HLB, C18, C8, SDB, and Strata-X) and different masses of sorbents (60 mg, 200 mg, and 500 mg) using different organic solvents (methanol, ethanol, and acetonitrile) and different pH values of water samples (pH 7.00, 8.00, and 9.00). It was found that the highest extraction efficiency of the studied compounds was obtained with 200 mg/3 mL C18 cartridges with methanol as eluent at pH 9.00 of the water sample. The developed SPE-CE method for macrolide antibiotics and tiamulin was validated for linearity, precision, repeatability, the limit of detection (), the limit of quantification (), and recovery. Good linearity was obtained in the range of 0.3-30 mg L depending on the drug, with correlation coefficients higher than 0.9958 in all cases except clarithromycin (0.9873). Expanded measurement uncertainties were calculated for each pharmaceutical, accounting for 20.31 % (azithromycin), 38.33 % (tiamulin), 28.95 % (clarithromycin), 26.99 % (roxithromycin), and 21.09 % (tiamulin). Uncertainties associated with precision and calibration curves contributed the most to the combined measurement uncertainty. The method was successfully applied to the analysis of production waste-water from the pharmaceutical industry.
本文介绍了固相萃取（SPE）与毛细管电泳（CE）联用，用于测定水样中的大环内酯类抗生素（阿奇霉素、克拉霉素、罗红霉素、泰乐菌素）和替米考星。采用不同类型的吸附剂（Oasis HLB、C18、C8、SDB 和 Strata-X）和不同质量的吸附剂（60 mg、200 mg 和 500 mg），用不同的有机溶剂（甲醇、乙醇和乙腈）和不同 pH 值的水样（pH 7.00、8.00 和 9.00）提取这些化合物。结果表明，研究化合物的最高萃取效率是在 pH 9.00 的水样中用 200 mg/3 mL C18 小柱和甲醇作为洗脱液得到的。建立的 SPE-CE 法用于大环内酯类抗生素和替米考星的分析，对线性、精密度、重复性、检测限（LOD）、定量限（LOQ）和回收率进行了验证。除克拉霉素（0.9873）外，所有药物在 0.3-30 mg/L 范围内均得到良好的线性关系，相关系数均高于 0.9958。对每种药物都计算了扩展的测量不确定度，占 20.31%（阿奇霉素）、38.33%（替米考星）、28.95%（克拉霉素）、26.99%（罗红霉素）和 21.09%（替米考星）。精密度和校准曲线的不确定度对组合测量不确定度的贡献最大。该方法成功应用于分析制药工业生产废水中的目标化合物。
