Zalewski Przemysław, Talaczyńska Alicja, Korban Patrycja, Garbacki Piotr, Mizera Mikołaj, Cielecka-Piontek Judyta
Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Poznan University of Medical Sciences, Grunwaldzka 6, 60-780 Poznań, Poland.
Chromatographia. 2014;77(21-22):1483-1487. doi: 10.1007/s10337-014-2725-6. Epub 2014 Aug 17.
Stability-indicating LC methods were developed and validated for the quantitative determination of doripenem, meropenem and tebipenem in the presence of their degradation products formed during forced degradation studies. Isocratic HPLC and UHPLC separations were performed with a core-shell Kinetex 1.7, 2.6 and 5 µm, all C18, 100A, 100 × 2.1 mm columns and the mobile phase composed of acetonitrile and 12 mmol L ammonium acetate in different ratios. The flow rates of the mobile phase were: 0.5 mL min for 1.7 µm column, and 1.0 mL min for 2.6 and 5 µm ones. Detection wavelength was 298 nm and temperature was set at 30 °C. All analysed drugs were exposed to stress conditions which caused their hydrolysis and thermal degradation. The methods were validated by evaluation of linearity, accuracy, precision, selectivity and robustness. Proposed methods were successfully applied for the determination of investigated antibiotics during kinetic studies in aqueous solutions and in the solid state. The advantages of chromatographic procedures which are based on the use of C18 stationary phases with different particle sizes in the analysis of selected carbapenems were discussed.
建立了稳定性指示液相色谱法,并进行了验证,用于在强制降解研究过程中形成的降解产物存在的情况下,对多利培南、美罗培南和替比培南进行定量测定。采用核壳型Kinetex 1.7、2.6和5 µm的全C18、100A、100×2.1 mm色谱柱进行等度高效液相色谱和超高效液相色谱分离,流动相由乙腈和不同比例的12 mmol/L醋酸铵组成。流动相的流速分别为:1.7 µm色谱柱为0.5 mL/min,2.6和5 µm色谱柱为1.0 mL/min。检测波长为298 nm,温度设定为30℃。所有分析药物均经受导致其水解和热降解的应激条件。通过评估线性、准确度、精密度、选择性和稳健性对方法进行了验证。所提出的方法成功应用于水溶液和固态动力学研究中所研究抗生素的测定。讨论了在分析选定碳青霉烯类药物时,基于使用不同粒径C18固定相的色谱方法的优点。