目的 建立HPLC對注射用頭孢孟多酯鈉中有關物質(zhì)進行測定的方法。方法 菲羅門Luna C₁₈(2)色譜柱(250 mm×4.6 mm,5μm),流動相為1%三乙胺溶液(用磷酸調(diào)節(jié)pH值至2.5)-乙腈(76:24),體積流量為1.5 mL/min,檢測波長為254 nm,柱溫為40℃,進樣量為20μL。采用雜質(zhì)對照品法外標法計算雜質(zhì)D,采用加校正因子的主成分自身對照法計算雜質(zhì)A、E、C。結(jié)果 雜質(zhì)D為主要降解產(chǎn)物,定量限為0.01%,在0.02~0.20μg與峰面積線性關系良好。雜質(zhì)A、E、C的校正因子分別為1.14、1.25、1.14,檢測限分別為0.004%、0.02%、0.04%。結(jié)論 雜質(zhì)D、A、E、C作為特定雜質(zhì)應訂入質(zhì)量標準,可以更好地控制注射用頭孢孟多酯鈉中有關物質(zhì)。

Objective To establish an HPLC method for determination of related substances in Cefamandole Nafate for injection. Methods HPLC method was adopted. The determination was performed on Phenomenex C₁₈ (2) column (250 mm×4.6 mm, 5 μm), mobile phase was 1% triethylamine solution (phosphoric acid adjusted pH to 2.5)-acetonitrile (76:24) at a flow rate of 1.5 mL/min. The detection wavelength was set at 254 nm, the column temperature was at 40℃, and the injection volume was 20 μL. Impurity D was determined by external standard method, and impurity A, E, and C were determined by principal component self control method with correction factor. Results Impurity D was the main degradation products, the quantitative limits was 0.01%, and there had good linearity in the ranges of 0.02-0.20 μg/mL. The correction factors of impurity A, E and C were 1.14, 1.25, and 1.14, respectively, and the detection limits were 0.004%, 0.02%, and 0.04%, respectively. Conclusion Impurity D, A, E, and C should be adopted into the quality standard as specific impurities which can better control the related substances in Cefamandole Nafate for injection.