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快速HPLC法测定头孢硫脒有关物质
快速HPLC法测定头孢硫脒有关物质
陈红英,张〓静,胡海容,朱少璇

广州白云山医药集团股份有限公司白云山制药总厂,广州 510515
Determination of related substances of cefathiamidine by high-speed HPLC
(Guangzhou Bai Yun Shan Pharmaceutical Group Co., Ltd., Bai Yun Shan  Pharmaceutical Factory,Guangzhou 510515,China)

摘要参考文献相关文章

起始页:1784

摘要:目的:建立快速HPLC法测定头孢硫脒的有关物质。方法:采用Phenomenexkinetex C18 (50 mm×4.6 mm,2.6 μm),流动相为磷酸盐缓冲液-乙腈(86∶14),等度洗脱,流速为1.0 mL·min-1,检测波长为254 nm。结果:头孢硫脒在0.099~7.462 μg·mL-1范围内线性关系良好(r=1);杂质C在0.103~7.762 μg·mL-1范围内线性关系良好 (r=1),平均回收率为99.9%,RSD=2.9% (n=9)。头孢硫脒检测限为0.05 μg·mL-1,定量限为0.1 μg·mL-1;杂质C检测限为0.02 μg·mL-1,定量限为0.05 μg·mL-1。方法的专属性、重复性及供试品溶液在4 ℃条件下的稳定性良好。结论:本方法快速、简便、准确、专属性强,可作为测定头孢硫脒的有关物质的有效方法。

关键词:快速HPLC; 头孢硫脒;有关物质;杂质C;总杂质

通讯作者:朱少璇,女,硕士,教授级高工,主要从事新药研究。

基金项目:

作者简介:陈红英,女,硕士,高级工程师,主要从事新药研究。

Abstract:Objective: To develop a high-speed HPLC method for determination of related substances of cefathiamidine. Methods: Phenomenexkinetex C18 (50 mm×4.6 mm,2.6 μm) was adopted, phosphate buffer-acetonitrile (86∶14) was used as mobile phase, isocratic elution was performed at the flow rate of 1.0 mL·min-1, and the detection wavelength was 254 nm. Results: The linear response ranges of cefathiamidine and the impurity C were 0.099~7.462 μg·mL-1(r=1) and 0.103~7.762 μg·mL-1(r=1), respectively. The average recovery was 99.9% (RSD=2.9%, n=9). The limits of detection of cefathiamidine and the impurity C was 0.1 and 0.05 μg·mL-1, respectively. The limits of quantitation of cefathiamidine and the impurity C were 0.05 and 0.02 μg·mL-1, respectively. This method had good repeatability and specificity, and the test solution was stable when stored at 4 ℃. Conclusion: The method is simple, accurate, sensitive, and specific, which is suitable for determination of related substances of cefathiamidine.

Key words:high-speed HPLC; cefathiamidine; related substances; impurity C; total impurities

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