注射用盐酸头孢替安有关物质测定方法的改进  

Improvement on the determination method of related substances in cefotiam hydrochloride for injection

作　　者：王珵[1] 徐憬 林泽鹏 林玲[1] WANG Cheng;XU Jing;LIN Zepeng;LIN Ling(Guangzhou Institute for Drug and Control, Guangzhou 510160, China)

机构地区：[1]广州市药品检验所

出　　处：《中国药品标准》2019年第3期205-211,共7页Drug Standards of China

摘　　要：目的:改进注射用盐酸头孢替安的有关物质测定方法。方法:采用高效液相色谱法。色谱柱为PhenomenexC18色谱柱,流动相A为0.05mol·L^-1磷酸盐缓冲液(pH值7.6~7.8),流动相B为乙腈,梯度洗脱,流速为1.0mL·min^-1,柱温为25℃,检测波长为254nm,进样量为20μL。结果:在该条件下头孢替安峰与各有关物质峰分离良好。检测限为63ng·mL^-1。三批供试品单个最大杂质分别为0.6%、0.7%和0.6%,杂质总量分别为3.8%、3.4%和3.6%。结论:优化后的方法采用梯度洗脱法,较等度洗脱法提高了杂质分离度和检出率;对供试品溶液进行了比较,简化了试验操作步骤;优化了系统适用性试验条件,为其产品质量提高提供了依据。Objective:To optimize the high performance liquid chromatography (HPLC) method for determination of related substances in cefotiam hydrochloride for injection. Methods:The test was performed in Phenomenex C 18 column under the gradient elution of mobile phase A 0.05 mol·L^-1 phosphate buffer solution(pH 7.6-7.8) and mobile B acetonitrile. The flow rate was 1.0 mL·min^-1 , the column temperature was 25 ℃, the detection wavelength was 254 nm and the injection volume was 20 μL. Results:The peak of cefotiam and peaks of other impurities can be well separated under the established chromatographic condition. The LOD of cefotiam was 63 ng ·mL^-1 . The test results of 3 batches of samples showed that the maximal individual impurities were 0.6%, 0.7% and 0.6%, and the total impurities were 3.8%, 3.4% and 3.6%. Conclusion:The optimized method adopts the gradient elution which increases the resolution and detects more impurities compared to the isocratic elution. The preparation procedure of test solution is simplified, and the system suitability condition is optimized. The optimized method ensures the high quality control.

关 键 词：注射用盐酸头孢替安 有关物质 高效液相色谱 

分 类 号：R921.2[医药卫生—药学]