HPLC法测定头孢氨苄胶囊杂质F的研究

目的:建立测定头孢氨苄胶囊中杂质Δ2-头孢氨苄(杂质F)含量的方法。方法:采用HPLC法,色谱条件为:采用手性柱CHIRALPAK R AD-H柱;以0.78%磷酸二氢钠溶液(7.8 g磷酸二氢钠溶于1 L水中,用磷酸调pH至4.0)为流动相A和0.78%磷酸二氢钠(pH 4.0)-乙腈=55∶45为流动相B;采用梯度洗脱,流速为1.0 mL·min-1;于220 nm处检测。结果:头孢氨苄和杂质F在此条件下分离度良好,分离度大于10.0。结论:经方法学验证,本法可用于对头孢氨苄原料及胶囊中杂质F的质量控制。

Determination of Impurity F in Cefalexin Capsules by HPLC

Objective:To establish an HPLC method for determination ofΔ2-cefalexin(impurity F)in Cefalexin Capsules.Methods:The test was performed in a CHIRALPAKR AD-H column.0.78%sodium dihydrogen phosphate buffer(dissolve 7.8 g sodium dihydrogen phosphate with 1 L water,then adjust pH as 4.0 with phosphoric acid)was used as mobile phase A,and 0.78%sodium dihydrogen phosphate(pH 4.0)-acetonitrile(55∶45)as mobile phase B.The gradient elution procedure was used.The flow rate was 1.0 mL·min-1,and the UV detection wavelength was at 220 nm.Results:Cefalexin and impurity F were separated well under the chromatographic condition and the resolution was more than 10.0.Conclusion:The methodology validation results show that the established method can be suitable for control of impurity F in drug substance cefalexin and Cefalexin Capsules.