Qualitative and quantitative assessment of related substances in the Cefixime for Oral Suspension by HPLC-TOF-MS and HPLC
Objective To establish qualitative and quantitative method to analyze related substances in the Cefixime for Oral Suspension.Methods An HPLC-TOF-MS method in combination with PeakView and MasterView software was used to preliminarily identify the chemical structure of known impurities and unknown impurities in the Cefixime for Oral Suspension.An HPLC method was developed for the determination of the related substances in Cefixime for Oral Suspension.The mobile phase was acetonitrile-tetrabutylammonium hydroxide solution,with a flow rate of 1.0 mL·min-1.Gradient elution was used.The detection wavelength was set at 254 nm and the column temperature was maintained at 40 ℃.Results According to the mass spectrometry information of reference substances and literature data,six related substances in suspension were identified,including Impurity A,Impurity B,Impurity D,Impurity E,Impurity H and Cefixime tert-butyl ester.Cefixime for Oral Suspension contains five of them,namely Impurity A,Impurity B,Impurity D,Impurity E and Cefixime tert-butyl ester.The method was able to achieve baseline separation.Impurity E and degradation Impurity H had good linear relationships in the concentration range of 0.212 1-21.21 and 0.205 3-20.53 μg·mL-1(r were 0.999 9 and 1.000 0).The recoveries were 105.0％and 93.2％(RSD≤2.3％).Conclusion The developed method is simple,rapid,accurate and effective for testing related substances in the Cefixime for Oral Suspension to control its quality,thus ensuring the safety of clinical medication.
Cefixime for Oral SuspensionHPLCrelated substancesstructure identification
万方数据
维普
