An HPLC method for routine quality control of biapenem was established.A Dikma Diamonsil C_(18) column(250mm×4.6 mm,5μm) was used with diode array detection and single wavelength detection at 220 nm.The mobile p...An HPLC method for routine quality control of biapenem was established.A Dikma Diamonsil C_(18) column(250mm×4.6 mm,5μm) was used with diode array detection and single wavelength detection at 220 nm.The mobile phase was consisted of acetonitrile-0.1%triethylamine water(1:99,v/v).The liner range for biapenem quantification was 0.05-10.0 mg/mL(r^2= 0.999). The LOD and LOQ of impurity were 4.8 ng(S/N = 3) and 18.5 ng(S/N = 10),respectively.Intra-day RSD of main impurity and total impurity were 1.84%and 3.37%(n = 3);inter-day RSD of main impurity and total impurity were 4.84%and 7.58% (n = 9).The test solution was stable when stored at 4℃for 6 h.The impurity peaks of biapenem can be identified by chromatographic spectral correlation analysis using high-performance liquid chromatography-diode array detection data from the quality control method by calculating correlation coefficients without reference standards.Two hydrolysis degradation products with relative retention times(RRTs) of 0.528 and 0.743,two dimers with RRTs of 1.062 and 2.817 were identified in the quality control chromatogram.It provides a new way to identify impurity peaks by the routine HPLC-UV method.展开更多
基金National Key New Drug R&D Program Foundation of China(Grant No.2009ZX09313-027).
文摘An HPLC method for routine quality control of biapenem was established.A Dikma Diamonsil C_(18) column(250mm×4.6 mm,5μm) was used with diode array detection and single wavelength detection at 220 nm.The mobile phase was consisted of acetonitrile-0.1%triethylamine water(1:99,v/v).The liner range for biapenem quantification was 0.05-10.0 mg/mL(r^2= 0.999). The LOD and LOQ of impurity were 4.8 ng(S/N = 3) and 18.5 ng(S/N = 10),respectively.Intra-day RSD of main impurity and total impurity were 1.84%and 3.37%(n = 3);inter-day RSD of main impurity and total impurity were 4.84%and 7.58% (n = 9).The test solution was stable when stored at 4℃for 6 h.The impurity peaks of biapenem can be identified by chromatographic spectral correlation analysis using high-performance liquid chromatography-diode array detection data from the quality control method by calculating correlation coefficients without reference standards.Two hydrolysis degradation products with relative retention times(RRTs) of 0.528 and 0.743,two dimers with RRTs of 1.062 and 2.817 were identified in the quality control chromatogram.It provides a new way to identify impurity peaks by the routine HPLC-UV method.
