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目的利用HPLC色谱杂质谱对头孢西酮钠中杂质进行定量分析和利用液质联用法初步推断主要杂质结构。方法采用18烷基硅烷键合硅胶为填充剂,以磷酸盐缓冲液(50 mmol·L~(-1)磷酸水溶液,用三乙胺调p H4.0)-乙腈(体积比为85∶15)为流动相,检测波长278 nm,流速1.0 m L·min~(-1),柱温35℃,进样量10μL,检测头孢西酮钠杂质谱;通过HPLC-MS初步鉴定杂质。分别用自身对照法和系统指纹定量法对统一化杂质谱的杂质数目和分布情况以及杂质总含量进行评价。结果根据头孢西酮钠合成路线和HPLC-MS测定结果初步推断5个杂质的可能结构,并测定11个杂质含量。用系统指纹定量法对杂质谱的杂质数目和分布情况及杂质总含量的评价结果基本反应了杂质总量情况。结论系统指纹定量法对杂质数目和含量分布情况及杂质总量评价具有快速便捷的特点,《药物杂质谱数字化定量评价系统》5.0软件能快速计算杂质含量。
OBJECTIVE To quantitatively analyze the impurities in cefoselime sodium by HPLC chromatographic impurity profile and to primarily infer the major impurity structure by using liquid chromatography-mass spectrometry. Methods 18 alkylsilane bonded silica gel was used as filler, and phosphate buffer (50 mmol·L -1 phosphoric acid) and p H 4.0 (acetonitrile) (85:15 ) Was used as the mobile phase. The detection wavelength was 278 nm, the flow rate was 1.0 m L · min -1 and the column temperature was 35 ℃. The injection volume was 10 μL. The impurity spectrum of cefoxitin sodium was determined. The impurities were identified by HPLC-MS. The number and distribution of impurities in the impurity profile and the total content of impurities were evaluated by self-control method and system fingerprint quantification method respectively. Results According to the synthesis route of cefoxitin sodium and the results of HPLC-MS, the possible structures of five impurities were preliminarily determined and 11 impurity contents were determined. The system fingerprint quantitative method for impurity spectrum of the number and distribution of impurities and the total content of impurities in the evaluation results basically reflect the total amount of impurities. Conclusions System fingerprinting quantitative and quantitative analysis of the number and content of impurities and the total amount of impurities with quick and easy features, “Drug impurity spectra digital quantitative evaluation system” 5.0 software can quickly calculate the impurity content.