顶空进样气相色谱内标法测定注射用头孢哌酮钠舒巴坦钠的残留溶剂

Determination of residual solvents of cefoperazone sodium and sulbactam sodium for injection by headspace gas chromatography with internal standard

目的改进顶空进样气相色谱内标法并加以验证,用于考察注射用头孢哌酮钠舒巴坦钠制剂的残留溶剂。方法使用Agilent DB-624(30 m×0.53 mm,3.0μm)毛细管柱;氮气流速为3.0 mL·min^(-1);柱温采用程序升温。以N,N-二甲基甲酰胺(DMF)为溶剂,2-丁酮为内标物;进样口温度为230℃;火焰离子化检测器温度为250℃。结果各待测溶剂之间的分离度满足要求,待测溶剂与内标物峰面积之比的精密度良好,与浓度之间的线性关系较好,平均回收率在82.58%~105.46%之间。结论该方法可以准确测定注射用头孢哌酮钠舒巴坦钠中的14种残留溶剂。183批样品均检出丙酮残留,平均残留量为0.67%,多数样品检出限度以内的乙醇、异丙醇和正己烷,少量样品检出二氯甲烷、乙酸乙酯、环己烷和正丁醇。

Objective To modify and validate a headspace gas chromatography with internal standard to determine residual solvents in cefoperazone sodium and sulbactam sodium for injection.Methods Nitrogen was used as carrier gas and the samples were analyzed on an Agilent DB-624(30 m×0.53 mm,3.0μm)capillary column at a flow rate of 3.0 mL·min^(-1),in which dimethyl formamide(DMF)was used as dissolvent and 2-butanone as internal standard.The oven temperature was programmed.The inlet temperature was set at 230℃and the flame-ionization detector temperature was 250℃.Results Excellent performance was achieved in terms of resolution,repeatability,linearity and sensitivity of all analytes with recovery rates of 82.58%-105.46%.Conclusion This modified method is accurate and suitable for the determination of 14 residual solvents in cefoperazone sodium and sulbactam sodium for injection.All 183 batches contained acetone with a mean residual of 0.67%.Most sample contained ethanol,isopropanol and hexane within the limit,while dichloromethane,ethyl acetate,cyclohexane and n-butanol was detected in few samples.