气相色谱法测定注射用盐酸头孢吡肟中异亚丙基丙酮

Determination of mesityl oxide in cefepime hydrochloride for injection by GC

目的建立注射用盐酸头孢吡肟中基因毒性杂质异亚丙基丙酮的含量测定方法。方法气相色谱法,采用DB-WAX毛细管柱(30 m×0.53 mm,1.0μm),程序升温,起始柱温45℃,维持5 min,10℃/min的速率升温至180℃;进样口温度200℃,检测器(FID)温度250℃,氮气流量为5 mL/min;顶空法进样,顶空温度80℃,平衡时间20 min。结果异亚丙基丙酮与难分离物质二甲基甲酰胺可良好分离;在浓度0.41~8.2μg/mL范围内,线性良好,回归方程y=0.2457x-0.0066,相关系数r=0.9998;平均回收率为99.1%;检测限0.5 ppm,定量限1.5 ppm。结论该方法专属性及耐用性良好,准确度及灵敏度高,可用于注射用盐酸头孢吡肟中异亚丙基丙酮杂质的含量测定。

Objective To establish a method for the determination of the content of the genotoxic impurity mesityl oxide in cefepime hydrochloride for injection.Methods Gas Chromatography was used,with a DB-WAX capillary column(30 m×0.53 mm,1.0μm)and temperature programmed.The initial column temperature was 45℃,maintained for 5 min,and the temperature rose to 180℃at the rate of 10℃/min;the inlet temperature was 200℃,the detector(FID)temperature was 250℃,and the flow rate of nitrogen was 5 mL/min.The head space temperature was 80℃and the equilibrium time was 20 min.Results Mesityl oxid could be well separated from dimethylformamide,which was difficult to separate;The linear range was 0.41~8.2μg/mL(y=0.2457x-0.0066,r=0.9998).The average recovery rate was 99.1%.The limit of detection was 0.5 ppm and the limit of quantitation was 1.5 ppm.Conclusion The method has good specificity,durability,accuracy,and sensitivity,and can be used for the determination of content of mesityl oxid in cefepime hydrochloride for injection.