顶空气相色谱法测定头孢克肟中三乙胺的残留量  

Determination of Residual Triethylamine in Cefixime by Headspace Gas Chromatography

作　　者：郑磊 ZHENG Lei(Jiangsu Jinglixin Pharmaceutical Technology Co.,Ltd.,Nanjing 210000,China)

机构地区：[1]江苏晶立信医药科技有限公司,江苏南京210000

出　　处：《山东化工》2025年第1期162-165,共4页Shandong Chemical Industry

摘　　要：目的:建立顶空气相色谱法测定头孢克肟中三乙胺残留量的方法。方法:以Agilent DB-624毛细管柱(30 m×0.53 mm×3.0μm)为色谱柱;升温程序为初始温度60℃,维持2 min,以10℃/min的升温速率升至150℃,再以20℃/min的升温速率升至220℃,维持10 min;流速为1.0 mL/min;检测器为氢火焰离子化检测器(FID),温度为240℃;分流比为5∶1;顶空瓶平衡温度为85℃,平衡时间为30 min。结果:溶剂峰不与三乙胺峰重合,三乙胺峰和相邻峰之间分离良好;在0.5095~3.821μg/mL的质量浓度范围内,三乙胺的进样浓度与其峰面积呈良好的线性关系(r=0.9961);定量限为0.2584μg/mL;回收率为93.9%~108.7%。四批样品中三乙胺均未检出。结论:该方法的专属性、灵敏度和准确度均良好,能够有效检出头孢克肟中三乙胺的残留量。Objective:To establish a headspace gas chromatography method for the determination of residual triethylamine in cefixime.Methods:The determination was performed with Agilent DB-624 capillary column(30 m×0.53 mm×3.0μm).The oven temperature was programming increased.The initial column temperature is set to 60℃,and lasting for 2 minutes,after raised to 150℃at 10℃/min,after raised to 220℃at 20℃/min,lasting for 10 minutes.The column flow rate is 1.0 mL/min.The temperature of flame ionization detector was set at 240℃.The split ratio is 5∶1.The equilibrium temperature of the sample bottle is 85℃and the balance time of the sample bottle is 30 min.Results:The solvent did not exhibit a peak at the position of triethylamine,and the resolution between the triethylamine peak and adjacent peaks meets the requirements.In the range of 0.5095~3.821μg/mL,triethylamine had a good linear relationship(r=0.9961).The quantification limit is 0.2584μg/mL.The average recovery was 93.9%~108.7%.Triethylamine was not detected in multiple batches of samples.Conclusion:The specificity,sensitivity,and accuracy of this method were all good,and can effectively detect the residual triethylamine in cefixime.

关 键 词：头孢克肟 三乙胺 顶空气相色谱法 

分 类 号：O657.7[理学—分析化学]