药用辅料苯甲酸钠中的有机杂质的检测

Determination of Organic Impurities in Pharmaceutical Excipient Sodium Benzoate

目的:建立药用辅料苯甲酸钠中有机杂质的测定方法。方法:采用GC法,Agilent DB-FFAP毛细管柱(0.32 mm×30 m,0.5μm);程序升温:起始温度60℃,保持3 min,再以10℃·min^-1速率升温到230℃后,维持8 min;检测器为火焰离子化检测器(FID);进样口温度为260℃,检测器温度为310℃,并以气-质联用法对检测结果进行确证。结果:各杂质在一定范围内峰面积与浓度呈良好的线性关系(r≥0.9993),平均回收率为95.7%~102.8%,定量限为0.17~1.36 ng。样品中均检出苯甲酸。结论:本方法简便快捷、结果准确,可用于药用辅料苯甲酸钠中有机杂质的检测。

Objective:To establish a method to determine the organic impurities in pharmaceutical excipient sodium benzoate.Methods:GC method was used with an Agilent DB-FFAP eapillary column(0.32 mm×30 m,0.5μm)at programmed temperature:the initial temperature was 60℃,maintained for 3min,and then heated to 230℃at the rate of 10℃·min^-1,and maintained for 8 min.The detector was a flame ionization detector(FID).The inlet temperature was 260℃,and the detector temperature was 310℃.The detection results were confirmed by GC-MS.Results:Within a certain range,each impurity peak area and concentration had good linear relationship(r≥0.9993).The recovery rates were between 95.7%and 102.8%.The limit of quantification was between 0.17 ng and 1.36 ng.Benzoic acid was detected out in all the samples.Conclusion:The method is simple,rapid and accurate,and can be used for the determination of organic impurities in pharmaceutical adjuvant sodium benzoate.