HPLC法测定药用辅料苯扎氯铵的含量及不同级别样品质量评价

Determination of Benzalkonium Chloride by HPLC and Quality Evaluation of Different Grade Samples

目的建立高效液相法测定药用辅料苯扎氯铵的含量,并对不同级别样品质量进行评价,为苯扎氯铵质量标准提高提供依据。方法采用Inertsil CN-3色谱柱(4.6×250 mm,5μm),以0.1 mol·L^(-1)醋酸钠溶液(醋酸调节pH值至5.0)-乙腈(60∶40)为流动相,流速为2.0 mL·min^(-1),检测波长为254 nm,进样体积为20μL,柱温为35℃。结果苯扎氯铵各组分分离完全,线性关系良好(r均大于0.9990),精密度、重复性及回收率实验结果均符合含量测定要求,n-C_(12)、n-C_(14)、n-C_(16)的加标回收率在98.3%~100.67%范围内;药用辅料级别样品含量均值明显高于化工试剂样品,样品含量数据相对更加集中。结论该方法操作简便、准确可靠,可用于药用辅料苯扎氯铵的含量测定;苯扎氯铵药用辅料级样品的质量控制明显好于化工级样品。

OBJECTIVE To establish a method for the assay of benzalkonium chloride in pharmaceutical excipients by HPLC,and to evaluate the quality of samples of different grades,so as to provide a basis for improving the quality standard of benzalkonium chloride.METHODS The analysis was performed on an Inertsil CN-3 column(4.6×250 mm,5μm).The mobile phase was was 0.1 mol·L^(-1) sodium acetate solution(pH adjusted to 5.0 by acetic acid)-acetonitrile(60∶40)at a flow rate of 2 mL·min^(-1).The detection wavelength was set at 254 nm,the sample volume was 20μL,and the column temperature was 35℃.RESULTS Each component of benzalkonium chloride was completely separated and the linear relationship was good(r>0.9990).The experimental results of precision,repeatability and recovery met the content determination requirements,the average recoveries of n-C_(12),n-C_(14) and n-C_(16) were 99.22%,99.40%and 99.85%,respectively.The average content of samples on the grades of pharmaceutical excipients was significantly higher than chemical reagents,and more concentrated.CONCLUSION The method is handy,accurate and reliable,and can be used for the content determination of benzalkonium chloride.The quality control of benzalkonium chloride on the grades of pharmaceutical excipients was obviously better than that of chemical excipients.