HPLC-MS法鉴定苯扎氯铵同系物

Identification of preparative homolog of benzalkonium chloride by HPLC-MS

目的建立制备的苯扎氯铵同系物鉴定方法。方法采用HPLC进行纯度分析,并采用HPLCMS鉴定制备的苯扎氯铵3种同系物。使用Inertsil CN-3色谱柱(4.6 mm×250 mm×5μm),以醋酸钠溶液-乙腈(53∶47)为流动相,流速为0.5 m L·min^(-1)。以电喷雾离子源(ESI)正离子模式将样品离子化,子离子扫描模式裂解3种同系物以鉴定结构。结果粗品经纯化得到化学纯度分别为97.8%、96.5%、99.6%的产品,根据裂解碎片可初步鉴定制备的同系物结构。结论该方法实用性强,可为本品的生产企业及监管部门提供技术支持。

Objective To establish a quantitative method to determine the homolog of benzalkonium chloride. Methods HPLC was used for the purity analysis. HPLC-MS method was used to determine the preparative homolog of benzalkonium chloride. The chromatographic column was Inertsil CN-3（4.6 mm×250 mm×5 μm）. The mobile phase was sodium acetate-acetonitrile（53∶47） and the flow rate was 0.5 m L·min^（-1）. The eletrospray ionization（ESI） with positive source of the mass spectrometer and product ion scan mode were used to pyrolyse the homolog for structure identification. Results The chemical purity of the products was 97.8%, 96.5%, 99.6%. The cracking fragment could help preliminarily identify the structure of homolog. Conclusion The method is practical, which provides technical support for enterprises and supervisors.