UPLC-MS/MS法检测冠心苏合制剂10种非法添加色素

UPLC-MS/MS method to detect 10 pigments illegally added in Guanxin Suhe preparations

目的建立UPLC-MS/MS法检测冠心苏合制剂10种非法添加色素金胺O、金橙Ⅱ、碱性橙2、日落黄、柠檬黄、孔雀石绿、亮蓝、亮绿、碱性橙21、碱性橙22。方法以Waters ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.8μm)为色谱柱;负模式流动相为10 mmol·L^-1甲酸铵溶液和乙腈,正模式流动相为20 mmol·L^-1甲酸铵-0.1%甲酸溶液和乙腈,梯度洗脱;流速为0.4 mL·min^-1;柱温为35℃。选择ESI离子源,正离子扫描,负离子扫描;多反应监测(MRM)模式。结果10种色素呈现良好的线性关系,r均大于0.9984,检测限为0.01~0.03 ng·mL^-1,平均加样回收率为91.3%~105.2%,RSD均小于3%。结论该方法准确、可靠,可为冠心苏合制剂的质量评价提供参考。

Objective To determine 10 illegally added pigments,including auramine O,orangeⅡ,alkaline orange 2,sunset yellow,tartrazine,malachite green,brilliant blue,brilliant green,alkaline orange 21,and alkaline orange 22 in Guanxin Suhe preparations by UPLC-MS/MS.Methods Waters ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.8μm)was used as the chromatographic column.The mobile phase was 10 mmol·L^-1 ammonium formate solution and acetonitrile in the negative mode,20 mmol·L^-1 ammonium formate-0.1%formic acid solution and acetonitrile in the positive mode,with gradient elution.The flow rate was 0.4 mL·min^-1,and the column temperature was 35℃.A positive-ion source,a negative-ion source and an MRM mode were used.Results All 10 pigments showed a good linear relationship,r were greater than 0.9984,the detection limit was 0.01-0.03 ng·mL^-1,the average sample recovery was 91.3%-105.2%,and the RSDs was less than 3%.Conclusion The establish method is accurate and reliable,which provides a reference for the quality evaluation of Guanxin Suhe preparation.