LC-MS/MS法测定消肿止痛酊中马兜铃酸Ⅰ的含量

Content determination of aristolochic acid I in Xiaozhong Zhitong Tincture by LC-MS/MS method

目的 建立消肿止痛酊中马兜铃酸Ⅰ的专属性检测方法,为消肿止痛酊的质量安全控制提供理论依据。方法 通过液相色谱-质谱联用法对消肿止痛酊中的马兜铃酸Ⅰ进行含量测定。采用Poroshell 120SB-C18(2.1 mm×100 mm,2.7μm)色谱柱进行分离,以0.1%甲酸溶液(含5 mmol/L甲酸铵)-乙腈为流动相进行梯度洗脱,柱温30℃,流速0.3 ml/min,在电喷雾离子化正离子模式下,进行多反应检测,外标法定量。结果 马兜铃酸Ⅰ在0.1~40 ng/ml范围内线性关系良好(相关系数r=0.9999),平均回收率为114.0%(RSD=8.7%),方法重复性及精密度均良好。结论 该方法操作简单,可实现对消肿止痛酊中马兜铃酸Ⅰ的含量测定。

Objective To establish a specific detection method for aristolochic acid I in Xiaozhong Zhitong Tincture,so as to provide theoretical basis for quality control of Xiaozhong Zhitong Tincture.Methods The content determination of aristolochic acidⅠin Xiaozhong Zhitong Tincture was carried out by liquid chromatography-mass spectrometry(LC-MS/MS).Separation was carried out on a Poroshell 120 SB-C18(2.1 mm×100 mm,2.7μm)column,gradient elution was carried out with 0.1%formic acid solution(containing 5 mmol/L ammonium formate)-acetonitrile as the mobile phase,the column temperature was 30℃,and the flow rate was 0.3 ml/min.In the positive ion mode of electrospray ionization,multiple reaction monitoring was carried out,and external standard method was used for quantification.Results The linear relationship of aristolochic acid I was good in the range of 0.1-40 ng/ml(correlation coefficient r=0.9999),the average recovery rate was 114.0%(RSD=8.7%),and the repeatability and precision of the method were both good.Conclusion The method is simple and can be used to carry out the content determination of aristolochic acid I in Xiaozhong Zhitong Tincture.