醒脑再造丸中马兜铃酸Ⅰ的含量测定

Determination of Aristolochic AcidⅠin Xingnao Zaizao Pill

目的建立醒脑再造丸中马兜铃酸Ⅰ的含量测定方法,进行产品质量安全控制。方法样品经甲醇提取、中性氧化铝柱吸附、甲醇洗脱杂质,以含5%甲酸的甲醇解吸附马兜铃酸Ⅰ,之后采用高效液相色谱法、紫外检测器进行含量测定。结果马兜铃酸Ⅰ对照品浓度在0.10~20.06μg/mL范围内线性关系良好(r≥0.9998),平均回收率分别为76.2%、105.8%、87.7%;该方法的重复性良好[共测定6次,相对标准偏差(RSD)≤3.9%],检出限为1μg/g(0.0001%)。3批样品均未检出马兜铃酸Ⅰ。结论该方法专属性好、准确可靠、灵敏度高,可用于醒脑再造丸中马兜铃酸Ⅰ的限量检查,对产品质量安全控制具有重大意义。

Objective To establish a method for determining the content of aristolochic acidⅠin Xingnao Zaizao pill for product qual⁃ity and safety control.Methods The sample was extracted with methanol,adsorbed on a neutral alumina column,and impurities were eluted with methanol.Aristolochic acidⅠwas desorbed with methanol containing 5%formic acid,and then the content was deter⁃mined by high-performance liquid chromatography and ultraviolet detector.Results The concentration of reference substance for aris⁃tolochic acidⅠranges from 0.10 to 20.06μg/mL,the linear relationship was good(r≥0.9998),the average recovery rate was 76.2%,105.8%and 87.7%.The reproducibility of the method was good[6 measurements,relative standard deviation(RSD)≤3.9%],and the detection limit was 1μg/g(0.0001%).No aristolochic acidⅠwas detected in all three batches of samples.Conclusion This method has good specificity,accuracy,reliability,and high sensitivity,and can be used for the limit inspection of aristolochic acidⅠin Xing⁃nao Zaizao pill.It is of great significance for product quality and safety control.