黄地吉仙片中金丝桃苷含量测定方法的建立

Establishment of method for determination of the contents of hyperin in Huangdi Jixian Tablets

目的为了提高黄地吉仙片的质量标准,建立高效液相色谱法(HPLC)测定其菟丝子含量,并对其进行重金属及砷盐的检查。方法色谱柱Symmetry C_(18)(5μm,6 mm×150 mm);流动相:乙腈-0.1%磷酸水(18∶82);流速:1.0 mL/min;检测波长:353 nm;进样量10μL。参考《中国药典》(2010年)方法对重金属、砷盐进行杂质限量检查。结果金丝桃苷在2.0~100.0μg/mL范围内,与峰面积呈良好的线性关系(R2=0.9998),平均回收率为75.61%。重金属小于百万分之十,砷盐小于百万分之二,与《中国药典》(2010年)对中药制剂重金属、砷盐的要求相符。结论 HPLC测定金丝桃苷含量方法简便,灵敏度高,重复性好,可用于黄地吉仙片中金丝桃苷的含量测定;黄地吉仙片的重金属、砷盐检查符合要求,为临床用药安全提供了依据。

Objective To improve the quality standard of Huangdi Jixian Tablets, high performance liquid chromatography（HPLC） method was established to detect the contents of hyperin and the contents of heavy metal and arsenic salt in Huangdi Jiexian Tablets were detected. Methods Symmetry C_（18）（5 μm, 6 mm×150 mm） column was used. The mobile phase contained acetonitrile and 0.1% phosphoric acid（18∶82）. The flow rate was 1.0 mL/min and the detection wavelength was 353 nm. The injection volume was 10 μL. In addition, the impurity of heavy metal and arsenic salt was also detected according to Chinese Pharmacopoeia（2010）. Results Within the range from 2.0 to 100.0 μg/mL, hyperin presented an ideal linear relationship with the peak areas（R2= 0.9998）. The average recovery rate was 75.61%. Heavy metal was less than 10 parts per million and arsenic salt was less than 2 parts per million. These results conformed to the requirements of Chinese Pharmacopoeia（2010）. Conclusion HPLC method for determining the content of hyperin is simple, with high sensitivity and good repeatability, which can be used for the content determination of hyperin in Huangdi Jixian Tablets. The contents of heavy metal and arsenic salt are conformed to the requirement, which provides evidence for the safety of clinical medication.