芩夏止喘颗粒中黄芩苷的稳定性研究

 目的 建立芩夏止喘颗粒中黄芩苷含量测定的HPLC，并以此确定黄芩苷的热稳定性，为确定芩夏止喘颗粒的保质期提供参考。方法 甲醇超声提取样品，流动相：乙腈-水(0.05% H₃PO₄)＝30∶70；流速：1 ml·min^-1；检测波长：278 nm。采用加速实验法对黄芩苷的热稳定性进行了研究。结果 HPLC在6.05～291 μmol·L^-1内线性良好，相关系数R²＞0.9999(n=8)，回收率为98.1%(n=3)；3个批号样品中黄芩苷的含量分别为14.69，14.70，14.67 mg·g^-1；复方中黄芩苷的变化为一级反应；测得100，90℃下的反应速率常数分别为6.45×10^-3，2.99×10^-3h^-1。由Arrhenius公式得出常温下(20℃)的反应速率常数为3.21×10^-6h^-1。进而得出常温下复方药品以黄芩苷为指标的保质期为3.74年。结论 本方法的建立为快速确定药品的保质期，缩短新药的开发周期具有实际意义。

Investigationon the stability of baicalin in Qinxia Zhichuan Keli

OBJECTIVE To establish a HPLC method for the determination of baicalin in a Chinese traditional compound medicine Qinxia Zhichun Keli and investigate the thermo-stability of baicalin. METHOD The content of baicalin in Qinxia Zhichuan Keli was determined on a C₁₈column with a mobile phase consisting of acetonitrile-water (0.05%H₃PO₄)(30∶70) at a flow rate of 1.0 ml·min^-1and detected at 278 nm.The stability of baicalin was investigated according to the principle of chemical dynamics.RESULTS A linearity was obtained from 6.05 μmol·L^-1to 291 μmol·L^-1of baicalin with a good correlation (R2＞0.9999，n=8).The content of baicalin in three different batches were 14.69,14.70 and 14.67 μmol·L^-1,respectively.The variation of baicalin against time at different temperatures was studied.The reaction of baicalin was determined to be first-order reaction and the rate constants at 100℃ and 90℃ were determined to be 6.45×10-3h^-1and 2.99×10-3h^-1respectively.The rate constant at 20℃ was deduced by Arrhenius Equation and the quality guaranteed time of the medicine was given as 3.74 years.CONCLUSION This was a fast and simple method to determine the quality guaranteed time of a chinese traditional medicine.It is useful in the development of a new medicine.