清开灵注射液生产过程中栀子提取液的快速质量检测

Rapid quality control of Fructus Gardeniae extraction in the preparation of Qingkailing injection

目的:建立清开灵注射液生产过程中栀子提取液中栀子苷的快速准确的定量方法以及栀子液合格与否的快速判断方法。方法:利用反相高效液相色谱法对栀子提取液中的栀子苷进行定量,确定栀子苷的含量范围;同时测定紫外光谱并对其进行波长点的数据筛选,选择和栀子苷含量相关性最好的波长点进行回归分析,建立栀子苷含量和所选定波长点的吸收度之间的关系方程,通过测定吸收度值预测栀子苷的含量;根据预测结果及栀子苷含量范围判断栀子液的合格与否;另取20批栀子液采用高效液相色谱法测定栀子苷的含量,和预测的结果进行比较,检验预测方程的可靠性。结果:约90%的栀子提取液中栀子苷含量分布在8.5～16.0 mg·mL^(-1);和栀子苷含量相关性最好的波长点为242 nm,栀子苷含量与242nm 下的吸收度的关系方程为:栀子苷含量 C(mg·mL^(-1))=(0.0176×A_(242 nm)-0.0001)×500;判断栀子液合格的标准为:8.5<(0.0176×A_(242 nm)-0.0001)×500<16(mg·mL^(-1))合格,其他不合格;栀子苷含量测定值和预测值之间具有良好的相关性(r=0.9901,n=20),紫外法预测栀子苷含量方程可靠。结论:此法简单、快速、准确,可作为清开灵注射液生产过程中栀子提取液的在线质量控制方法。

Objective： To establish a rapid and accurate method for geniposide determination in Fructus Gardeniae extraction in the preparation of Qingkailing injection and estimation of qualifi aqueous solution of ed aqueous solution of Fructus Gardeniae extraction. Methods： Geniposide content in aqueous solution of Fructus Gardeniae extraction was measured by RP - HPLC and the range of geniposide content was limited. The UV spectra of the same samples were scanned simultaneously. The wavelength of the best correlation between UV absorbance and geniposide content determined by HPLC was chosen to regress analyze and the genipeside content of aqueous solution of Fructus Gardeniae extraction was estimated by regression equation. The qualified aqueous solution of Fructus Gardeniae extraction was estimated by the value of predicted geniposide content and the range of genipeside content. Other 20 batches of aqueous solution of Fructus Gardeniae extraction was used for testing the regression equation by comparison of the values of geniposide content determined by HPLC and regression equation. Results： The value of geniposide content in about 90 percent aqueous solution of Fructus Gardeniae extraction were 8.5 - 16.0 mg·mL^-1; The most suitable wavelength correlating with geniposide content was 242 nm. The regression equation： geniposide content （mg·mL^-1） = （0.0176×A242nm - 0.0001）×500; The criterion of qualified aqueous solution of Fructus Gardeniae extraction： 8.5 〈 （0.0176×A242nm - 0.0001）×500 〈 16（mg·mL^-1）. Good correlation between genipeside content determined by HPLC and predicted results was found （r = 0.9901, n = 20）. Conclusion： This method is rapid, simple and accurate, and can be used for the on - line quality control of aqueous solution of Fructus Gardeniae extraction in the preparation of Qingkailing injection.