黄芩炒炭过程中主要成分与色度值的变化规律及其止血作用研究

目的 通过分析黄芩Scutellariae Radix炒炭过程中化学成分与色度值的动态变化规律及其止血作用评价，以期为黄芩炒炭过程中的质量控制提供科学依据，同时为黄芩炒炭终点的判断奠定基础。方法 制备不同炮制程度的黄芩炭样品（H1～H10），采用紫外-可见分光光度法测定不同炮制程度黄芩炭样品的总黄酮含量和炭吸附力；采用HPLC法测定不同炮制程度黄芩炭样品中没食子酸、5-羟甲基糠醛、野黄芩苷、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素及千层纸素A含量；采用分光测色仪测定不同炮制程度黄芩炭样品的L^*（亮度值）、a^*（红绿色值）、b^*（黄蓝色值）、E_ab^*（总色值）；采用SPSS 19.0和SIMCA 14.1软件进行颜色与主要成分的关联分析。最后，采用剪尾法及玻片法进行不同炮制程度黄芩炭样品对正常小鼠止血及凝血时间的药效评价。结果 在黄芩炭炮制过程中，随着炭化程度的增加，样品中总黄酮、没食子酸、5-羟甲基糠醛、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、千层纸素A的含量呈先增后降的趋势，野黄芩苷呈下降趋势。样品粉末的L^*、b^*、E_ab^*值呈降低趋势，a^*值呈先增后降趋势。L^*值、b^*值和E_ab^*值与野黄芩苷、黄芩苷、汉黄芩苷呈正相关，a^*值与没食子酸、5-羟甲基糠醛、黄芩素、汉黄芩素、千层纸素A呈正相关，总黄酮与L^*、a^*、b^*、E_ab^*呈正相关。主成分分析（principal component analysis，PCA）结果显示，不同炮制程度黄芩炭样品各自归类成簇，可区分不同程度的炮制品。回归分析显示，仅没食子酸、5-羟甲基糠醛、汉黄芩素可通过色度值结合回归方程来预测含量，其余成分则不能。结合PCA、炭吸附力及药理实验结果表明，黄芩炭炮制前后炭吸附力和止血、凝血作用差异较大，样品H7（180 ℃、9 min）炭吸附力作用较强，结合止血及凝血时间，H7样品止血作用较好。结论 黄芩炒炭过程中的颜色与化学成分的变化存在相关性，可为黄芩炒炭终点判断提供数据支撑。

Research on change discipline of main composition and chromaticity value and hemostatic effect of Scutellariae Radix in process of frying charcoal

Objective By analyzing the dynamic change rule of chemical composition and chromaticity value in the processing of Huangqintan (Carbonized Scutellariae Radix, CSR) and the evaluation of hemostatic effect, in order to provide a scientific basis for the quality control of CSR, and lay a foundation for the judgment of the end point of CSR production. Methods CSR samples (H1—H10) with different processing degrees were prepared, and the total flavonoids content and carbon adsorption capacity of the samples were determined by ultraviolet and visible spectrophotometry. Gallic acid, 5-hydroxymethylfurfural, scutellarin, baicalin, wogonoside, baicalein, wogonin and oroxylin A in different samples with different processing degrees were determined by HPLC. The L^* (brightness value), a^* (red green value), b^* (yellow blue value), E_ab^* (total color value) of different samples with different processing degrees were measured by spectrophotometer. SPSS 19.0 and SIMCA 14.1 softwares were used to analyze the correlation between color and main compositions. Finally, pharmacodynamic evaluation on hemostasis and coagulation time of normal mice with different processing degree of samples was conducted by tail clipping method and slide method. Results With the increase of carbonization degree, the contents of total flavonoids, gallic acid, 5-hydroxymethylfurfural, scutellarin, baicalin, wogonoside, baicalein, wogonin and oroxylin A in the sample increased first and then decreased, while scutellarin showed a decreasing trend. The L^*, b^*, and E_ab^* values of the sample powder showed a decreasing trend, while the a^* value increased first and then decreased. The L^*, b^*, and E_ab^* values were positively correlated with scutellarin, baicalin, and wogonoside. The a^* value was positively correlated with gallic acid, 5-hydroxymethylfurfural, baicalein, wogonin and oroxylin A. Total flavonoids were positively correlated with L^*, a^*, b^*, and E_ab^*. The results of principal component analysis (PCA) showed that the samples with different processing degrees were classified into clusters, which could distinguish different processed products. Regression analysis showed that only gallic acid, 5-hydroxymethylfurfural and wogonin could be predicted by the color value combined with the regression equation, while the other components could not. The results of PCA, carbon adsorption and pharmacological experiments showed that there were significant differences in carbon adsorption and hemostatic and coagulation effects before and after processing of CSR, the carbon adsorption effect of sample H7 (180 ℃, 9 min) was stronger, and combined with hemostatic and clotting time, the H7 sample had a better hemostatic effect. Conclusion There is a correlation between the color and chemical composition in the processing of CSR, which can provide data support for the judgment of the end point of charcoal frying.