基于差示光谱及指纹图谱结合偏最小二乘回归分析法研究决明子提取物的平衡溶解度

Study on the equilibrium solubility of Cassiae Semen extract based on differential spectrum and fingerprint combined with partial least squares regression analysis

目的:确定决明子提取物的最佳溶出介质,分析决明子提取物中主要成分在最佳溶出介质中对平衡溶解度的贡献程度,明确决明子提取物平衡溶解度的标志物。方法:以总蒽醌含量为指标,采用差示分光光度法测定决明子提取物在37℃时于水、0.1 moL/L盐酸和pH 6.8磷酸盐缓冲液中不同时间点的平衡浓度,确定最佳溶出介质。以决明子提取物总蒽醌指纹图谱为参照,采用HPLC法建立决明子提取物在最佳溶出介质中不同平衡时间点平衡浓度的指纹图谱,筛选决明子提取物平衡溶解度的标志物。结果:决明子提取物在37℃时于水、0.1 moL/L盐酸和pH 6.8磷酸盐缓冲液中平衡溶解度分别为10.344、10.910、11.099μg/mL,达到平衡时间点的时间分别为24 h、3 h和7 h。在最佳溶出介质中,VIP值>1的化学成分有22个,其中VIP值分别为1.13987、1.15565、1.12806、1.14825、1.14880的化学成分分别为已知成分橙黄决明素、大黄酸、大黄素、大黄酚和大黄素甲醚。结论:pH 6.8磷酸盐缓冲液为决明子提取物的最佳溶出介质,可以橙黄决明素、大黄酸、大黄素、大黄酚和大黄素甲醚为溶解度标志物考察决明子提取物的平衡溶解度。

Objective:To determine the best dissolution medium of Cassiae Semen extract,analyze the contribution degree of the main components in Cassiae Semen extract to equilibrium solubility in the optimal dissolution medium,and clarify the markers of equilibrium solubility of Cassiae Semen extract.Methods:The equilibrium concentrations of Cassiae Semen extract were determined at different time points in water,0.1 mol/L hydrochloric acid and pH 6.8 phosphate buffer at 37℃by differential spectrophotometry with taking the content of total anthraquinone as the index,and the optimal dissolution medium was determined.The equilibrium concentration fingerprint of Cassiae Semen extract at different equilibrium time points in the optimal dissolution medium was established by HPLC,and the markers of equilibrium solubility of Cassiae Semen extract were screened.Results:The equilibrium solubility of Cassiae Semen extract in water,0.1 mol/L hydrochloric acid and pH 6.8 phosphate buffer at 37℃was 10.344,10.910 and 11.099μg/mL,respectively.The time to reach the equilibrium time point was 24 h,3 h and 7 h,respectively.In the optimal dissolution medium,there were 22 chemical components with VIP value greater than 1,of which the chemical components were the known components aurantio-obtusin,rhein,emodin,chrysophanol and physcion,which ranked first,second,fifth,ninth and thirteenth,respectively.Conclusions:pH 6.8 phosphate buffer is the best dissolution medium of Cassiae Semen extract.The equilibrium solubility of Cassiae Semen extract can be investigated by using aurantio-obtusin,rhein,emodin,chrysophanol and physcion as solubility markers.