黄芩素制备工艺及含量测定方法的研究

STUDY ON THE PREPARED PROCESS AND ASSAYING METHOD FOR BAICALEIN

目的:研究由黄芩苷制备黄芩素的最佳工艺,并建立黄芩素的含量测定方法。方法:采用直接酸水解黄芩苷制备黄芩素,并以四因素三水平正交实验法,以黄芩素含量、制备率两项考察指标综合评析的方法,对工艺进行了优化。采用聚酰胺薄膜层析法进行定性检测和高效液相色谱(HPLC)法定量检测。结果:四因素三水平的正交实验表明,水(溶媒)用量为黄芩苷的100倍、浓硫酸量为黄芩苷的7倍,制备时间为6h,萃取次数为三次为最佳制备工艺。建立了反相高效液相色谱法测定黄芩素含量的方法,DiscoveryC_(18)(250mm×4.6mm)5μm,紫外检测波长275nm,柱温32℃,流速1.0ml/min,进样量10μl,流动相为甲醇-水-冰醋酸(48:52:0.2)。结论:黄芩素的制备工艺简单,制备率较高,其定性、定量方法操作简单,结果准确可靠,重现性好,可作为其含量测定的常用方法。

Objective：To study the optimal prepared process for baicalein and its assaying method.Methods： The baicalein was prepared by direct acid hydrolysis; And the prepared process was optimized by the orthogonal test L9（34） and the content of baicalein and preparing ratio were taken as observing indexes.The land-parts was used for qualitation determination and HPLC method for quantitation determination.Results：The results of orthogonal test showed that the dosage of water and concentrated sulfuric acid were respectively 100 times and 7 times of baicalin content. The best prepared process was prepared time 6h and abstraction 3 times.The assaying method for baicalein by RP-HPLC was also established：Discovery ClS chromato bar,5 μm;The detecting wave length of ultra-violet was 275nm;The column temperature was 32℃ ;The flow rate was 1.0ml/min; The mobile phase was columbian spirit-water-glacial acetic acid （48：52：0.2）.Conclusions：The prepared process for baicalein is simple, accurate, reliable and has good reproducibility; This prepared process can be used as a common method for determining the baicalein content.