徐黄合剂的制备工艺优化及含量测定

Preparation Process Optimization and Content Determination of Xuhuang Mixture

优化徐黄合剂最佳提取工艺并建立制剂含量测定方法。以黄芪甲苷含量为提取工艺及含量测定评价指标,采用L_(9)(3^(4))正交试验法,选取加水量、煎煮时间及煎煮次数为考察因素确定最佳提取工艺,并考察常压浓缩和减压浓缩对黄芪甲苷含量的影响。另外建立黄芪甲苷高效液相色谱测定方法并进行方法学考察。结果显示,最佳提取工艺为加6倍量水,沸后提取1 h,提取2次;两种不同的浓缩方法对制剂含量影响无显著性差异;黄芪甲苷在0.048 16~0.963 20 mg/mL范围内线性关系良好,阴性样品无干扰,精密度、重复性、稳定性测得的RSD<3%;平均加样回收率为101.85%(RSD=2.54%,n=9),表明该含量测定方法灵敏、准确。

To optimize the extraction process of Xuhuang mixture and establish the determination method of content.Taking the content of Astragaloside IV as the index to evaluate the extraction process and content determination,and using the L9(34)orthogonal test to optimize the extraction process with the amount of water,decocting time and decocting times as investigation factors.The effects of concentration at atmospheric and vacuum pressure on the content of Astragaloside IV were investigated.In addition,a method for the detection of Astragaloside IV with high performance liquid chromatography was established and the methodology was investigated.The results showed that the best extraction process was as follow:the herbs were with twice decoction with one hour for each time,and the added water amount was 6-fold of the herbs.Concentration at atmospheric or vacuum pressure had no signif icant effect on Astragaloside IV’s content in the mixture.Moreover,the linear range was 0.04816-0.96320 mg/mL,the negative samples have no interference,and the RSD of precision,repeatability and stability were less than 3%.The average recovery was 101.85%(RSD=2.54%,n=9),which indicated the method was sensitive and accurate.