柴苓护肝颗粒的质量标准研究

Study on Quality Standard of Chailing Hugan Granules

目的:建立柴苓护肝颗粒的质量标准。方法:采用薄层色谱法(TLC)对制剂中柴胡、白术、甘草药材进行定性鉴别,采用紫外-可见分光光度法测定制剂中总黄酮(以芦丁计)的含量,并对制剂的水分、溶化性、粒度进行检查。结果:柴胡、白术、甘草的TLC图斑点清晰,分离度好,阴性对照无干扰。芦丁检测质量浓度线性范围为0.050～0.300 mg/mL(r=0.999 8);精密度、稳定性、重复性试验的RSD均小于2%;加样回收率为97.89%～100.01%(RSD=0.68%,n=9);样品含量为1.920～2.018 mg/g。3批样品的水分含量分别为1.54%、1.62%、1.57%,均在5 min内溶化,不能通过一号筛且能通过五号筛的总和分别为2.13%、2.51%、2.38%,均符合2015年版《中国药典》(四部)的规定。结论:初步拟定柴苓护肝颗粒中总黄酮的含量应不得低于1.57 mg/g(以芦丁计);所建质量标准的相关方法简便、快速、准确、重复性好,可用于柴苓护肝颗粒的质量控制。

OBJECTIVE:To establish the quality standard of Chailing hugan granules.METHODS:TLC was used for qualitative identification of Radix bupleuri,Atractylodes macrocephala and Glycyrrhiza uralensis.The content of total flavonoids(by rutin)in preparation was determined by UV-visible spectrophotometry.The moisture,dissolubility and granularity of preparation were determined.RESULTS:TLC spots of R.bupleuri,A.macrocephala and G.uralensis were clear and well-separated without interference from negative control.The linear range of rutin was 0.050-0.300 mg/mL(r=0.999 8).RSDs of precision,stability and reproducibility tests were all lower than 2%.The recoveries were 97.89%-100.01%(RSD=0.68%,n=9).The content of samples were 1.920-2.018 mg/g.The contents of moisture in 3 batches of samples were 1.54%,1.62%and 1.57%;all samples dissolved within 5 min.The sum of granules not passing through No.1 sieve and passing through No.5 sieve were 2.13%,2.51%,2.38%,which were all in line with the requirements of Chinese Pharmacopeia(2015 edition,VolⅣ).CONCLUSIONS:The content of total flavonoicle in Chailing hugan granules should be no less than 1.57 mg/g(by rutin).Established quality standard is simple,rapid,accurate and reproducible,and can be used for quality control of Chailing hugan granules.