发酵虫草菌粉片剂的溶出度测定方法研究

Dissolution Determination Method of Fermented Cordyceps Mycelia Powder Tablets

目的:建立一种发酵虫草菌粉片的溶出度测定方法,以评价相关产品的质量差异。方法:采用溶出度测定法(小杯法),以pH 1.2盐酸溶液为溶出介质,转速50r·min^(-1),温度37℃,分别于5、10、20、30、45、60 min取样。采用HPLC法进行测定,色谱柱C_(18)(250 mm×4.6 mm,5μm),流动相为甲醇-0.1 mol·L^(-1)磷酸二氢钾(10∶90),流速为1.0 mL·min^(-1),检测波长为254 nm;以外标法定量计算。结果:腺苷在2.0437~51.0196μg·mL^(-1)范围内与峰面积线性关系良好(r=0.999),平均回收率在98.1~100.1%,RSD=0.6%(n=6)。15批产品中11批的溶出度>80%,其他4批<80%。不同企业间样品溶出曲线存在差异,企业内批间也存在差异。结论:该方法操作简单,专属性强,精密度、稳定性、重复性和准确度好,能反映不同企业不同批次产品的质量差异,可为发酵虫草菌粉固体制剂的质量控制提供参考。

Objective:To establish a dissolution determination method in order to evaluate the quality differences of related products.Methods:Using dissolution determination method(small cup method),hydrochloric acid solution(pH 1.2)was used as the dissolution medium.The speed was 50 r·min^(-1).The temperature was 37℃,and the samples were taken at 5,10,20,30,45,and 60 minutes.The determination method was HPLC,and the chromatographic column was C_(18)(250 mm×4.6 mm,5μm).The mobile phase was methanol:0.1 mol·L^(-1)potassium dihydrogen phosphate(10∶90),and the flow rate was 1.0 mL·min^(-1).The detection wavelength was 254 nm.Quantitative calculation was through the external standard method.Results:Adenosine was 2.0437-51.0196μg·mL^(-1),there was a good linear relationship between peak area and concentration(r=0.999),the average recovery rate was 98.1-100.1%and the RSD of was 0.6%(n=6).Among the 15 batches of products,the dissolution rate of 11 batches was Above than 80%,the dissolution rate of 4 batches was under than 80%.There are differences in the dissolution curves of products between different enterprises,and there are also differences in products within enterprises.Conclusion:The method was easy to operate,and has strong specificity,good precision,stability,repeatability,and accuracy,and can reflect the quality differences of different batches of products from different enterprises.It can provide reference for the quality control of fermented cordyceps powder solid preparations.