摘要
目的 建立芩蓟凉血颗粒的质量标准.方法 采用薄层色谱(TLC)法对制剂中黄芩、大蓟、生地黄、炙甘草、茜草(炭)进行定性鉴别,采用高效液相色谱(HPLC)法对制剂中槐角(炭)进行定性鉴别;采用HPLC法测定制剂中黄芩苷、柳穿鱼叶苷的含量,色谱柱为Dikma Platisil ODS柱(250 mm×4.6 mm,5µm),流动相为 0.1%磷酸溶液-乙腈溶液(梯度洗脱,黄芩苷、柳穿鱼叶苷)、0.07%磷酸溶液-乙腈-甲醇(68∶20∶12,V/V/V,槐角苷),检测波长为 280 nm(黄芩苷)、330 nm(柳穿鱼叶苷)、260 nm(槐角苷),柱温为 30℃,进样量为 10µL.结果 黄芩、大蓟、生地黄、甘草、茜草的TLC图斑点清晰,分离度好,且阴性对照无干扰;槐角苷专属性良好,且阴性对照无干扰.黄芩苷、柳穿鱼叶苷的质量浓度分别在 77.68～776.82µg/mL和 9.80～98.00µg/mL范围内与各自峰面积线性关系良好(r=1.000 0,n=6);精密度、稳定性、重复性试验结果的RSD均小于 2.5%(n=6);平均加样回收率分别为 97.15%和 94.34%,RSD分别为 2.08%和 3.00%(n=9).3 批样品中黄芩苷、柳穿鱼叶苷的平均含量分别为 30.620,0.947 mg/g.结论 所建立的方法操作简单、结果准确、专属性良好,可用于芩蓟凉血颗粒的质量控制.
Abstract
Objective To establish the quality standard for Qinji Liangxue Granules.Methods Thin-layer chromatography(TLC)method was used to qualitatively identify Scutellaria Baicalensis Radix,Cirsii Japonici Radix,Rehmanniae Radix,Glycyrrhizae Radix,and Rubiae Radix et Rhizoma(charred)in the preparation.High-performance liquid chromatography(HPLC)method was used to qualitatively identify Sophorae Fructus(charred)in the preparation.HPLC method was used to determine the content of baicalin and salidroside in the preparation,the chromatographic column was Dikma Platisil ODS column(250 mm×4.6 mm,5 µm),the mobile phases were 0.1%phosphoric acid solution-acetonitrile(gradient elution,baicalin,salidroside)and 0.07%phosphoric acid solution-acetonitrile-methanol(68∶20∶12,V/V/V,sophocarpin),the detection wavelengths were 280 nm(baicalin),330 nm(salidroside),and 260 nm(sophocarpin),the column temperature was 30℃,and the injection volume was 10 µL.Results The TLC spots of Scutellaria Baicalensis Radix,Cirsii Japonici Radix,Rehmanniae Radix,Glycyrrhizae Radix,and Rubiae Radix et Rhizoma were clear,with good separation,and no interference from the negative control.Sophorae Fructus had good specificity and the negative control has no interference.The linear ranges of baicalin and salidroside were 77.68-776.82 µg/mL and 9.80-98.00 µg/mL,respectively(r=1.000 0,n=6).The RSDs of precision,stability,and repeatability test results were all lower than 2.5%(n=6).The average recoveries of baicalin and salidroside were 97.15%and 94.34%,with RSDs of 2.08%and 3.00%,respectively(n=9).The average contents of baicalin and salidroside in three batches of samples were 30.620 and 0.947 mg/g,respectively.Conclusion The established method is simple,accurate,feasible,and has good specificity,which can be used for quality control of Qinji Liangxue Granules.
维普
万方数据