摘要
目的:建立芩栀鱼合剂的质量标准.方法:运用薄层鉴别(TLC)的方法对芩栀鱼合剂中鱼腥草、甘草、黄芩三味中药进行鉴别;运用高效液相(HPLC)的方法对芩栀鱼合剂中特征性成分黄芩苷、栀子苷的含量进行测定,色谱柱C18(250 mm×4.6 mm,5 μm,Wondasil);流动相为乙腈-0.1%甲酸水溶液(梯度洗脱);柱温为 30℃;流速为1.0 mL·min-1;进样量为10 μL;检测波长分别为283 nm(黄芩苷)、238 nm(栀子苷).结果:鱼腥草、甘草、黄芩薄层色谱(TLC)图专属性强、特征明显且阴性对照无干扰;黄芩苷、栀子苷分别在浓度26.14～261.40 μg·mL-1(r=0.9999,n=6)、20.40～204.00 μg·mL-1(r=0.9997,n=6)范围内与对应浓度的峰面积线性关系良好;黄芩苷和栀子苷平均加样回收率分别为 99.50%(RSD=1.39%,n=6)和 98.97%(RSD=1.10%,n=6);方法学考察验证,两种特征性成分含量测定方法均符合要求.结论:所建方法操作简单、可行性强且结果准确,适用于芩栀鱼合剂的质量控制.
Abstract
Objective:To establish the quality standard for Qinzhiyu mixture.Methods:Houttuyniae Herba,Glycayrrhizae Radix et Rhizoma and Scutellarie Radix were qualitatively identified by TLC method;the contents of baicalin and geniposide in Qinzhiyu mixture were deter mined by HPLC on a C18 analytical column(Wondasil,250 mm×4.6 mm,5 μm),and the mobile phase was composed of acetonitrile-0.1%formic acid solution with gradient elution,the column temperature was 30℃,the flow rate was 1.0 mL·min-1,the volume injection was 10 μL and the detection wavelengths were 283 nm(baicalin)and 238 nm(geniposide).Results:The TLC identification characteristics of Houttuyniae Herba,Glycayrrhizae Radix et Rhizoma and Scutellarie Radix were obvious and specific without negative interference;the linear range of baicalin and geniposide were 26.14～261.40 μg·mL-1(RSD=1.39%,n=6)and 20.40～204.00 μg·mL-1(RSD=1.10%,n=6);the average recovery was 99.50%(RSD=1.39%,n=6)and 98.97%(RSD=1.10%,n=6),respectively.The results of the methodological investigation showed that the contents of all index components met the requirements.Conclusion:The method has been established is simple,feasible and accurate,which can be used for the quality control of Qinzhiyu mixture.
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