芩黄清肺散的质量标准研究

Study on Quality Standard of Qinhuang Qingfei Powder

为建立芩黄清肺散的质量标准,采用显微鉴定和薄层色谱法(TLC)对方剂中黄芩、大黄、枇杷叶和甘草进行定性鉴别。采用高效液相色谱法(HPLC)对黄芩苷进行含量测定,色谱柱为依利特C18柱(250mm×4.6mm,5μm);流动相为甲醇-水-磷酸(47∶53∶0.2);流速1mL/min;检测波长280nm;柱温40℃;进样量20μL。显微鉴定结果表明,韧皮纤维单个散在或数个成束,梭形,长60μm^250μm,壁厚,孔沟细(黄芩);草酸钙族晶,直径60μm^140μm(大黄);非腺毛为单细胞,常弯曲(枇杷叶);木纤维成束,周围薄壁细胞含草酸钙方晶,形成晶鞘纤维(甘草)。TLC结果表明,供试品中,在与对照品或对照药材色谱相应的位置上显示相同颜色的斑点,阴性对照无干扰。HPLC结果显示,黄芩苷在0.241μg^1.208μg(r=0.999 9)具有良好的线性范围,精密度、稳定性、重复性的RSD<3.0%,加样回收率为100.49%(RSD=1.71%,n=9)。该研究所建立标准可用于芩黄清肺散的质量控制。

The objective was to establish the quality standard of Qinhuang Qingfei powder.The qualitative identification of Radix Scutellariae,Radix et Rhizoma Rhei,Folium Eriobotryae and Radix et Rhizoma glycyrrhizae was conducted by microscopic identification and thin layer chromatography(TLC)in the prescription.The content of baicalin in the prescription was determined by high performance liquid chromatography(HPLC):the column was elite C18column(250 mm×4.6 mm,5μm)with the mobile phase of methanol-water-phosphoric acid(47∶53∶0.2)at a flow rate of 1mL/min;the detection wavelength was280nm;column temperature was 40℃;and the injection volume was 20μL.The results of microscopic identification were showed below.Phoem fibers scattered singly or in bundles,fusiform,60μm-250μm long,thick-walled,with fine pit-canals(Radix Scutellariae).Clusters of calcium oxalate,60μm-140μm in diameter(Radix et Rhizoma Rhei).Non-gland hairs,large,unicellular and curved(Folium Eriobotryae).Xylem fibers in bundles,which were surrounded by parenchymatous cells containing prisms of calcium oxalate and formed crystal sheath-fibres(Radix et Rhizoma glycyrrhizae).TLC results showed that there were the same color spots on the chromatography corresponding positions between test samples and reference substance or reference drug,and no interference in negatiive control.The linear range of the carlibation was 0.241μg-1.208μg(r=0.999 9).The RSDs of precision,stability and reproducibility tests were lower than 3.0%.The recovery rate was 100.49%(RSD=1.71%,n=9).The established standard can be used for the quality control of Qinhuang Qingfei powder.