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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。
In order to establish the quality standard of Qinhuang Qingfei San, the qualifications of Radix Scutellariae, rhubarb, loquat leaf and licorice were qualitatively identified by means of microtitration and TLC. The content of baicalin was determined by high performance liquid chromatography (HPLC). The column was Eluting C18 column (250 mm × 4.6 mm, 5 μm). The mobile phase was methanol-water-phosphoric acid (47:53:0.2) / min; detection wavelength 280nm; column temperature 40 ℃; injection volume 20μL. The results of microscopic examination showed that the bast fibers were single or in bundles with a spindle shape with a length of 60μm ~ 250μm, wall thickness, pore ditch (Scutellaria baicalensis), calcium oxalate family crystal with a diameter of 60μm ~ 140μm (rhubarb) Hair is a single cell, often curved (loquat leaf); wood fibers into bundles, the surrounding parenchyma cells contain calcium oxalate crystals, crystal sheath fibers (licorice). TLC results show that for the test, in the reference substance or reference drug chromatography corresponding position shows the same color spots, the negative control without interference. The results of HPLC showed that the linear range of baicalin was 0.241μg ~ 1.208μg (r = 0.999 9), the RSD of precision, stability and repeatability was less than 3.0% and the recovery was 100.49% (RSD = 1.71% , n = 9). The Institute established standards for the quality control of Qinhuang Qingfei Powder.