四季草颗粒质量标准提升研究

Improvement of Sijicao Granule Quality Standard

目的:改进四季草颗粒头花蓼的TLC鉴别方法,分别建立四季草颗粒质量标准中车前草的TLC鉴别和槲皮苷的HPLC含量测定方法。方法:TLC法以聚酰胺为固定相,分别用甲醇-甲酸(10∶1)和30%醋酸为展开剂,采用头花蓼和车前草对照药材鉴别方中头花蓼和车前草;HPLC法采用C18色谱柱,以甲醇-0.1%磷酸水溶液为流动相,流速1.0 ml/min,检测波长360 nm,柱温40℃,测定槲皮苷含量。结果:头花蓼和车前草的TLC检出明显,阴性无干扰;槲皮苷含量测定中进样浓度在0.012 5～0.201 g/L的范围内线性关系良好(r=0.999 9),平均加样回收率为99.84%,RSD为2.6%(n=9),方法耐用性良好。结论:四季草颗粒中头花蓼和车前草药材TLC鉴别和含量测定方法可用于该制剂的质量控制。

Objective： To improve thin layer chromatography （ TLC ） method for identification of Polygonum capitatum in Sijicao granules, and to establish TLC method and high pressure liquid chromatography （HPLC） method for determination of Plantago asiatica and quercitrin contents in Sijicao granules respectively. Method： TLC tests were carried out using polyamide as stationary phase, methanol-formic acid （10：1 ） and 30% acetic acid as developing phase and Polygonum capitatum and Plantago asiatica as reference medicinal materials. HPLC was carried out on C18 column （40 °C ） using methanol -0.1% phosphoric acid as mobile wavelength of 360nm. Results： The TLC methods phase, and a flow rate of 1.0 ml/min, detection were effective in detection of Polygonum capitatum and Plantago asiatica, and the negative one didnt exhibit interference. The calibration curve for quer- citrin was linear in the range of 0. 012 5 ~0.201 g/mL. The average recovery was 99.48%, and PSD was 2.6% （n = 9 ）. The method was reproducible. Conclusion： The established TLC and HPLC methods for determination of Polygonum capitatum and Plantago asiatica can be employed in the quality control of Siiicao zranules.