无糖型外感风痧颗粒质量标准的研究

Study on quality standard of sugarless Waiganfengsha Granules

目的建立无糖型外感风痧颗粒质量控制的标准。方法使用薄层色谱法(TLC),以石油醚(60~90℃)-乙酸乙酯-冰醋酸(16∶2∶1)为展开剂,10%硫酸乙醇溶液为显色剂,定性鉴别藤苦参;以甲苯-乙酸乙酯-冰醋酸(10∶3∶1)为展开剂,紫外光灯(365 nm)下观察,定性鉴别岗梅;采用高效液相色谱法(HPLC),色谱柱:岛津C18色谱柱(4.6 mm×150 mm,5μm),流动相:乙腈-0.4%磷酸溶液(13∶87),流速0.5 ml/min,柱温25℃,检测波长327 nm,进样量10μl,采样时间60 min,对产品中的绿原酸进行含量测定。结果按TLC法,供试品色谱中,在与对照药材藤苦参色谱相应的位置上,显一个或一个以上相同颜色的斑点,在与对照药材岗梅色谱中相应的位置上,显一个或一个以上相同颜色的亮斑,斑点清晰,专属性强,重现性好,阴性无干扰;绿原酸进样量在6.2968~201.5μg范围内与峰面积线性关系良好(r=0.9991),平均回收率为100.11%,RSD=0.14%(n=6),测定10批无糖型外感风痧颗粒样品中绿原酸的平均含量为1.1069 mg/g(RSD=0.45%)。结论所采用的质量控制方法具有方法灵敏、专属性强、重现性好、稳定性高的特点,可作为无糖型外感风痧颗粒的质量标准控制方法。

Objective To set up the quality control standard of sugarless Waiganfengsha Granules.Methods Thin layer chromatography（TLC） was used,and petroleum ether（60-90℃）-ethyl acetate-glacial acetic acid（16 ∶2∶1） was the developing agent,and 10% sulfuric acid ethanol solution selected as the chromogenic agent to qualitatively identify Streptocaulon griffithii.Toluene-ethyl acetate-glacial acetic acid（10∶3∶1） was the developing agent,and it was observed under ultraviolet lamp（365 nm） to qualitatively identify Holly root.HPLC was used,chromatographic column：Shimadzu C18 chromatographic column（4.6 mm×150 mm,5 μm） was adopted,and mobile phase：acetonitrile-0.4% phosphoric acid solution（13∶87）,current speed：0.5 ml/min,and column temperature：25℃,detection wavelength was 327 nm,sample size：10 μl,and sampling time was 60 min.The content of chlorogenic acid in the product was determined.Results According to TLC method,in test sample chromatography,in the corresponding position with Streptocaulon griffithii chromatogram of contrast medicinal material,1 or more than 1 spots in same color were displayed while in the corresponding position with Holly root chromatogram of contrast medicinal material 1 or more than 1 bright spots in same color were displayed,and the spots were clear,and the specificity was strong with good reproducibility,and it had no interference of negative.Chlorogenic acid had a good linear relationship with peak area in the range of 6.2968-201.5 μg（r=0.9991） of sample size,and the average recovery rate was 100.11%,and RSD was 0.14%（n=6）.The average content of Chlorogenic acid was 1.1069 mg/g（RSD=0.45 %） among 10 batches of sample tablets.Conclusion The quality control method used has a characteristics of sensitive method,strong specificity,good reproducible and high stability,and it can be used as the quality standard control method of sugarless Waiganfengsha Granules.