消肿接骨贴中苷类成分的定性定量研究

目的:建立消肿接骨贴中苷类成分的定性定量方法。方法:应用薄层色谱(TLC)法对制剂中的续断和黄芪同时进行定性鉴别,以三氯甲烷-甲醇-水(13∶7∶2,V/V/V)的下层溶液为展开剂,10%(V/V)的硫酸乙醇溶液为显色剂。应用高效液相色谱(HPLC)法对制剂中的柚皮苷进行含量测定:色谱柱为Thermo C18(250 mm×4.6 mm,5μm),流动相为乙腈-水(18∶82,V/V),检测波长为283 nm。结果:续断和黄芪的TLC斑点清晰、分离良好,阴性对照无干扰。柚皮苷进样量在0.062 1⁰.621 0μg范围内与其峰面积积分值呈良好线性关系(r=0.999 7);精密度、稳定性、重复性试验的RSD<2%;平均加样回收率为99.31%,RSD=1.73%(n=9)。结论:本研究建立的方法专属性强、灵敏度高、简便、准确、重复性好,可以用于消肿接骨贴中苷类成分的定性定量研究。

Qualitative and Quantitative Study of Glycosides in Xiaozhong Jiegu Plasters

OBJECTIVE： To establish a method for qualitative and quantitative study of glycosides in Xiaozhong jiegu plaster. METHODS ：Dipsacus asper and Astragali Radix were identified simultaneously by TLC using chloroform-methyl alcohol-water（ 13： 7：2, V/V/V）as developing solvent and 10 % （V/V）sulfuric acid ethanol as chromogenic agent. HPLC method was used to determine the content of naringin. The determination was performed on Thermo C18（250 min×4.6 mm, 5 μm） with mobile phase consisted of acetonitrile-water（18 ： 82, V/V） and the detection wavelength was set at 283 nm. RESULTS： TLC spots ofD. asper and Astragali Radix were clear and well-separated without interference from negative control. The linear range of naringin was 0.062 1-0.621 0 μg （r=0.999 7） with an average recovery of 99.31% （RSD= 1.73 %, n=9）. RSD of precision, stability and reproducibility tests were all lower than 2%. CONCLUSIONS： The method is specific, sensitive, simple, accurate and reproducible, and it is suitable for qualitative and quantitative identification of glycosides in Xiaozhong jiegu plasters.