藏药材苞叶雪莲质量控制方法研究

Quality control method of Tibetan medicine Saussureae obvalltae

为了对藏药材苞叶雪莲进行有效的质量控制,该研究建立了藏药苞叶雪莲的质量控制方法与标准。参照2010年版《中国药典》附录相关方法,对苞叶雪莲药材的水分、灰分、酸不溶性灰分及醇溶性浸出物进行测定;采用显微鉴别,对苞叶雪莲全草及其叶子的粉末建立显微鉴别方法;采用薄层色谱法,以硅胶G为薄层板,乙酸乙酯-丁酮-甲酸-水(10∶6∶1∶2)的上层溶液为展开剂,以绿原酸和芦丁为对照,建立其薄层鉴别方法;采用Agilent ZORBAX Eclipse XDB-C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-0.1%磷酸溶液(17∶83)为流动相,流速为1.0 m L·min^(-1),柱温40℃,检测波长为350 nm。结果不同产地的藏药材苞叶雪莲全草及其叶子的显微特征一致;薄层色谱在日光下检视,能得到较好的分离;含量测定方法学研究结果表明,绿原酸在0.119 2~0.715 4μg(r=0.999 9),芦丁量在0.160 7~0.964 4μg(r=1.000),与峰面积呈良好的线性关系,平均回收率分别为105.4%(RSD 1.4%)和99.50%(RSD 0.91%);醇溶性浸出物的结果为26.01%~31.59%;水分为7.16%~8.04%,总灰分为8.46%~11.14%,酸不溶性灰分为0.50%~1.87%。上述结果表明建立的方法具有良好的专属性和准确性,可用于藏药苞叶雪莲药材的质量控制。

To control the quality of Tibetan medicine Saussureae obvalltae,the quality control method and standard were established in this study. The water content,total ash,acid-insoluble ash and ethanol-soluble extractives of Saussureae obvalltae were determined according to the methods recorded in appendix of Chinese Pharmacopeia（ 2010 edition）. Microscopical identification was performed for the plant and powder of the leaves. The TLC method was established,with chlorogenic acid and rutin as control substances,and a mixture of acetate-btuanone-formic acid-water（ 10∶ 6 ∶ 1 ∶ 2） as developing solvent and silica gel G as thin layer plate. Agilent ZORBAX Eclipse XDB-C18（ 4. 6 mm × 250 mm,5 μm） column was adopted and eluted with the mobile phase of acetonitrile-0. 1% phosphoric acid（ 17∶ 83） in a gradient mode at a flow rate of 1. 0 m L·min^- 1. The column temperature was 40 ℃ and the detection wavelength was 350 nm. As a result,the plant and leaves of Saussureae obvalltae of different origins showed constent microscopic features. Chlorogenic acid,rutin and the other constituents were well separated on TLC detected under the sun light. According to the results of the methodological study,chlorogenic acid and rutin were in good linear correlation in the ranges of 0. 119 2-0. 715 4 μg（ r = 0. 999 9） and0. 160 7-0. 964 4 μg（ r = 1. 000）,and the average recoveries were 105. 4%（ RSD 1. 4%） and 99. 50%（ RSD 0. 91%）,respectively. The content of ethanol-soluble extractives,water content,total ash and acid-insoluble ash were 26. 01%-31. 59%,7. 16%-8. 04%,8. 46%-11. 14%,0. 50%-1. 87%,respectively. According to the study,the established method was specific and accurate,which could be used for the quality control of this drug.