知识与财富的链接
为了对绿豆药材进行有效的质量控制,该研究建立了绿豆药材的质量控制方法与标准。参照《中国药典》2010年版附录相关方法,对绿豆药材的水分、灰分及醇溶性浸出物进行测定;采用薄层色谱法,以硅胶GF254为薄层板,乙酸乙酯-甲醇-水 （10：1.7：1.3）为展开剂,以牡荆苷和异牡荆苷为对照,建立其薄层鉴别方法;采用HPLC建立主要有效成分牡荆苷和异牡荆苷的含量测定方法： 采用Prevail C18 （4.6 mm×250 mm,5 μm）色谱柱,以乙腈-水（23：77）为流动相,流速1.0 mL·min-1,柱温30℃;检测波长337 nm。结果绿豆中各成分在紫外光灯（254 nm）下检视,能得到较好的分离;含量测定方法学研究结果表明,牡荆苷在6.12~98 mg·L-1,异牡荆苷在6.85~109.6 mg·L-1线性关系良好,回归方程分别为Y=46.213X-7.100 （r=1.000）和Y=54.515X+6.829（r =1.000）;平均回收率分别为98.2%（RSD 1.9%）和97.2%（RSD 0.79%）。25批绿豆药材样品的测定结果表明,牡荆苷的质量分数为1.076~2.062 mg·g-1,异牡荆苷的质量分数为1.127~2.303 mg·g-1,不同产地样品中牡荆苷和异牡荆苷的含量差异不大;醇溶性浸出物的结果为13.27%~18.46%,水分为9.59%~12.43%,总灰分为2.63%~3.53%。上述结果表明建立的标准具有很好的专属性和准确性,可用于绿豆药材的质量控制。
In order to control the quality of Vigna radiata, the quality control method and standard were established in this study. The tests of water content, ash and ethanol-soluble extractives of V. radiata were carried out according to the methods recorded in appendix of Chinese Pharmacopeia (2010 edition, volume 1). The TLC method was established by using vitexin and isovitexin as references, and a mixture of acetate-method-water(10:1.7:1.3)as the developing solvent system on GF254 thin layer plate. The contents of vitexin and isovitexin were determined by HPLC on a Prevail C18 (4.6 mm×250 mm, 5 μm) column, using acetonitrile:water (23:77) as mobile phase at a flow rate of 1.0 mL·min-1. The column temperature is 30℃ and the detection wavelength is 337 nm. As a result, vitexin, isovitexin and the other constituents were well separated on TLC detected under the UV light (254 nm). The methodology validation for the assay of vitexin and isovitexin presented that they were in good linear correlation in the ranges of 6.12-98 mg·L-1 and 6.85-109.6 mg·L-1, with the regression equations of Y=46.213X-7.100(r=1.000) and Y=54.515X+6.829 (r=1.000), and the average recoveries were 98.2% (RSD 1.9%) and 97.2% (RSD 0.79%), respectively. The content ranges of vitexin and isovitexin from 25 different batches of V. radiata were 1.076-2.062 mg·g-1 and 1.127-2.303 mg·g-1, respectively, suggesting that the qualities of V. radiata are relatively stable. The ethanol-soluble extractives, water content and total ash of 25 samples varied in the ranges of 13.27%-18.46%, 9.59%-12.43% and 2.63%-3.53%, respectively. All of the above data proved that the established quality of coutrol method V. radiata is specific and accurate, which can be used for the quality control of this drug.
