摘要
乌奴龙胆为常用的藏药,但其质量标准仅有性状鉴别项。作为2015年版《中国药典》民族药质量标准提高的拟定品种,该研究建立该品种质量控制方法与标准。参照《中国药典》2010年版附录相关方法,对乌奴龙胆药材水分、灰分、酸不溶性灰分及醇溶性浸出物进行测定;以乌奴龙胆苷A为对照物质,建立薄层鉴别方法;采用HPLC建立主要成分乌奴龙胆苷A的含量测定方法。结果以三氯化铝试液为显色剂,乌奴龙胆中各成分在紫外光灯（366 nm）下检视,能得到较好的分离,在与对照品的相应位置上显示相同的颜色荧光斑点;含量测定方法学研究结果表明,乌奴龙胆苷A在0.009 95~0.398 g·L-1呈良好的线性关系,回归方程为Y=1 467.1X＋41.407（r=0.999 9）,平均回收率为98.3%（RSD 2.2%）。15批乌奴龙胆药材样品的测定结果表明,乌奴龙胆苷A的质量分数为0.175%~1.83%;醇溶性浸出物为29.2%~35.2%,水分为8.60%~9.93%;10批代表性样品总灰分范围在10.2%~17.2%;酸不溶性灰分范围在5.26%~10.8%。以上结果表明建立的标准具有较好的专属性和准确性,可用于乌奴龙胆药材的质量控制。建议规定乌奴龙胆药材的水分含量不超过12.0%;总灰分不得过15.0%;酸不溶性灰分不得过8.0%;浸出物不得少于26.0%;含乌奴龙胆苷A（C40H52O22）不得少于0.80%。
Gentianae Urnulae Herba, dried whole herb of Gentiana urnula,is a commonly used Tibetan medicine. However, only the character identification is used as quality control standard officially at present. As a part of project for the Chinese Pharmacopoeia （2015 edition）, the quality standard of this species was established in this study. The tests of water content, total ash, acid-insoluble ash and ethanol-soluble extractives of the （：rude drugs were carried out following the methods recorded in appendix of Chinese Pharmacopeia（ 2010 edition, volume 1 ）. The TLC identification method was established by using gentiournoside A as reference substance, and a mixture of ethyl acetate-methanol-water-formic acid（7： 1.5： 1： 0. 2） as the developing solvent system on silica gel G TLC plate. The content of gentiournoside A was assayed by HPLC on an Agilent Zorbax SB-C18 （4- 6 mm μ250 mm,5 mm）column, using acetonitrilewater（0. 1% phosphoric acid） （26： 74） as the mobile phase at a flow rate of 1.0 mL - min-1. The column temperature is at 30 ℃and the detection wavelength is at 240 nm. As a result, gentiournoside A and the other constituents were separated and presented the same fluorescence light comparing with the reference substance on TLC detected under the UV light （366 nm）. The methodology validation for the assay of gentiournoside A showed that it was in a good linear correlation in the range of 0. 009 95-0. 398 g· L- 1 with the regression equation of Y= 1 467. 1X ＋41. 407（r =0. 999 9）, and the average recovery was 98.3% （ RSD 2.2% ）. The mass fractions of gentiournoside A, water content, ethanol-soluble extraetives of 15 batches samples were varied in the ranges of 0. 175%-1. 83% , 8.60%- 9.93% and 29.2% -35.2% , respectively. Total ash and acid-insoluble ash were 10. 2% -17.2% and 5.26% -10. 8% detected from 10 batches samples. The recommended standards of quantitative indexes are that the mass fractions of gentiournoside A and extraetives are not less than 0.80% and 26.
出处
《中国中药杂志》
CAS
CSCD
北大核心
2015年第19期3878-3882,共5页
China Journal of Chinese Materia Medica
基金
上海市自然基金项目(14ZR1441200)
上海市教委创新项目(13YZ046)
2015年版中国药典标准提高项目(M14)
