蔓生百部质量标准研究

目的: 为控制蔓生百部药材的质量,建立蔓生百部药材的显微和薄层鉴别、水分、总灰分、酸不溶性灰分、浸出物以及含量测定标准。方法: 从全国范围内收集10批蔓生百部药材,采用横切面及粉末进行显微鉴别;TLC法对生物碱类成分进行薄层鉴别;采用中国药典附录方法,对水分、总灰分、酸不溶性灰分、浸出物进行测定;HPLC法测定蔓生百部中原百部碱含量,采用Phenomenex Gemini C₆-phenyl色谱柱(250 mm×4.6 mm,5 μm),流动相为乙腈-0.1%三乙胺(34:66),流速1.0 mL·min^-1,检测波长306 nm,柱温为30 ℃。结果: 与中国药典2010年版一部相比增加了质地、断面、气味、根被细胞的特征、中柱中韧皮部束与木质部束的个数和粉末特征等内容。增加的薄层色谱鉴别色谱斑点清晰,分离度较好。含量测定,原百部碱浓度在10.9~218.7 mg·L^-1范围内线性关系良好(r=1.0000),平均回收率为99.7%(RSD为1.6%,n=6)。结论: 本文建立的显微鉴别、检查、TLC鉴别及含量测定方法,可用于蔓生百部药材的质量标准。

Objective: To control the quality of root tuber of Stemona japonica (Bl.)Miq.by establishing standards of transverse section,powder,TLC,water,total ash,acid-insoluble ash,extractives and assay. Methods: The quality standards were established based on 10 batches of Stemona japonica (Bl.)Miq. samples from nationwide.Transverse section and powder were used for analysis of microscopic characteristics.TLC was adopted to analyze the alkaloid components.Water,total ash,acid-insoluble ash and extractives were determined by methods in the appendices of Chinese Pharmacopoeia.The content of protostemonine was determined by HPLC.The Phenomenex Gemini C₆-phenyl column(250 mm×4.6 mm,5 μm)was used,the mobile phase was acetonitrile-0.1% triethylamine(34:66)at a flow rate of 1.0 mL·min^-1,the column temperature was 30 ℃,and the detection wavelength was at 306 nm. Results: Compared with the Chinese Pharmacopoeia(2010 Version,Volume Ⅰ),texture,fracture,odor,taste,microscopic characteristics of velamen,the number of phloem bundles and xylem bundles in stele,and microscopic identification of powder were supplied.The TLC was added and its spots developed were fairly and simply identical.The concentration of protostemonine showed a good linear relationship at the range of 10.9-218.7 mg·L^-1(r=1.0000), the average recovery was 99.7%(RSD was 1.6%,n=6). Conclusion: The method established in this paper such as microscopic identification,inspection,TLC identification and content determination,can be used for the quality standard of roots of Stemona japonica (Bl.)Miq.medicinal materials.