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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,5μm),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 100 medicinal plants, establish microscopic and lamellar identification, water content, total ash content, acid-insoluble ash content, extract content and determination standards of 100 medicinal materials. Methods: Ten batches of wild herbs were collected from all over the country. The cross-sections and powder were used for microscopic identification. TLC was used to identify alkaloid constituents. The Chinese Pharmacopoeia appendix was used to analyze the water, total ash, acid-insoluble Ash and leachate were determined by HPLC. Phencynex was measured on a Phenomenex Gemini C6-phenyl column (250 mm × 4.6 mm, 5 μm) using a mobile phase of acetonitrile-0.1% triethylamine (34: 66), the flow rate was 1.0 mL · min-1, the detection wavelength was 306 nm and the column temperature was 30 ℃. Results: Compared with the first edition of Chinese Pharmacopoeia (2010 edition), the contents of texture, cross section, odor, root cells and cells, the number of phloem bundles and xylem bundles in the middle column and powder characteristics were increased. Increased thin layer chromatography identification Chromatography spots clear, better resolution. The linear range was 10.9 ~ 218.7 mg · L-1. The average recovery was 99.7% (RSD = 1.6%, n = 6). Conclusion: The method of microscopic identification, examination, TLC identification and content determination established in this paper can be used for the quality standard of Chinese herbal medicine.