直立百部质量标准研究

目的：为控制直立百部药材的质量，建立直立百部药材的显微鉴别、薄层鉴别、水分、总灰分、酸不溶性灰分、浸出物和含量测定标准。方法：采用横切面及粉末进行显微鉴别；采用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；采用HPLC法测定直立百部中原百部碱含量，色谱条件：色谱柱为Phenomenex Gemini C₆-phenyl（250 mm×4.6 mm，5 μm），流动相为乙腈-0.1%三乙胺（34：66），柱温为30 ℃，流速为1.0 mL·min^-1，检测波长306 nm。结果：横切面及粉末的显微特征与中国药典及文献记载基本一致，唯中柱中韧皮部束与木质部束的个数不同于药典规定。薄层鉴别色谱斑点清晰，分离度较好。含量测定中原百部碱在6.257~156.42 mg·L^-1浓度范围内线性关系良好（r=0.9998），平均回收率为100.2%（RSD为1.6%，n=6）。结论：本文采用的方法操作简便，准确，重复性好，可用于控制直立百部药材的质量。

Objective: To control the quality of root tuber of Stemona sessilifolia(Miq.)Miq by establishing standards of transverse section,powder,TLC,water,total ash,acid-insoluble ash,extractives and assay. Methods: The quality standards were established according to 10 batches of Stemona sessilifolia (Miq.)Miq samples from nationwide.Microscopical characteristics were studied for transverse section and powder.TLC was adopted to analyze the alkaloids components.Water,total ash,acid-insoluble ash and extractives were determined by methods described in appendices of Chinese Pharmacopoeia.The content of protostemonine was determined by HPLC.The Phenomenex Gemini C₆-phenyl(250 mm×4.6 mm,5 μm)column was used,the mobile phase was acetonitrile-0.1% triethylamine(34:66),the column temperature was 30 ℃,the flow rate was 1.0 mL·min^-1,and the detection wavelength was at 306 nm. Results: Microscopical characteristics of transverse section and powder were in good accordance with Chinese Pharmacopoeia(2010 version,volume I)and literatures,except the number of phloem bundles and xylem bundles in stele.The TLC showed the spots developed clearly and the separation was good.The concentration of protostemonine showed a good linear relationship in the range of 6.2569-156.42 mg·L^-1(r=0.9998),and the average recovery was 100.2%(RSD was 1.6%,n=6). Conclusion: The method is simple,accurate with good reproducibility and can be used for the quality control of roots of Stemona sessilifolia(Miq.)Miq.