海南地不容药材定性定量方法研究

Qualitative and quantitative study of Stephania hainanensis H.S.Lo et Y.Tsoong

目的:建立海南地不容药材的定性定量方法。方法:采用薄层色谱法对海南地不容药材进行定性鉴别;采用高效液相色谱法测定巴马汀、延胡索乙素、防己诺林碱、粉防己碱的含量,色谱柱为Hypersil-C18(4.6 mm×250 mm,5μm),流动相为甲醇-0.1%三乙胺体系,梯度洗脱,流速1.0 mL.min-1,柱温25℃,检测波长281 nm。参照中国药典2010年版一部所述方法测定水分及总灰分。结果:在薄层色谱鉴别中,延胡索乙素和巴马汀斑点分离效果良好,具专属性,可用于海南地不容药材的定性鉴别;高效液相色谱测定中,巴马汀、延胡索乙素、防己诺林碱、粉防己碱进样量分别在0.288～2.88,0.0978～0.815,1.44～9.60,0.116～0.776μg范围内线性关系良好(r=0.9997～0.9999);平均加样回收率(n=6)分别为97.4%,98.3%,100.8%,97.9%。结论:所建立的方法可准确地对海南地不容进行定性、定量分析,用于其质量控制。

Objective：To establish a qualitative and quantitative method for Stephania hainanensis H. S. Lo et Y. Tsoong. nethods：TLC method was used for qualitative identification;An HPLC system was used in the quantitative analysis of four compounds of palmatine, tetrahydropalmatine, fangchinoline and tetrandrine on the analytical column of Hypersil - C18 （4. 6 mm × 250 mm ,5 μm）, the mobile phase was methanol -0. 1% triethylamine with gradient elution at a flow rate of 1.0 mL · min^-1 ,the detection wavelength was 281 nm and the column temperature was 25 ℃. The contents of moisture and ash were determined with the methods in Chinese Pharmacopeia（ChP） 2010. Resuits： Tetrahydropalmatine and palmatine could be identified by TLC ; In the system of HPLC, palmatine, tetrahydropalmatine, fangchinoline and tetrandrine showed good linear relationship in the ranges of 0. 288 - 2.88 （ r = 0. 9997） ,0. 0978 - 0. 815 （ r = 0. 9999 ）, 1.44 - 9.60 （ r = 0. 9998 ）, and 0. 116 - 0. 776 （ r = 0. 9997 ） μg, respectively. The average recoveries （ n = 6） were 97.4% , 98.3%, 100.8 % and 97.9% , respectively. Conclusion： The methods can be used exactly for the qualitative and quantitative analysis of Stephania hainanensis H. S. Lo et Y. Tsoong.