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作 者:储美娜[1] 董志[1] 朱毅[1,2] 陈国彪[2]
机构地区:[1]重庆医科大学,重庆400016 [2]海南省药品检验所海南省药物质量研究重点实验室,海口570216
出 处:《药物分析杂志》2012年第1期116-119,共4页Chinese Journal of Pharmaceutical Analysis
基 金:海南省重点科技项目(No.090125)
摘 要: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.
关 键 词:药用植物山乌龟 海南地不容(金不换) 巴马汀 延胡索乙素 防己诺林碱 粉防己碱 水分 总灰分 薄层色谱 高效液 相色谱 质量控制
分 类 号:R917[医药卫生—药物分析学]
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