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作 者:易艳萍[1] 邹盛勤[2] 谢晚彬[1] 陈武[1]
机构地区:[1]宜春学院化学与生物工程学院,江西宜春336000 [2]江西省天然药物活性成分研究重点实验室,江西宜春336000
出 处:《时珍国医国药》2008年第4期799-800,共2页Lishizhen Medicine and Materia Medica Research
基 金:国家“863”计划重点资助项目(No.2002AA2Z3217)
摘 要:目的提取鉴定毛泡桐叶中的乌索酸,并建立其含量测定方法。方法采用“醇提凝析法”新工艺分离制备乌索酸,IR,MS,NMR鉴定其结构。建立反相高效液相色谱测定其含量的方法,色谱柱为Krom asilC18柱,流动相为乙腈-甲醇-水-磷酸(体积比168∶682∶150∶1.68),流速0.8 m l/m in,检测波长210 nm,柱温25℃。结果乌索酸在0.92-16.56μg范围内线性关系良好(r=0.999 6)。样品乌索酸含量为99.61%,得率为30.5%。结论“醇提凝析法”分离制备乌索酸工艺先进,实用可行,为工业试验生产乌索酸提供了技术条件;RP-HPLC法测定乌索酸含量准确、精密度高、重复性好、线性范围宽,可作为控制乌索酸质量的方法。Objective:To extract and identify ursolic acid from Paulownia tomentosa (Thunb.) Steud leaves and to establish a determination method of ursolic acid. Methods:Ursolic acid was extracted from Paulownia tomentosa( Thunb. ) Steud leaves by adopting a new method of ethanol extraction and agglutination separation, and its structure was identified by IR, MS and NMR. A determination method of ursolic acid in Paulownia tomentosa ( Thunb. ) Steud leaves by reversed - phase high performance liquid chromtograph was established. The chromatographic column ( KromasilC18, 4.6 mm x 250 mm, 5μm ), acetonitrile - methanol -water- phosphoric acid mobile phase( 168:682:150:1.68, V/V) with 0.8 ml/min flow rate, the detected wavelength (210 nm) and the column temperature (25℃) were adopted. Results:Ursolic acid showed good linear relationship in the range of 0. 92 - 16.56μg( r = 0. 999 6 ). The average recovery rate was 99.82% ( RSD was 0.75% ). The content was 99.61% and the gain rate was 3.05‰. Conclusion: The method of ethanol extraction and agglutination separation to extract ursolic acid is ad- vanced, rational, practical and feasible, and it provides technology condition for industrial production of ursolic acid. RP - HPLC is simple and accurate, it has good repeatability and wider linear range, and it can be used to evaluate the quality of ursolic acid.
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