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    高效液相色谱法测定藜麦中齐墩果酸的含量

    Determination of Oleanolic Acid in Quinoa by High Performance Liquid Chromatography

    • 摘要: 建立了高效液相色谱法(HPLC)测定藜麦中齐墩果酸含量的方法。称取藜麦样品1.5 g,用甲醇40 mL和3 mol·L-1盐酸溶液10 mL溶解,超声提取20 min,再回流水解1.5 h,将其中的齐墩果酸转化成苷元,以排除杂质干扰。所得提取液以体积比为85:15的甲醇-0.1 mol·L-1乙酸铵溶液的混合液为流动相,采用HPLC分离并测定样品提取液中齐墩果酸的含量。结果表明:齐墩果酸的质量浓度在5~500 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.3 mg·kg-1;对藜麦样品进行3个浓度水平的加标回收试验,齐墩果酸的回收率为98.0%~101%,测定值的相对标准偏差(RSD,n=5)为4.2%~7.5%。方法用于12个实际样品的测定,齐墩果酸的检出量为0.51~21.26 g·kg-1

       

      Abstract: A method for determination of oleanolic acid in quinoa by high performance liquid chromatography (HPLC) was established. Quinoa sample of 1.5 g was dissolved in 40 mL of methanol and 10 mL of 3 mol·L-1 hydrochloric acid solution, and oleanolic acid was extracted by ultrasonic for 20 min, following by reflux hydrolysis for 1.5 h, which could convert oleanolic acid into aglycone in order to avoid the interference of impurities. A mixture of methanol and 0.1 mol·L-1 ammonium acetate solution at volume ratio of 85:15 was used as the mobile phase, and the content of oleanolic acid in the sample extract was determined by HPLC. As shown by the results, linear relationship between mass concentration of oleanolic acid and its peak area was kept in the range of 5-500 mg·L-1, with detection limit (3S/N) of 0.3 mg·kg-1. Recovery test was made on quinoa samples at 3 concentration levels by standard addition method, giving results in the range of 98.0%-101%, and RSDs (n=5) of the determined values ranged from 4.2% to 7.5%. This method was applied for determination of oleanolic acid in 12 actual samples, and the detection amounts of oleanolic acid were in the range of 0.51-21.26 g·kg-1.

       

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