高效液相色谱法测定栀子中的活性成分
摘要
本文研究了中药栀子（Gardenia jasmindies Eills）中三种高效活性成分——栀子苷（Geniposide）、京尼平（Genipin）和栀子苷酸（Geniposide acid）的高效液相色谱测定方法。通过对样品预处理，流动相的种类，流动相的配比以及检测流速等条件进行优化，确定了高效液相色谱法测定栀子苷、京尼平和栀子苷酸的方法。（1）确定测定栀子苷的最佳测定条件为：λ=238nm，大连依利特C18色谱柱（4.6mm×250mm，5μm），甲醇-水（60：40）为流动相，分析时间10min,栀子苷浓度在0.01～0.2mg·mL~(-1)范围内峰面积与进样量呈良好的线性关系，平均回收率为102.30%。（2）以甲醇-水（60：40）为流动相，在λ=238nm，C18色谱柱（4.6mm×250mm，5μm）的色谱条件下，分析时间为10min,京尼平在0.01～0.2mg·mL-1范围内峰面积与进样量呈良好的线性关系，得到回归方程为Y=3.31×10~(7)X+22321，R=0.9997。（3）设定流速为0.4mL·min-1时，在λ=236nm处，高效液相测定栀子中活性成分栀子苷酸，进样浓度在0.01～0.3mg·mL-1范围内，栀子苷酸的出峰时间为4.758min，线性关系良好，平均回收率为102.19%，RSD=0.71%。
由于栀子苷、京尼平和栀子苷酸的高效液相色谱检测的波长、所采用的色谱柱、流动相等因素相似，确定了一种简便的同时测定栀子苷、京尼平和栀子苷酸的高效液相色谱方法。该方法具有重复性好、准确、快速等优点，适用于栀子苷、京尼平和栀子苷酸的同时测定。
This paper established methods for determination of three high-active ingredients inChinese medicine Gardenia jasmindies Eills by high performance liquid chromatographic,including geniposide,genipin and geniposide acid.Through the optimizations of the samplepretreatment,the type of mobile phase, the ratio of mobile phase and test conditions, ect,determined the methods of determination of genoposide,genipin and geniposide acid byHPLC.(1)Determined the best determination conditions for geniposide,the detection wave-length was238nm,Elite C18chromatographic column (4.6mm×250mm,5μm) was used, themobile phase was methanol and water (60:40),the analytical time is10min,with the con-centration of geniposide in the range of0.01～0.2mg·mL-1,the peak area had a good line-ar relationship with the injection quantity of the sample, the average recovery rate was102.30%.(2) With methanol and water(60:40) as the mobile phase, in the wavelength of238nm,using C18chromatographic column (4.6mm×250mm,5μm) and analyzing for10min, the concentration of genipin in the range of0.01～0.2mg·mL-1, the injection quantityof the sample and its peak area had a good linear relationship and getted the regressionequation is Y=3.31×10~(7)X+22321，R=0.9997.(3)Setted the velocity at0.4mL·min-1,in thewavelength of236nm,determinated the active-ingredient geniposide acid in gardenia, inthe range of0.01～0.3mg·mL-1of sample concentration,the peak time is4.758min,had agood linear relationship and the average recovery is102.19%,RSD is0.71%.
For the similitude of the factors for determinations of geniposide,genipin and genipo-side acid by HPLC,such as the wavelength,the chromatographic column and the velocity,established a simple method for determination of geniposide,genipin and geniposide acidsimultaneously by HPLC.This method is repeatable,accurate,rapid and effective for thesimultaneous determination of geniposide,genipin and geniposide acid.
由于栀子苷、京尼平和栀子苷酸的高效液相色谱检测的波长、所采用的色谱柱、流动相等因素相似，确定了一种简便的同时测定栀子苷、京尼平和栀子苷酸的高效液相色谱方法。该方法具有重复性好、准确、快速等优点，适用于栀子苷、京尼平和栀子苷酸的同时测定。
This paper established methods for determination of three high-active ingredients inChinese medicine Gardenia jasmindies Eills by high performance liquid chromatographic,including geniposide,genipin and geniposide acid.Through the optimizations of the samplepretreatment,the type of mobile phase, the ratio of mobile phase and test conditions, ect,determined the methods of determination of genoposide,genipin and geniposide acid byHPLC.(1)Determined the best determination conditions for geniposide,the detection wave-length was238nm,Elite C18chromatographic column (4.6mm×250mm,5μm) was used, themobile phase was methanol and water (60:40),the analytical time is10min,with the con-centration of geniposide in the range of0.01～0.2mg·mL-1,the peak area had a good line-ar relationship with the injection quantity of the sample, the average recovery rate was102.30%.(2) With methanol and water(60:40) as the mobile phase, in the wavelength of238nm,using C18chromatographic column (4.6mm×250mm,5μm) and analyzing for10min, the concentration of genipin in the range of0.01～0.2mg·mL-1, the injection quantityof the sample and its peak area had a good linear relationship and getted the regressionequation is Y=3.31×10~(7)X+22321，R=0.9997.(3)Setted the velocity at0.4mL·min-1,in thewavelength of236nm,determinated the active-ingredient geniposide acid in gardenia, inthe range of0.01～0.3mg·mL-1of sample concentration,the peak time is4.758min,had agood linear relationship and the average recovery is102.19%,RSD is0.71%.
For the similitude of the factors for determinations of geniposide,genipin and genipo-side acid by HPLC,such as the wavelength,the chromatographic column and the velocity,established a simple method for determination of geniposide,genipin and geniposide acidsimultaneously by HPLC.This method is repeatable,accurate,rapid and effective for thesimultaneous determination of geniposide,genipin and geniposide acid.
引文
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