Method for analyzing ferulaic acid butyric glyceride by high performance liquid chromatography
A technology of glyceryl butyrate and high-performance liquid chromatography, which is applied in the field of chromatographic separation, can solve the problems of researchers, difficulties in controlling the reaction process, isomers, etc., reduce the number of experiments, and the method is simple, fast and simplified Effect of separation and purification steps
Inactive Publication Date: 2010-11-17
DONGHUA UNIV
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Problems solved by technology
However, due to the difficulty in controlling the reaction process and the similar polarity of the generated mixture, even the phenomenon of isomers, it is difficult to find suitable separation conditions in the process of analysis and separation, which has brought great troubles to researchers. and impedes research on the properties of these compounds
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Embodiment 1
[0028] Esters, 120mg Novozym435 lipase, 5mL tert-butanol, shake in an air bath at 50°C at 150r / min for 120h, and remove the enzyme by filtration.
[0029] 2. Pretreatment for the analysis of ferulic acid butyrin by high performance liquid chromatography
[0030] The reaction medium isobutanol was removed by rotary evaporation of the above reaction mixture, and unreacted tributyrin was extracted with anhydrous ether / n-hexane (80 / 20, V / V). Finally, the residual organic medium in the reaction system was removed by nitrogen purging. Dissolve 1 mg of the mixed product in 1 mL of methanol, filter through a microporous membrane with a pore size of 0.45 μm, and set aside.
[0031] 3. Separation and analysis of ferulic acid butyric acid mixture by high performance liquid chromatography
[0032] (1) Take 10 μL of the reaction sample, dilute it to 1 mL with HPLC grade methanol, and then take 5 μL of the sample through a microsampler and add it to the injection valve.
[0033] (2) Mobi...
Embodiment 2
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Abstract
The invention relates to a method for compartment analysis of ferulic acid glycerol monobutyralte through the high performance liquid chromatography, comprising the following: firstly, a step of pretreatment, during which, ferulic acids and absolute ethyl alcohols generate reflux heating reaction under the catalysis of thionyl chlorides and are dissolved in aether and then ferulic acid methyl ethyl oxalate is obtained after extraction through sodium bicarbonate; under the temperature of between 30 and 50 DEG C, tertiary butyl alcohol is used as reaction medium and the ferulic acid glycerol monobutyralte is obtained through oscillating reaction of the ferulic acid methyl ethyl oxalate, glycerol monobutyralte and Novozym435 lipase in an air bath; the ferulic acid glycerol monobutyralte is dissolved in methanol, filtered and then diluted by HPLC-level methanol; secondly, a step of compartment analysis, which is to adopt a chromatographic column (Ph-3 column Inertsil, IDx250mm) with a column temperature of ambient temperature. A solid phase adopts silica gel filler and the ultraviolet detection wavelength is between 280 and 325 nanometers; a moving phase is gradient mixing of methanoland water; the sample feeding quantity is 5 mu L and the flow speed is 1mL / min. The method selects filler of the chromatographic column and the special ultraviolet scanning wavelength according to the characteristics of materials to be comparted, is quick, high-efficient and accurate and is convenient for industrial analysis and application.
Description
technical field [0001] The invention belongs to the field of chromatographic separation, in particular to a method for separating and analyzing ferulic acid butyrin by high performance liquid chromatography (HPLC). Background technique [0002] Ferulic acid butyrin is a derivative of natural phenolic acid ferulic acid (Ferulic acid). Glyceryl monobutyrate, glyceryl ferulic acid dibutyrate and a mixture of glyceryl ferulic acid, they all have many physiological activities of ferulic acid and butyric acid, and at the same time overcome the inability to be used in oils due to their short alkane chains Due to the disadvantages of industrial application, it can be widely used in food, pharmaceutical and cosmetic industries. Synthesizing tributyrin with strong fat solubility and ethyl ferulic acid with strong water solubility can not only achieve mutual protection, reduce the level of oxidative denaturation, and improve their chemical stability, but also The dual purpose of mutu...
Claims
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IPC IPC(8): C12P7/62C07C59/68G01N30/50G01N30/06G01N30/74A23L3/3517
Inventor 朱利民郑妍权静蒋波
Owner DONGHUA UNIV
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