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Method for preparing high-purity hesperidin

A high-purity technology for hesperidin, which is applied in the field of preparation of high-purity hesperidin, can solve the problems of low purity of hesperidin, large environmental pollution, and low energy consumption, and achieve good impurity removal effect and low energy consumption , The effect of improving the total yield

Inactive Publication Date: 2014-10-29
四川天予植物药业有限公司
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  • Application Information

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Problems solved by technology

[0006] In order to overcome the technical deficiencies of low purity of hesperidin produced by the existing preparation process and high energy consumption and large environmental pollution during the preparation process, the present invention provides a preparation method of high-purity hesperidin, which includes impurity removal and gradient extraction , crystallization, separation and other steps, the prepared product not only has high purity, but also has low energy consumption and low environmental pollution during the preparation process, which is suitable for popularization and use on an industrial scale

Method used

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Examples

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Embodiment 1

[0019] Example 1 A preparation method of hesperidin

[0020] A preparation method for hesperidin, comprising the steps of:

[0021] 1) Impurity removal: Grind 100g of Citrus aurantium raw material, add 500mL of 40% n-butanol aqueous solution, use dilute hydrochloric acid to adjust the pH of the solution to 3.5 and heat the solution to 50°C, soak for 50 minutes and then filter;

[0022] 2) Gradient extraction: Add 500mL of sodium hydroxide-ethanol-water solution to the filtered filter residue to carry out the first step of extraction, wherein the mass fraction of sodium hydroxide in the sodium hydroxide-ethanol-water solution is 5%, ethanol The volume fraction is 70%, heating and maintaining the extraction temperature at 70°C, extracting and soaking for 3 hours and then filtering to obtain the filtrate; add 300mL of sodium hydroxide-ethanol-water solution to the filtered filter residue for the second step of extraction, in which the hydroxide The mass fraction of sodium hydrox...

Embodiment 2

[0024] Example 2 A preparation method of hesperidin

[0025] A preparation method for hesperidin, comprising the steps of:

[0026] 1) Impurity removal: crush 100g of citrus aurantium raw material, add 500mL of 40% n-butanol aqueous solution, use dilute hydrochloric acid to adjust the pH of the solution to 4 and heat the solution to 40°C, soak for 40 minutes and then filter;

[0027] 2) Gradient extraction: Add 500mL of sodium hydroxide-ethanol-water solution to the filtered filter residue to carry out the first step of extraction, wherein the mass fraction of sodium hydroxide in the sodium hydroxide-ethanol-water solution is 5%, ethanol The volume fraction is 70%, heating and maintaining the extraction temperature at 69°C, extracting and soaking for 2 hours and then filtering to obtain the filtrate; add 300mL of sodium hydroxide-ethanol-water solution to the filtered filter residue for the second step of extraction, in which the The mass fraction of sodium hydroxide in the s...

Embodiment 3

[0029] Example 3 The preparation method of hesperidin of the present invention

[0030] A preparation method for hesperidin, comprising the steps of:

[0031] 1) Impurity removal: crush 100g of citrus aurantium raw material and add 500mL of 40% n-butanol aqueous solution, use dilute hydrochloric acid to adjust the pH of the solution to 3.5 and heat the solution to 45°C, soak for 60 minutes and then filter;

[0032] 2) Gradient extraction: Add 500mL of sodium hydroxide-ethanol-water solution to the filtered filter residue to carry out the first step of extraction, wherein the mass fraction of sodium hydroxide in the sodium hydroxide-ethanol-water solution is 5%, ethanol The volume fraction is 70%, heating and maintaining the extraction temperature at 74°C, extracting and soaking for 2.25 hours and then filtering to obtain the filtrate; add 300mL of sodium hydroxide-ethanol-water solution to the filtered filter residue for the second step of extraction, in which the The mass fr...

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Abstract

The invention relates to a method for preparing high-purity hesperidin, which belongs to the technical field of traditional Chinese medicine extraction and is used overcoming the technical defects that the purity of hesperidin prepared by using a conventional preparation process is relatively low and the energy consumption is large and the environment is severely polluted in the preparation process. The method for preparing high-purity hesperidin comprises the steps of impurity removal, gradient extraction, crystallization separation and the like. Not only is a product prepared by using the method high in purity, but also the energy consumption is low and the environment pollution is low in the preparation process, so that the method is applicable to popularization and application on industrial scale.

Description

technical field [0001] The invention relates to a preparation method of high-purity hesperidin, belonging to the technical field of traditional Chinese medicine extraction. Background technique [0002] Hesperidin has the functions of increasing the resistance of capillaries, maintaining the normal permeability of blood vessels, inhibiting the increase of blood cholesterol and preventing arteriosclerosis. It is widely used as medical drugs, health products and food additives. Diosmin, which is semi-synthesized using hesperidin as a raw material, is commonly used in Europe to treat various symptoms related to venous lymphatic insufficiency and various symptoms related to acute hemorrhoids. Bureau approved for clinical use. [0003] At present, the process for preparing hesperidin on an industrial scale is mainly to crush the citrus aurantium fruit and decoct it for 1 to 2 times to remove water-soluble impurities, then use alkaline solution to leak and extract, and produce cr...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08
Inventor 张雄修李选民李威
Owner 四川天予植物药业有限公司
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