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Method for crystallizing D-glucuronic acid gamma-lactone

A technology of glucuronic acid and lactone, which is applied in the field of D-glucuronic acid γ-lactone crystallization, can solve the problems of easy decomposition of D-glucuronic acid, difficult separation of crystals, and high cost, so as to reduce production costs and overcome crystallization. The effect of difficult separation and simplified production process

Inactive Publication Date: 2009-11-11
SHAANXI UNIV OF SCI & TECH
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0002] D-glucuronic acid γ-lactone has wide application prospects in the medicine, food, and health care products industries. At present, the nitric acid oxidation process is mainly used in the industry. The biggest disadvantage of this process is: serious pollution, and the product needs to be separated by low temperature freezing. High energy consumption, not in line with national industrial policies
However, this method uses butyl acetate as the secondary water-carrying agent, which has high cost, and due to the high boiling point of butyl acetate, D-glucuronic acid is easy to decompose, the liquid is viscous, and the problems of crystals being difficult to separate are still not well resolved. solve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Embodiment 1: 1) first with 100g cornstarch, the water of 150mL and the FeSO of 0.1g 4 Add it into a three-neck flask with stirring, adjust the pH value to 10 with 0.1mol / L NaOH, and slowly add 6g of H 2 o 2 , reacted at 45°C for 4h, heated to boiling after the reaction to obtain oxidized starch; the purpose is to let the excess H 2 o 2 Heating and decomposing to avoid further oxidation of aldehyde groups (glucuronic acid, glucose) in the enzymolysis solution to obtain oxidized starch with carboxyl content ≥ 8% and carbonyl content ≤ 0.2%;

[0013] 2) Adjust the pH of the oxidized starch solution to 6.2, add α-amylase with an activity of 20,000 μ / g at a ratio of 120 μ α-amylase / g starch, hydrolyze at 90 ° C for 0.5 h, heat to boiling and keep for 10 min , killing α-amylase to obtain liquefaction solution;

[0014] 3) Cool the liquefied liquid to 62°C and adjust its pH value to 4.5, add glucoamylase with an activity of 10000μ / g according to the ratio of 120μ glucoamy...

Embodiment 2

[0017] Embodiment 2: 1) at first with 100g cornstarch, the water of 180mL and the FeSO of 0.08g 4 Add it into a three-neck flask with stirring, adjust the pH value to 9 with 0.1mol / L NaOH, and slowly add 8g of H 2 o 2 , react at 45°C for 4 hours, and after the reaction is completed, heat up to boiling to obtain oxidized starch;

[0018] 2) Adjust the pH value of the oxidized starch solution to 6.5, add α-amylase with an activity of 20000 μ / g at the ratio of 140 μ α-amylase / g starch, hydrolyze at 86 ° C for 1.5 h, heat to boiling and keep for 10 min , killing α-amylase to obtain liquefaction solution;

[0019] 3) Cool the liquefied liquid to 65°C and adjust its pH value to 4.2, add a glucoamylase with an activity of 10,000 μ / g at a ratio of 140 μ glucoamylase / g starch, incubate at 60°C for 16 hours, heat to inactivate the enzyme and keep it hot filter;

[0020] 4) Concentrate the filtrate, add ethanol to the filtrate and stir until the filtrate is cloudy, let stand, collect...

Embodiment 3

[0022] Embodiment 3: 1) first with 100g cornstarch, the water of 160mL and the FeSO of 0.05g 4 Add it into a three-neck flask with stirring, adjust the pH value to 11 with 0.1mol / L NaOH, and slowly add 5g of H 2 o 2 , react at 45°C for 4 hours, and after the reaction is completed, heat up to boiling to obtain oxidized starch;

[0023] 2) Adjust the pH value of the oxidized starch solution to 6.0, add α-amylase with an activity of 20000 μ / g at a ratio of 100 μ α-amylase / g starch, hydrolyze at 88°C for 1 hour, heat to boiling and keep for 10 minutes, Kill α-amylase to obtain liquefaction solution;

[0024] 3) Cool the liquefied liquid to 61°C and adjust its pH value to 4.0, add glucoamylase with an activity of 10000μ / g according to the ratio of 100μ glucoamylase / g starch, keep it warm at 64°C for 13 hours, heat to inactivate the enzyme and keep it hot filter;

[0025] 4) Concentrate the filtrate and add ethanol to the filtrate to fully stir until the filtrate is turbid, let ...

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Abstract

The invention provides a method for crystallizing D-glucuronic acid gamma-lactone. According to characteristic difference of products of enzymatic hydrolysis of oxidized starch, ethanol is used for separating purification, so that the normal-temperature crystallization of the D-glucuronic acid gamma-lactone is realized, the mother solution is recycled, the yield of the D-glucuronic acid gamma-lactone is improved, and the clean production of the D-glucuronic acid gamma-lactone is realized. The method comprises the following steps: mixing corn starch, water and FeSO4, and adjusting the pH value to between 9 and 11 by NaOH; adding H2O2 for reaction; after reaction, heating up until boiling, and adjusting the pH value to between 6.0 and 6.5; adding alpha-starch for enzymatic hydrolysis, and then heating to kill the alpha-amylase; adjusting the pH value to between 4.0 and 4.5; adding maltogenic amylase and filtering; adding ethanol into the filtrate; collecting the supernatant and condensing, adding acetic acid and acetic anhydride to obtain a micro seed crystal; and separating the micro seed crystal and recrystallizing with the ethanol to obtain a product of which all indexes meet the standards of the national pharmacopoeia. The method simplifies market process and reduces production cost.

Description

technical field [0001] The invention belongs to the field of production of pharmaceutical raw materials or health care products, and in particular relates to a crystallization method of D-glucuronic acid γ-lactone. Background technique [0002] D-glucuronic acid γ-lactone has wide application prospects in the medicine, food, and health care products industries. At present, the nitric acid oxidation process is mainly used in the industry. The biggest disadvantage of this process is: serious pollution, and the product needs to be separated by low temperature freezing. The energy consumption is large, which is not in line with the national industrial policy. In foreign countries, glucuronolactone is produced by glucuronide oxidation. The oxidation reaction requires Pt / C as a catalyst, which is very expensive and the catalyst is not easy to obtain. To a certain extent, the production cost has been reduced, but the problems such as difficult product separation have not been well...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P19/00C12P17/18C07H7/033C07D493/04C07H1/06
Inventor 李祥马建中杨明伟于巧真郭凌华王勇
Owner SHAANXI UNIV OF SCI & TECH
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