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Separation method of D-glucuronic acid gamma-lactone

A glucuronic acid and separation method technology, applied in the field of separation of D-glucuronic acid γ-lactone, can solve the problems of difficult separation of crystals, easy decomposition of D-glucuronic acid, high cost, etc., to overcome the difficulty of crystal separation, The effect of reducing production cost and simplifying production process

Inactive Publication Date: 2012-10-10
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • 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

[0015] 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, after the reaction was completed, the temperature was raised to boiling to obtain the oxidized starch liquid; the purpose was to allow 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%;

[0016] 2) Cool and adjust the pH value of the oxidized starch solution to 6.2, add an α-amylase with an activity of 20000 μ / g at a ratio of 120 μ α-amylase / g starch, hydrolyze at 90° C. for 0.5 h, heat to boiling and Hold for 10 minutes to kill α-amylase to obtain liquefaction solution;

[0017] 3) Cool the liquefied liquid to 62°C and adjust its pH value to 4.5, add glucoamylase with...

Embodiment 2

[0021] 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 , reacted at 45°C for 4h, after the reaction was completed, the temperature was raised to boiling to obtain the oxidized starch liquid; the purpose was to allow 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%;

[0022] 2) Cool and adjust the pH value of the oxidized starch solution to 6.5, add an α-amylase with an activity of 20000 μ / g at a ratio of 140 μ α-amylase / g starch, hydrolyze at 86° C. for 1.5 h, heat to boiling and Hold for 10 minutes to kill α-amylase to obtain liquefaction solution;

[0023] 3) Cool the liquefied liquid to 65°C and adjust its pH value to 4.2, add glucoamylase w...

Embodiment 3

[0027] 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 , reacted at 45°C for 4h, heated to boiling after the reaction to obtain oxidized starch liquid; 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%;

[0028] 2) Cool and adjust the pH of the oxidized starch solution to 6.0, add α-amylase with an activity of 20000μ / g at the ratio of 100μα-amylase / g starch, hydrolyze at 88°C for 1 hour, heat to boiling and keep 10min, kill α-amylase to obtain liquefaction solution;

[0029] 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 of ...

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Abstract

The invention relates to a separation method of D-glucuronic acid gamma-lactone, which carries out alcoholic fermentation on glucose and other fermentable saccharides in a zymolysis product by adopting an alcoholic fermentation process according to the property differences of oxidized starch and the zymolysis product to seperate the glucuronic acid of the zymolysis product from the glucose and other fermentable saccharides. The invention reduces the dosage of alcohol, thereby lowering the production cost of glucuronic acid lactone. Each index of the glucuronic acid obtained by the separation method meets the standard of the national formulary, and the invention simplifies the production process and lowers the 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 method for separating 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. The production cost has been reduced to a certain extent, but problems such as product separation have not been well studied, and it st...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C12P19/00C12P19/14C07H13/02C07H1/06C12R1/865
Inventor 李祥马建中王勇赵倩张青郭凌华
Owner SHAANXI UNIV OF SCI & TECH
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