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New crystalline technology of fructose-1, 6-trisodium diphosphate

A trisodium diphosphate salt and a new process technology, which is applied in the direction of sugar derivatives, sugar derivatives, esterified saccharides, etc., can solve the problems of uneven product particle size and poor stability, and achieve easy control operation and improved Good uniformity and repeatability

Inactive Publication Date: 2005-08-10
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because this method is prone to primary heterogeneous nucleation when producing FDP crystals, resulting in uneven product particle size and poor stability

Method used

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  • New crystalline technology of fructose-1, 6-trisodium diphosphate
  • New crystalline technology of fructose-1, 6-trisodium diphosphate
  • New crystalline technology of fructose-1, 6-trisodium diphosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Dissolve 100g of anhydrous FDP trisodium salt in 300mL of water, adjust the pH to 4.8 with acetic acid, add 10g of sodium acetate, add 450ml of ethanol while stirring, and keep stirring at 25°C until crystallization is complete. The suspension was suction-filtered, the resulting white solid was washed with 85% ethanol, and vacuum-dried to obtain 128 g of the product with a crystallization yield of 95%.

[0027] Product analysis result C 6 h 11 o 12 P 2 Na 3 ·8H 2 O (molecular weight 550.18)

[0028] Element Measured value (%) Theoretical value (%)

[0029] C 13.6 13.10

[0030] H 5.02 4.96

[0031] O 58.28 58.16

[0032] P 11.23 11.26

[0033] Na 12.31 12.53

Embodiment 2

[0035] In the 30% FDP solution, adjust the pH values ​​to 4.5, 4.8, 5.0, and 5.2 respectively, add 8% sodium acetate, add 1.6 times the volume of ethanol of the FDP solution while stirring, and keep stirring at 30°C until crystallization is complete. Suction filtration, washing with ethanol, and vacuum drying. Table 1.1 gives the product particle size distribution.

[0036] It can be concluded that pH has a great influence on the distribution of crystal particles. The pH of the solution increased from 4.5 to 5.2 with a difference of 0.7, but the average particle size difference of the crystals was 84 μm. Therefore, the purpose of controlling the particle size of the crystals can be achieved by controlling the pH value of the solution.

[0037] pH

Embodiment 3

[0039] Add 8% sodium acetate to the 30% FDP solution at pH 4.5, add 1.6 times the volume of ethanol of the FDP solution while stirring, and keep stirring at 20°C, 25°C, and 30°C until crystallization is complete. Suction filtration, washing with ethanol, and vacuum drying. Table 1.2 gives the product particle size distribution.

[0040] temperature

[0041] Temperature has a great influence on FDP crystallization, especially on the size of FDP crystal grains. The crystallization temperature increases from 20°C to 30°C, while the crystal particles increase from 92μm to 241μm. Therefore, crystals of different particle sizes can be produced by adjusting the crystallization temperature.

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PUM

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Abstract

A process for crystallizing pectose-1,6-trisodium biphosphate includes such steps as slowly and proportionally adding sodium acetate and alcohol to FDP solution, stirring at 20-40 deg.C while crystallizing, filtering, washing with alcohol and vacuum drying.

Description

Technical field: [0001] The present invention relates to the production of crystalline form fructose-1,6-diphosphate trisodium salt (FDPNa) by utilizing fructose-1,6-diphosphate aqueous solution 3 H·8H 2 O) the new method and use this method to prepare fructose-1,6-diphosphate trisodium salt injection, application clinically obviously reduces the stimulation of medicine to muscles and blood vessels. technical background: [0002] Fructose 1,6-diphosphate (FDP) is also called Harden Young's ester (esterof Harden Young). It is an important intracellular metabolite and an intermediate product in the glycolytic metabolic pathway in humans. It can directly regulate many metabolic pathways and can be regarded as a metabolic regulator, especially playing an important role in energy metabolism and regulating certain enzyme activities. Clinically, it can regulate the activity of several enzymes in glucose metabolism, restore and improve cell metabolism at the molecular level, act ...

Claims

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Application Information

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IPC IPC(8): C07H11/04
Inventor 应汉杰欧阳平凯吕浩赵谷林史隽
Owner NANJING UNIV OF TECH
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