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Membrane filtration, separation and purification method of levodopa conversion solution

A technology of membrane filtration separation and levodopa, which is applied in the direction of organic chemical methods, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of long reaction time, high residual concentration of substrate, low crystallinity, etc., and achieve improvement The effect of moisture uniformity, shortening the production cycle, and reducing production costs

Active Publication Date: 2016-11-16
CHANGXING PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on the industrialization of levodopa prepared by biological methods
The existing biological method for preparing levodopa has a series of problems such as long reaction time, many by-products, low conversion rate, high residual substrate concentration, poor color of the finished product, low crystallinity, and high impurity content.

Method used

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  • Membrane filtration, separation and purification method of levodopa conversion solution
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  • Membrane filtration, separation and purification method of levodopa conversion solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1 Tyrosine phenol lyase biocatalytic process

[0031]Put initial pyruvate into the water, control the pH at 7.0-9.0 with concentrated ammonia water; then add antioxidants, chelating agents, ammonium salts, pyridoxal 5-phosphate in sequence, and control the pH at 7.0-9.0 with concentrated ammonia water again, add The enzyme solution of recombinant tyrosine phenol lyase with a concentration of 80-200g / L is passed through nitrogen, the temperature is adjusted to the reaction temperature, the pH is adjusted to 7.0-9.0 with ammonia water, and catechol is added to start the reaction; the initial basic substrate o The molar ratio of hydroquinone to pyruvic acid and its sodium salt is 1:1-1.5. Afterwards, add the substrates catechol and pyruvate (or ammonium pyruvate, only pyruvate unless otherwise specified) at 2 g / L every 10 minutes, and the final concentration of catechol is 50-70 g / L (calculated based on the initial volume), the final concentration of pyruvic a...

Embodiment 2

[0036] Example 2 2500L transformation system

[0037] Take 2500 L of the levodopa conversion solution obtained in Example 1, with a concentration of 110 g / L, add concentrated hydrochloric acid to adjust the pH to 0.96, and the consumption of concentrated hydrochloric acid is 190 kg. The temperature of the feed liquid rises to 30-40°C, and the ceramic membrane system is turned on for filtration. The ceramic membrane system of Jiangsu Jiuwu High-tech Co., Ltd. is selected. The ceramic membrane element has a pore size of 50nm and is made of zirconium dioxide. A single membrane has 19 channels, and the total membrane area is 21.2 square meters.

[0038] Use the ceramic membrane to collect the supernatant, and when the minimum circulation volume is reached, about 500L system, start to add purified water. Detect the content of levodopa in the retentate, when down to 5g / L, stop filtering, the total volume of retentate is 530L. The collected supernatant has a volume of 3000 L, and t...

Embodiment 3

[0046] Example 3 5000L transformation system

[0047] Take 5000L of the levodopa conversion liquid obtained in Example 1, the concentration is 115g / L, add concentrated nitric acid to adjust the pH to 1.04, the amount of concentrated nitric acid is 325kg, the temperature of the feed liquid is raised to between 30-40°C, and the ceramic membrane system is started for filtration. The ceramic membrane system of Jiangsu Jiuwu High-tech Co., Ltd. is selected. The ceramic membrane element has a pore size of 50nm and is made of zirconium dioxide. A single membrane has 19 channels, and the total membrane area is 21.2 square meters.

[0048] Use the ceramic membrane to collect the supernatant, and when the minimum circulation volume is reached, about 700L system, start to add drinking water. Detect the content of levodopa in the retentate, when down to 8g / L, stop filtering, the total volume of retentate is 830L. The volume of the collected supernatant is 6200L, and the content of levodo...

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Abstract

The invention discloses a membrane filtration, separation and purification method of a levodopa conversion solution. The conversion solution containing levodopa is obtained through tyrosine phenol-lyase biological conversion, the pH of the conversion solution is adjusted to be strongly acidic by means of acid fluid, clear liquid is collected through a ceramic membrane filtration system after proper temperature increasing, and after activated carbon is added into the collected ceramic membrane filtration clear liquid, stirring, temperature increasing and decoloring are conducted; after clear liquid is filtered, alkali adjustment and crystallization are conducted, then filtering is conducted to obtain crystal, the crystal is dried, and levodopa anhydrous crystal powder is obtained. The method effectively removes residual substrates, protein and pigment in the conversion process on the basis of industrial production, the anhydrous crystal powder obtained during production is high in quality and high in light transmittance, total impurities are not larger than 0.1% by HPLC peak area percentage, and the crystallization degree of the crystal powder is 90% or above.

Description

technical field [0001] The invention relates to the field of biochemical industry and separation and purification, in particular to a membrane filtration separation and purification method of levodopa conversion liquid. Background technique [0002] Levodopa (3,4-dihydroxylphenylalanine, Levodopa), also known as L-dopa, chemical name is 3,4-dihydroxyphenylalanine, CAS: 59-92-7; white crystalline powder, odorless Odorless; it is an important biologically active substance in organisms and an important intermediate product in the biochemical metabolic pathway from L-tyrosine to catechol or melanin. Its structural formula is as follows: [0003] [0004] Levodopa and compound levodopa (such as Madopar) have been used in the treatment of Parkinson's disease, a common senile disease, for more than 40 years. They are still the most effective drugs for Parkinson's disease, and they are well tolerated. Slowing of movement, relief of major symptoms, and prolongation of life in pa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C227/40C07C229/36C07C227/34C07C227/42C12P13/22
CPCC07B2200/07C07C227/34C07C227/40C07C227/42C12P13/225C07C229/36
Inventor 杨卫华肖延铭陈明亮龚彬成钱敏帆谈聪
Owner CHANGXING PHARMA
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