Supercharge Your Innovation With Domain-Expert AI Agents!

15N-proline separating and purifying meethod

A purification method and proline technology, applied in the direction of organic chemistry and the like, can solve the problems of many operation steps, difficult to recycle, low boiling point of diethyl ether, etc., and achieve the effects of simple process, convenient operation and snow-white color.

Inactive Publication Date: 2004-09-15
SHANGHAI RES INST OF CHEM IND
View PDF1 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The nitrosation method has problems such as many operation steps and long pretreatment period; the alumina chromatography method has problems such as time-consuming and unsuitable for expanding the scale; although the pentachlorophenol salt-forming precipitation method has the characteristics of good specificity, the pentachlorophenol severe Toxic, labor protection is a problem; the separation and purification of ethanol-ether method is not thorough, and it is easy to oxidize the proline crystals and turn yellow. In addition, ether has a low boiling point, is flammable and explosive, and is not easy to recycle; while the water and low The mixture purification method of carbon alcohol is to use methanol, ethanol, isopropanol and n-butanol in combination as a purification solvent, but 15 N-L-proline is used as a tracer in medicine, food and other industries. Methanol, isopropanol, and n-butanol should not be used as purification solvents; and in general ion exchange resin methods, flocculants must be added before loading to the column. The fermented liquid is pretreated ["Journal of East China Institute of Chemical Technology", 1989 (4), 456-460], or decolorized with a decolorizing agent ["Acta Microbiology", 1993 (2), 87-90], and before refining eluent for decolorization

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] obtained after fermentation 15 The N-L-proline high-abundance fermentation broth is adjusted to pH=3.2 with oxalic acid, centrifuged with a centrifuge to obtain a supernatant, and 350 mL of the supernatant is taken. The supernatant contains 15 N-L-proline 2.11% (weight), upper gel strong acid styrene resin (Amberjet 1500H strong acid resin) column, empty column flow rate SV=0.2%, clean the resin column to neutrality with distilled water afterwards, then use 0.1M Ammonia desorption adsorbed on the resin column 15 N-L-proline, the desorbed solution was concentrated and dried under vacuum at 50°C to obtain heteroacid-containing 15 N-L-proline crude product 9.24g.

[0021] Add 350mL of distilled water to dissolve 15 N-L-proline crude product, adjust its pH=9.9 with ammonia water, go up styrene series anion exchange resin (201 * 4OH type strong basic resin) column, empty column flow rate SV=0.15%, clean the resin column to medium with distilled water afterwards propertie...

Embodiment 2

[0024] obtained after fermentation 15 N-L-proline low-abundance fermented liquid is adjusted pH=5.0 with oxalic acid, centrifuges with centrifuge to obtain supernatant, gets supernatant 150mL, and this supernatant contains 15 N-L-proline 2.50% (weight), upper gel strong acid styrene resin (001 * 7H type strong acid resin) post, empty column flow velocity SV=1.0%, clean the resin post to neutrality with distilled water afterwards, then use 0.1M ammonia water was desorbed to obtain 15 The desorption solution of N-L-proline, the desorption solution was concentrated and dried under vacuum at 55°C to obtain the heteroacid-containing 15 N-L-proline crude product 4.65g.

[0025] Add 150mL of distilled water to dissolve 15 N-L-proline crude product, adjust its pH=10.2 with ammoniacal liquor, go up styrene series anion exchange resin (201 * 7OH type strong basic resin) column, empty column flow rate SV=1.0%, clean the resin column with distilled water afterwards to medium propertie...

Embodiment 3

[0028] obtained after fermentation 15 The N-L-proline high-abundance fermentation broth is adjusted to pH=4.1 with oxalic acid, and the supernatant is obtained by centrifuging with a centrifuge, and 400 mL of the supernatant is taken. The supernatant contains 15 N-L-proline 2.11% (weight), upper gel strong acid styrene resin (Amberjet 1500H strong acid resin) column, empty column flow rate SV=0.6%, clean the resin column to neutrality with distilled water afterwards, then use 0.2M Ammonia desorption, obtained containing 15 The N-L-proline stripping liquid was concentrated and dried under vacuum at 60°C to obtain the heteroacid-containing 15 N-L-proline crude product 10.59g.

[0029] Add 400mL of distilled water to dissolve 15 N-L-proline crude product, adjust its pH=10.8 with ammoniacal liquor, go up styrene series anion exchange resin (201 * 4OH type strong basic resin) column, empty column flow rate SV=0.6%, clean the resin column to medium with distilled water afterwards ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a separation and purification method of 15N-L-proline, which is characterized by that it adopts strong acid resin to remove colouring matter and impurity from fermenting liquor, and adopts strong base resin to separate proline from other amino acid heteroacid, then uses anhydrous alcohol to make refining to obtain the invented 15N-L-proline product which is high in purity, white in colour and does not yellow for long-time storage. Its total extracted yield rate is up to above 80%.

Description

technical field [0001] The present invention relates to a method for separation and purification of amino acids, more precisely to a 15 The separation and purification method of N-L-proline. Background technique [0002] L-proline is one of the important components of human protein. It is a heterocyclic amino acid and has important uses in medicine, agriculture, chemical and food industries. 15 Due to its special structure, N-L-proline is widely used as a tracer in medicine, pharmacy, agricultural science, life science and other research fields. 15 The preparation of N-L-proline generally adopts organic synthesis method and microbial fermentation method, but no matter which method is adopted, the problem of separation and purification of the product will be encountered. Since proline is the only amino acid soluble in alcohol, and its solubility in water is extremely high, which is 162.30g / 100mL water (25°C), therefore, the purification is more difficult. [0003] Existing...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07D207/16
Inventor 侯静华孙建春杜晓宁李良君宋明鸣
Owner SHANGHAI RES INST OF CHEM IND
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com