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A method for preparing high-purity cyclic peptide monomers by generating cyclic peptide crystals

A high-purity, cyclic peptide technology, applied in the preparation method of peptides, chemical instruments and methods, peptides, etc., can solve the problems of high operating costs, production costs, and high equipment requirements, and achieve low cost, simple preparation process, and production conditions. easily controlled effects

Active Publication Date: 2021-09-28
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods require high instrumentation, high operating and production costs

Method used

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  • A method for preparing high-purity cyclic peptide monomers by generating cyclic peptide crystals
  • A method for preparing high-purity cyclic peptide monomers by generating cyclic peptide crystals
  • A method for preparing high-purity cyclic peptide monomers by generating cyclic peptide crystals

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Effect test

Embodiment 1

[0033] A method for preparing high-purity cyclic peptide monomers by generating cyclic peptide crystals comprises the following steps.

[0034] (1) Dissolve the crude cyclic peptide solid powder in pure methanol according to the mass volume ratio of the crude cyclic peptide solid powder to pure methanol: 1g:16ml, centrifuge at 4500 r / min for 7 min, and collect the supernatant liquid.

[0035] (2) Rotate the supernatant to dryness at a temperature of 50° C. to obtain a preliminarily purified solid product.

[0036] (3) Add pure methanol dropwise to the obtained preliminary purified solid product according to the ratio of the mass volume ratio of the preliminary purified solid product to the final added pure methanol: 1g:4.2ml, and add methanol at a water bath temperature of 50°C dissolved until a saturated solution was obtained.

[0037] (4) Keep the temperature of the 50°C water bath in step (3) constant, and add distilled water dropwise to the saturated solution obtained in...

Embodiment 2

[0040] A method for preparing high-purity cyclic peptide monomers by generating cyclic peptide crystals comprises the following steps.

[0041] (1) Dissolve the crude cyclic peptide solid powder in pure methanol according to the mass volume ratio of the crude cyclic peptide solid powder to pure methanol: 1g:12.5ml, centrifuge at 3000 r / min for 10min, and collect the supernatant liquid.

[0042] (2) The supernatant was rotatably concentrated to dryness at a temperature of 40° C. to obtain a preliminarily purified solid product.

[0043] (3) Add pure methanol dropwise to the obtained preliminary purified solid product according to the ratio of the mass volume ratio of the preliminary purified solid product to the final added pure methanol: 1g:3.5ml, and add methanol at a water bath temperature of 60°C dissolved until a saturated solution was obtained.

[0044] (4) Keep the temperature of the water bath in step (3) constant, add distilled water drop by drop to the saturated sol...

Embodiment 3

[0047] A method for preparing high-purity cyclic peptide monomers by generating cyclic peptide crystals comprises the following steps.

[0048] (1) Dissolve the crude cyclic peptide solid powder in pure methanol according to the mass volume ratio of the crude cyclic peptide solid powder to pure methanol: 1g:20ml, centrifuge at 4000 r / min for 15min, and collect the supernatant .

[0049] (2) The supernatant was rotatably concentrated to dryness at a temperature of 45° C. to obtain a preliminarily purified solid product.

[0050] (3) Add pure methanol dropwise to the obtained preliminary purified solid product according to the ratio of the mass volume ratio of the preliminary purified solid product to the final added pure methanol: 1g:5ml, and add methanol while adding methanol at a water bath temperature of 45°C. Dissolve until a saturated solution is obtained.

[0051] (4) Keep the temperature of the water bath in step (3) constant, add distilled water drop by drop to the sa...

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Abstract

A method for preparing high-purity cyclic peptide monomers by generating cyclic peptide crystals, comprising: (1) dissolving crude cyclic peptide solid powder in pure methanol, centrifuging for 5-20 min, and collecting the supernatant; (2) dissolving The supernatant was spun and concentrated to dryness to obtain a preliminary purified solid product; (3) Add pure methanol drop by drop, and dissolve it while adding in a water bath temperature of 40~65°C until a saturated solution is obtained; (4) Keep the temperature of the water bath at Change, add distilled water drop by drop to the saturated solution until a supersaturated white emulsion is obtained; (5) naturally cool and stand for 1 to 3 days until the cyclopeptide crystals are obtained. In the present invention, crude cyclic peptides with low purity are used as raw materials, pure methanol with a specific mass-volume ratio is used as a solvent, and then pure methanol with a specific mass-volume ratio is used as a solvent in combination with water bath heating to form a saturated solution, distilled water is added and cooled naturally. The cyclic peptide crystals with a purity of ≥96% were obtained without any organic solvent residue.

Description

technical field [0001] The invention relates to the field of purification of cyclic peptides, in particular to a method for preparing high-purity cyclic peptide monomers by generating cyclic peptide crystals and the cyclic peptide crystals obtained therefrom. Background technique [0002] Cyclic peptides are formed by the cyclization of linear precursor peptides. Flaxseed cyclic peptides are a group of hydrophobic homologous cyclic plant peptides synthesized by ribosomes and naturally occurring in flaxseeds and rhizomes (the N-terminal and C-terminal of the polypeptide chain are ringed by amide bonds, and there is no ring cystine joint ), consisting of 8-9 amino acids with a molecular weight of approximately 1kDa. Studies have shown that flaxseed cyclic peptide has immunomodulatory, anti-malarial, anti-fungal, anti-inflammatory, anti-cancer and other activities. [0003] At present, the purification methods for cyclic peptides at home and abroad mainly include salting out ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/64C07K1/14
CPCC07K7/64
Inventor 李红艳邓泽元邹仙果
Owner NANCHANG UNIV
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