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A method for purifying nonapeptide-1

A surface activation and modification technology, applied in the field of peptide purification, can solve the problems of low purity of nonapeptide-1, reduced production cost, only 79%, etc., to reduce the steric hindrance effect, prolong the service life, and not destroy the activity Effect

Active Publication Date: 2022-03-29
浙江湃肽生物股份有限公司深圳分公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method of purifying nonapeptide-1 has high cost and low purification efficiency, and the purity of nonapeptide-1 obtained is low
In order to improve the purity of nonapeptide-1, increase purification efficiency, and reduce costs, numerous researchers have carried out improved research on the purification of nonapeptide-1. For example, patent CN106749526A discloses a low-cost method for purifying nonapeptide-1. It adopts high-performance liquid chromatography, and firstly uses a reversed-phase polymer column to purify a large amount of nonapeptide-1 crude product to remove impurities in the nonapeptide-1 crude product, and then uses a weak anion exchange column to convert trifluoroacetic acid type nonapeptide-1 1 is converted into acetic acid type nonapeptide-1, the purity of gained nonapeptide-1 is greater than 99%, and production cost has been reduced, but its yield is only 79%, therefore, it is still necessary to provide a kind of high yield, high purity Method for Purifying Nonapeptide-1

Method used

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Examples

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Embodiment 1

[0057] The present embodiment provides a modified silica gel chromatography filler, which is prepared by the following method:

[0058] 1) 1 g of silica gel microspheres was added to 20 mL of a mixed solution containing 8 wt% hydrochloric acid and 0.6 wt% methanesulfonic acid, stirred at 40 °C for 2 h, filtered with suction, washed with water until neutral, and dried under vacuum at 90 °C. to obtain surface-activated silica microspheres;

[0059] 2) 2 g vinyltriethoxysilane was mixed with 4.5 g 2-aminophenol-4-sulfonanilide, and the reaction was stirred at 30 °C for 2 h, and distilled under reduced pressure to obtain 2-aminophenol-4-sulfonanilide Modified silane coupling agent; under nitrogen protection, 1 g of surface-activated silica gel microspheres and 2.6 g of 2-aminophenol-4-sulfonanilide modified silane coupling agent were added to 30 g of toluene, and the reaction was stirred at 80 °C 4 h, filter after the reaction, the filter residue is washed with toluene, acetone, ...

Embodiment 2

[0063] This example provides another modified silica gel chromatography filler, the preparation method of which is basically the same as that in Example 1, the difference is that in step 1), vinyltriethoxysilane, 2-aminophenol-4-sulfonic acid The amount of anilide added was 2 g and 1 g, respectively.

Embodiment 3

[0065] This example provides another modified silica gel chromatography filler, the preparation method of which is basically the same as that in Example 1, the difference is that in step 1), vinyltriethoxysilane, 2-aminophenol-4-sulfonic acid The addition amount of the anilide was 2 g and 2 g, respectively.

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Abstract

The invention provides a method for purifying nonapeptide-1, which belongs to the technical field of polypeptide purification, and specifically adopts a combination method of gel chromatographic column chromatography, reversed-phase high-performance liquid chromatography, and anion-exchange chromatography to treat crude nonapeptide-1 For purification, the filler for reversed-phase high-performance liquid chromatography is a modified silica gel chromatography filler, which not only has good acid and alkali resistance stability, but also does not collapse during the separation process, prolonging the service life. Using the modified silica gel filler to separate Purification of nonapeptide-1 can improve peak shape, overcome peak broadening and tailing problems, and quickly and efficiently separate nonapeptide-1 with a faster peak time, achieving the purpose of improving the yield and purity of nonapeptide-1.

Description

technical field [0001] The invention belongs to the technical field of polypeptide purification, in particular to a method for purifying nonapeptide-1. Background technique [0002] Nonapeptide-1 is a small molecule skin-lightening active peptide containing nine amino acids. It is a biomimetic peptide of natural α-MSH, which can competitively inhibit the binding of a-MSH to the receptor MCI-R and prevent tyrosine Further activation of the enzyme blocks the production of melanin, reducing skin darkening and preventing brown spots. Nonapeptide-1 has become an extremely popular cosmetic raw material in recent years, often added to skin lightening creams, skin lightening foundations, powders and freckle creams. [0003] When nonapeptide-1 is used as a cosmetic raw material, the chromatographic purity must be ≥99%. However, due to various side reactions and incomplete removal of protective agents during the synthesis of nonapeptide-1, these factors cause the crude product of non...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/281B01J20/287B01J20/28B01J20/30C07K7/06C07K1/20C07K1/18C07K1/16
CPCB01J20/281B01J20/287B01J20/28019B01J20/28083B01J20/28061C07K7/06
Inventor 刘慧敏陈超虞慧飞傅小明
Owner 浙江湃肽生物股份有限公司深圳分公司
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