A kind of refining method of vasopressin [5-asp] impurity

A purification method, 5-asp technology, applied in the preparation method of peptide, oxytocin/vasopressin, chemical instruments and methods, etc., can solve the problem of uneconomical, large amount of hazardous waste liquid, and high waste liquid treatment cost problems, to achieve the effect of optimizing the production process and reducing the generation of hazardous waste

Active Publication Date: 2021-04-06
SPH NO 1 BIOCHEM & PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to overcome the large amount of organic waste liquid produced in the refining process of vasopressin [5-Asp] impurities in the prior art, and the amount of hazardous waste liquid is large, resulting in high cost of waste liquid treatment and uneconomical However, a method for refining the impurities of vasopressin [5-Asp] is provided

Method used

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  • A kind of refining method of vasopressin [5-asp] impurity
  • A kind of refining method of vasopressin [5-asp] impurity
  • A kind of refining method of vasopressin [5-asp] impurity

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preparation example Construction

[0055] In the following examples, the preparation method of the crude vasopressin [5-Asp] impurity solution includes: (1) adopting the solid phase synthesis method to obtain the crude vasopressin [5-Asp] impurity; The prototype vasopressin [5-Asp] impurity crude product is dissolved and diluted to obtain a reduced vasopressin [5-Asp] impurity crude product solution; (3) the reduced vasopressin [5-Asp] impurity crude product solution is oxidized Process to obtain the crude product solution of the vasopressin [5-Asp] impurity.

[0056] The solid-phase synthesis method includes the following steps: using Rink Amide MBHA resin as a starting material, using Fmoc-protected amino acids as monomers, using HOBt / DIC as a condensation agent, and sequentially connecting amino acids one by one; adding peptide cutting reagents to carry out Cut the peptide, add methyl tert-butyl ether for precipitation, and obtain the crude impurity product of reduced vasopressin [5-Asp]. The peptide cuttin...

Embodiment 1

[0057] Example 1 Load&Lock4002 preparative column with inner diameter of 50mm

[0058] Using Load&Lock dynamic axial compression and static locking technology, the packing is as described ODS-AQ, pore size 10nm, particle size 10μm, packed to a column bed pressure of 1000psi, Varian chromatography packing system, 300g dry powder described ODS-AQ super water-resistant filler, 600mL isopropanol is stirred and homogenized, poured into a Load&Lock4002 preparation column with an inner diameter of 50mm, the compression ratio is 1.5:1, and the carrier gas is N 2 , adjust the carrier gas pressure so that the oil pressure gauge pressure is 1500psi, and dynamically axially compress to a column bed height of 25cm, which is used as a preparative column for reverse-phase enrichment, reverse-phase salt conversion and reverse-phase purification schemes.

Embodiment 2

[0059] Example 2 Reverse Phase Enrichment, Reverse Phase Salt Conversion and Reverse Phase Purification of Vasopressin [5-Asp] Impurity Crude Solution

[0060] Instrument: Varian SD-1 high pressure liquid phase preparation system

[0061] Chromatographic column: the preparation column Load&Lock4002 50 * 250mm of embodiment 1, packing is ODS-AQ has a particle size of 10 μm and a pore size of 10 nm.

[0062] The structural formula of the vasopressin [5-Asp] impurity is The concentration of the reduced vasopressin [5-Asp] impurity crude product solution in the reduced vasopressin [5-Asp] impurity crude product solution is 1 mg / mL, and the solvent in the vasopressin [5-Asp] impurity crude product solution contains three Aqueous solutions of fluoroacetic acid and acetic acid.

[0063] Mobile phase A is 0.02% acetic acid / water solution by volume, mobile phase B is 0.02% acetic acid / acetonitrile by volume, sample C1 is vasopressin [5-Asp] impurity crude product solution, HPLC pu...

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Abstract

The invention discloses a method for refining impurities of vasopressin [5‑Asp]. The refining method of vasopressin [5-Asp] impurity comprises the steps of: adopting high performance liquid phase chromatography to carry out reverse-phase enrichment, reverse-phase salt conversion, reverse phase Phase purification can be done; the packing of high performance liquid phase chromatography is super water-resistant packing; reverse-phase enrichment, reverse-phase salt conversion, and reverse-phase purification are all completed in a one-step reverse-phase elution process. The purification method of the vasopressin [5‑Asp] impurity of the present invention produces mostly waste water in the purification process, which can be reused after simple treatment at a sewage station, and is economical and environmentally friendly.

Description

technical field [0001] The invention relates to a method for refining vasopressin [5-Asp] impurities. Background technique [0002] Vasopressin is a synthetic polypeptide consisting of nine amino acid residues with a chemical structure of The theoretical molecular weight of vasopressin is 1084.24. Belongs to neurohypophyseal hormone, also known as vasopressin or vasopressin, it has two receptors V1 and V2. V1 is mainly distributed on the membrane of vascular smooth muscle cells, and acts through the receptor-G protein-second messenger pathway to constrict blood vessels and increase blood pressure. V2 is found in the epithelial cells of the distal tubule and collecting duct of the kidney, and physiological doses can promote the reabsorption of water by the distal tubule and collecting duct of the kidney, thereby exerting an antidiuretic effect. [0003] As far as a drug is concerned, a small amount of impurities contained in it is the most important cause of side effects ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/16C07K1/20
Inventor 江锡铭朱鑫磊黄龙黄臻辉丁金国
Owner SPH NO 1 BIOCHEM & PHARMA CO LTD
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