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Refining method of pitressin [-NH2] impurities

A technology of -NH2 and refining method, which is applied in the field of refining vasopressin [-NH2] impurities, can solve the problems of uneconomical, large amount of hazardous waste liquid, and high cost of waste liquid treatment, so as to optimize the production process and reduce hazardous waste The effect of production volume

Active Publication Date: 2019-07-12
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 vasopressin [-NH 2 ] A large amount of organic waste liquid is produced in the refining process of impurities, and the amount of hazardous waste liquid is large, resulting in high cost of waste liquid treatment and uneconomical defects, and a vasopressin [-NH 2 ] Purification method of impurities

Method used

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  • Refining method of pitressin [-NH2] impurities
  • Refining method of pitressin [-NH2] impurities
  • Refining method of pitressin [-NH2] impurities

Examples

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preparation example Construction

[0054] In the following examples, vasopressin [-NH 2 ] The preparation method of impurity crude product solution comprises: (1) adopts solid-phase synthesis method to make reduced form vasopressin [-NH 2 ] impurity crude product; (2) the reduced vasopressin [-NH 2 ] The impurity crude product is dissolved and diluted to obtain reduced vasopressin [-NH 2 ] impurity crude product solution; (3) the reduced vasopressin [-NH 2 ] impurity crude product solution obtains described vasopressin [-NH 2 ] impurity crude product solution.

[0055] 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 reduced vasopressin [-NH 2 ] impurity crude product. The peptide cuttin...

Embodiment 1

[0056] Example 1 Load&Lock4002 preparative column with inner diameter of 50mm

[0057] 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

[0058] Example 2 Vasopressin [-NH 2 ] Reverse-phase enrichment, reverse-phase salt conversion and reverse-phase purification of impurity crude product solution

[0059] Instrument: Varian SD-1 high pressure liquid phase preparation system

[0060] 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.

[0061] Vasopressin [-NH 2 ] The structural formula of the impurity is reduced vasopressin [-NH 2 ] Reduced vasopressin [-NH 2 ] The concentration of impurity crude product is 1mg / mL, vasopressin [-NH 2 ] The solvent in the impurity crude product solution is a solution containing trifluoroacetic acid and acetic acid.

[0062] 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 [-NH 2 ] impurity crude product solution, the HPLC purity measured according to the HPLC method...

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Abstract

The invention discloses a refining method of pitressin [-NH2] impurities. The refining method of the pitressin [-NH2] impurities includes the following steps that a pitressin [-NH2] crude product solution is subjected to reverse enrichment, reverse salt converting and reverse purification in sequence with efficient liquid phase reverse chromatography. Filler of the efficient liquid phase reverse chromatography is super-water-tolerant filler. Reverse enrichment, reverse salt converting and reverse purification are all completed in the one-step reverse elution process. According to the refiningmethod of the pitressin [-NH2] impurities, most waste liquid generated in the purification process is waste water, the waste liquid can be reused after being easily treated in a sewage station, and the refining method is economical and environmentally friendly.

Description

technical field [0001] The present invention relates to a kind of vasopressin [-NH 2 ] The refining method of 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 c...

Claims

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Application Information

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IPC IPC(8): C07K7/16C07K1/20
CPCC07K7/16
Inventor 江锡铭朱鑫磊丁金国黄臻辉
Owner SPH NO 1 BIOCHEM & PHARMA CO LTD
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