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Method for refining oxytocin [5-Asp] impurities

A refining method, 5-asp technology, applied in the preparation method of peptide, chemical instrument and method, oxytocin/vasopressin and other directions, can solve the problem of uneconomical, low impurity removal rate and large amount of organic hazardous waste liquid and other problems to achieve the effect of reducing the production volume and optimizing the production process

Active Publication Date: 2019-07-23
SPH NO 1 BIOCHEM & PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is to overcome the low removal rate of impurities in the crude product solution of oxytocin [5-Asp] impurities when refining oxytocin [5-Asp] impurities in the prior art, and the organic hazardous waste produced The liquid volume is large, and the waste liquid treatment cost that causes is big, uneconomic defect, and a kind of purification method of oxytocin [5-Asp] impurity is provided

Method used

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  • Method for refining oxytocin [5-Asp] impurities
  • Method for refining oxytocin [5-Asp] impurities
  • Method for refining oxytocin [5-Asp] impurities

Examples

Experimental program
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Effect test

Embodiment 1

[0055] Embodiment 1 inner diameter 50mm L&L4002 preparative column packing:

[0056] Using Load&Lock dynamic axial compression and static locking technology, the packing is ODS-AQ, pore size 10nm, particle size 10μm, packed to column bed pressure 1000psi, using Varian chromatography packing system, 300g dry powder filler, 600ml isopropanol after stirring and homogenizing, poured into L&L4002 preparative column with inner diameter 50mm, compression ratio 1.5: 1, the carrier gas is N 2 , adjust the carrier gas pressure so that the oil pressure gauge pressure is 1500psi, and the dynamic axial compression to the height of the column bed is 25cm, which is used as a preparative column for reverse-phase enrichment, reverse-phase salt conversion and reverse-phase purification schemes.

Embodiment 2

[0057] Example 2 Reverse-phase enrichment, reverse-phase salt conversion and reverse-phase purification of oxytocin [5-Asp] impurity crude product solution

[0058] Instrument: Varian SD-1 high pressure liquid phase preparation system

[0059] Chromatographic column: self-packed preparative column Load&Lock4002 50 × 250mm of embodiment 1, ODS-AQ 10μm10nm

[0060] The structural formula of oxytocin [5-Asp] impurity is The concentration of the reduced oxytocin [5-Asp] impurity crude product in the reduced oxytocin [5-Asp] impurity crude product solution is 1 mg / ml, and the solvent in the oxytocin [5-Asp] impurity crude product solution is Aqueous solutions of trifluoroacetic acid and acetic acid.

[0061] Mobile phase A is 0.02% acetic acid / water by volume percentage, mobile phase B is 0.02% acetic acid / acetonitrile by volume percentage, sample C1 is the crude product solution of oxytocin [5-Asp] impurity, and the oxytocin [5-Asp] determined according to the HPLC method [ ...

Embodiment 3

[0066] Example 3 Reverse Phase Enrichment, Reverse Phase Salt Conversion and Reverse Phase Purification of Oxytocin [5-Asp] Impurity Crude Solution

[0067] Instrument: Varian SD-1 high pressure liquid phase preparation system

[0068] Chromatographic column: self-packed preparative column Load&Lock4002 50 × 250mm of embodiment 1, ODS-AQ 10μm10nm

[0069] The structural formula of oxytocin [5-Asp] impurity is The concentration of the reduced oxytocin [5-Asp] impurity crude product solution in the reduced oxytocin [5-Asp] impurity crude product solution is 1.5 mg / ml, and the solvent in the oxytocin [5-Asp] impurity crude product solution It is an aqueous solution of trifluoroacetic acid and acetic acid.

[0070] Mobile phase A is 0.02% acetic acid / water by volume percentage, mobile phase B is 0.02% acetic acid / acetonitrile by volume percentage, sample C1 is the crude product solution of oxytocin [5-Asp] impurity, and the oxytocin [5-Asp] determined according to the HPLC me...

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Abstract

The invention discloses a method for refining oxytocin [5-Asp] impurities. The refining method comprises the following steps: sequentially performing reversed-phase enrichment, reversed-phase salt transferring and reversed-phase purification on oxytocin [5-Asp] impurity crude product solutions by adopting a high-performance liquid-phase reversed phase chromatography method to obtain a final product, wherein the oxytocin [5-Asp] impurity crude product solutions are obtained through oxidizing reductive type oxytocin [5-Asp] impurity crude product solutions which are subjected to solid phase synthesis; and filler required in the the high-performance liquid-phase reversed phase chromatography is water-superresisting filler. According to the refining method disclosed by the invention, a polypeptide pure product is obtained through an on-line one-step method of the reversed-phase enrichment, reversed-phase salt transferring and reversed-phase purification, a removal ratio of the impurities in the oxytocin [5-Asp] impurity crude product solutions is higher, and production processes are optimized; and moreover, flowing phases of a column equilibration stage, a sampling enrichment stage anda salt transferring stage are aqueous solutions, environmental protection and pollution are avoided, and waste liquid which flows out can be directly applied to sewage treatment and can be also recycled.

Description

technical field [0001] The invention relates to a method for refining oxytocin [5-Asp] impurities. Background technique [0002] Oxytocin, also known as oxytocin, English name is Oxytocin, structural formula: [0003] [0004] The molecular formula is: C 43 h 66 N 12 o 12 S 2 , the molecular weight is 1007.2 [0005] Oxytocin is used to induce labor, oxytocin, postpartum and post-abortion uterine bleeding caused by uterine atony or poor abdominal contraction; understand placental reserve function (oxytocin provocation test); nasal drops can promote milk discharge. Oxytocin can indirectly stimulate the contraction of uterine smooth muscle, simulating the uterine contraction of normal childbirth, leading to cervical dilatation, and the uterine response to oxytocin gradually increases during pregnancy and reaches its peak at full term. Oxytocin can also stimulate the contraction of the smooth muscle of the mammary gland, which helps the milk to be discharged from the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/16C07K1/20
CPCC07K7/16
Inventor 江锡铭丁金国黄臻辉
Owner SPH NO 1 BIOCHEM & PHARMA CO LTD