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Purification method of desmopressin acetate

A desmopressin and polymer technology, applied in the preparation method of peptides, chemical instruments and methods, oxytocin/vasopressin, etc., can solve the problem of low yield of desmopressin finished products, Amopressin can not be effectively separated, and the purity of desmopressin finished product is not high, so as to achieve the effect of low impurity, high yield and high purity

Active Publication Date: 2015-05-13
ADLAI NORTYE BIOPHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The technical problem to be solved in the present invention is: select a kind of purification method of desmopressin, solve (1) desmopressin finished product purity is not high, (2) desmopressin finished product yield is not high, ( 3) The problem that desmopressin and impurity des-Gln4-desmopressin cannot be effectively separated

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  • Purification method of desmopressin acetate
  • Purification method of desmopressin acetate
  • Purification method of desmopressin acetate

Examples

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Embodiment 1

[0095] Synthesis of Step 1 Fmoc-Gly-RinkAmide-AM-Resin

[0096] Weigh Rink Amide AM resin (substitution degree 0.73mmol / g) (3.29g, 2.4mmol, 1.0equiv) into a solid-phase synthesis tube, add DCM (40mL), stir and swell at a temperature of 10-30°C for 30min, and remove by suction liquid. Then add DMF (20mL×2) to wash. Measure 20% (v / v, the same below) Piperidine / DMF solution (17mL), add it into the solid-phase synthesis tube, control the temperature at 20-30°C and stir for 5min, then remove the liquid by suction filtration. Measure 20% Piperidine / DMF solution (17mL) again, put it into the solid-phase synthesis tube, control the temperature at 20-30°C and stir for 10min, then remove the liquid by suction filtration. Measure DMF (20mL×6) into the solid-phase synthesis tube for washing, and remove the liquid by suction filtration. Separately weigh Fmoc-Gly-OH (2.14g, 3.0equiv) and Cl-HOBt (1.34g, 3.3equiv) into the beaker. Measure DMF (10mL) into a beaker, stir to dissolve comple...

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Abstract

The invention relates to a purification method of desmopressin acetate. The purification method of desmopressin acetate is characterized by comprising the following steps: firstly, dissolving a desmopressin acetate crude product with water, and regulating pH to be acid; secondly, setting a gradient according to volume fraction, and washing a polymer reversed phase chromatographic column; thirdly, loading the solution obtained in the step 1 into the polymer reversed phase chromatographic column; fourthly, setting the gradient according to the volume fraction, maintaining the set gradient for 2 minutes, then increasing the ratio of the flowing phase B to 25% within 5 minutes, then increasing the ratio of the flowing phase B to 40% within 30 minutes, and partially collecting an elution fraction, wherein a flowing phase during an initial state of an elution gradient is 5%; fifthly, drying the elution fraction to obtain the purified desmopressin acetate product.

Description

Technical field: [0001] The invention relates to a method for purifying desmopressin. Background technique: [0002] Desmopressin, English name: Desmopressin, is a cyclic polypeptide with the following structural formula: [0003] [0004] Can be abbreviated as: [0005] [0006] Desmopressin is a structural analogue of natural arginine salt vasopressin, which is obtained by making two changes to the chemical structure of the natural hormone, namely deamination of L-cysteine ​​and conversion of 8-D-arginine Acid substitution 8-L-arginine. Desmopressin acetate has good hemostatic effect and does not cause deep vein thrombosis. It is mainly used for the treatment of hemophilia, diabetes insipidus, therapeutic control of bleeding and prevention of bleeding before surgery. The effect is good and the side effect is small, and it is a polypeptide drug with a good market prospect. [0007] Chinese patent CN101372504 discloses a method for purifying desmopressin. The spec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/16C07K1/20
Inventor 路杨杨东晖陈晓航
Owner ADLAI NORTYE BIOPHARMA CO LTD