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Purification method for triptorelin

A technology of buffer salt and acetic acid, which is applied in the purification of polypeptide drugs and the purification of triptorelin, which can solve the problems of difficult to control the limit of impurities in raw materials and difficult to achieve purity

Active Publication Date: 2013-05-29
HYBIO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This separation and purification method is difficult to control the impurity limit of the raw material, and it is difficult to achieve the purity required for medicine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1 first step purification

[0026] Use 5% acetonitrile aqueous solution by volume to dissolve the crude peptide at a concentration of 100 g / L, stir to dissolve the sample completely, filter it with a filter membrane, and collect the filtrate.

[0027] Purification conditions: chromatographic column: a chromatographic column with octadecylsilane bonded silica gel as the stationary phase, and the diameter and length of the column are: 5cm×25cm. Mobile phase: Phase A: 0.1% phosphate buffer (v / v), adjust pH 2.0 with sodium hydroxide; Phase B: acetonitrile, flow rate: 60-80ml / min, gradient: B%: 20% ~ 40%, Linear gradient elution 60min; detection wavelength: 230nm. The injection volume was 1.5 g. Collect the target peak, purify the sample with a purity greater than 95% and less than 0.3% impurity, remove most of the acetonitrile and then convert to salt. The part with a purity of less than 95% and greater than 80% is recovered once, and the part with a purity gr...

Embodiment 2

[0028] Embodiment 2 first step purification

[0029] Dissolve the crude peptide with a volume ratio of 15% DMSO aqueous solution at a concentration of 100 g / L, stir to dissolve the sample completely, filter it with a filter membrane, and collect the filtrate.

[0030] Purification conditions: chromatographic column: a chromatographic column with octadecylsilane bonded silica gel as the stationary phase, and the diameter and length of the column are: 5cm×25cm. Mobile phase: Phase A: 0.8% phosphate buffer (v / v), adjust pH to 3.0 with ammonia water; phase B: acetonitrile, flow rate: 60-80ml / min, gradient: B%: 20%-40%, linear gradient Elution 60min; detection wavelength: 230nm. The injection volume was 1.5 g. Collect the target peak, purify the sample with a purity greater than 95% and less than 0.3% impurity, remove most of the acetonitrile and then convert to salt. The part with a purity of less than 95% and greater than 80% is recovered once, and the part with a purity great...

Embodiment 3

[0031] Embodiment 3 first step purification

[0032] Dissolve the crude peptide with a volume ratio of 10% isopropanol at a concentration of 100 g / L, stir to dissolve the sample completely, filter it with a filter membrane, and collect the filtrate.

[0033]Purification conditions: chromatographic column: a chromatographic column with octadecylsilane bonded silica gel as the stationary phase, and the diameter and length of the column are: 5cm×25cm. Mobile phase: Phase A: 0.2% sulfate buffer (v / v), adjust pH 2.0 with phosphoric acid; Phase B: acetonitrile, flow rate: 60-80ml / min, gradient: B%: 20%-40%, linear gradient Elution 60min; detection wavelength: 230nm. The injection volume was 1.5 g. Collect the target peak, purify the sample with a purity greater than 95% and less than 0.3% impurity, remove most of the acetonitrile and then convert to salt. The part with a purity of less than 95% and greater than 80% is recovered once, and the part with a purity greater than 95% an...

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Abstract

The invention provides a purification method for triptorelin, which comprises the following steps: firstly, dissolving a sample by using an aqueous solution containing organic solvents, and carrying out gradient elution on the sample by taking octadecylsilane chemically bonded silica as a stationary phase, taking buffer salts of a phosphoric acid or sulfuric acid as a phase A, and taking acetonitrile as a phase B; then, converting triptorelin phosphates into acetates by using a reversed-phase HPLC (high performance liquid chromatography) method and taking octadecylsilane chemically bonded silica as a stationary phase, and freeze-drying the obtained acetates, so that triptorelin acetates with a purity of more than 99.7% and an individual impurity of less than 99.7% of are obtained, and the total yield is as high as over 30%. The invention provides a triptorelin purification process which is low in cost, high in yield, simple in technological process, less in sample impurities, stable and controllable, and beneficial to the implementation of industrialization.

Description

technical field [0001] The invention relates to a purification method of polypeptide medicine, in particular to a purification method of triptorelin, belonging to the field of medicinal chemistry. Background technique [0002] Triptorelin, English name: Triptorelin, trade names tryptorelin, Dabijia, Decapeptyl, etc., is a gonadotropin-releasing hormone (GnRH) decapeptide analogue composed of 10 amino acids, and its structure is similar to Ge Serelin, its peptide sequence is: Pyr-His-Trp-Ser-Tyr-D-Trp-Leu-Arg-Pro-Gly-NH 2 , clinical use of its pamoate (storage preparation). [0003] Triptorelin is used as a gynecological drug, and its indications are mainly: 1. palliative therapy for advanced prostate cancer; 2. precocious puberty; 3. endometriosis, female infertility and uterine fibroids. When administered continuously at therapeutic doses, this product can strongly inhibit the secretion of gonadotropins, and its activity is stronger than that of natural GnRH. After the s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/23C07K1/20
Inventor 付信刘建马亚平袁建成
Owner HYBIO PHARMA
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