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A kind of purification method of triptorelin

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

Active Publication Date: 2016-03-30
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] Example 1 First step purification

[0026] Dissolve the crude peptide at a concentration of 100 g / L in an aqueous acetonitrile solution with a volume ratio of 5%, stir to completely dissolve the sample, filter 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, the diameter and length of the column: 5cm×25cm. Mobile phase: Phase A: 0.1% phosphate buffer (v / v), adjusted to pH 2.0 with sodium hydroxide; Phase B: Acetonitrile, flow rate: 60-80ml / min, gradient: B%: 20% to 40%, Linear gradient elution 60min; detection wavelength: 230nm. The injection volume is 1.5g. Collect the target peaks and purify the samples with purity greater than 95% and single impurities less than 0.3% to remove most of the acetonitrile, and then transfer the salt. The part with a purity of less than 95% and greater than 80% is recovered once, and the part wi...

Embodiment 2

[0028] Example 2 The first step purification

[0029] Use a 15% DMSO aqueous solution to dissolve the crude peptide at a concentration of 100g / L, stir to completely dissolve the sample, 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, the diameter and length of the column: 5cm×25cm. Mobile phase: Phase A: 0.8% phosphate buffer (v / v), adjusted to pH 3.0 with ammonia; Phase B: Acetonitrile, flow rate: 60-80ml / min, gradient: B%: 20%-40%, linear gradient Elution 60min; detection wavelength: 230nm. The injection volume is 1.5g. Collect the target peaks and purify the samples with purity greater than 95% and single impurities less than 0.3% to remove most of the acetonitrile, and then transfer the salt. The part with a purity of less than 95% and greater than 80% is recovered once, and the part with a purity of greater than 95% a...

Embodiment 3

[0031] Example 3 First step purification

[0032] Use a 10% isopropanol aqueous solution to dissolve the crude peptide at a concentration of 100 g / L, stir to completely dissolve the sample, filter 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, the diameter and length of the column: 5cm×25cm. Mobile phase: Phase A: 0.2% sulfate buffer (v / v), pH 2.0 adjusted 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 is 1.5g. Collect the target peaks and purify the samples with purity greater than 95% and single impurities less than 0.3% to remove most of the acetonitrile, and then transfer the salt. The part with a purity of less than 95% and greater than 80% is recovered once, and the part with a purity of greater than 9...

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PUM

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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 method for purifying polypeptide drugs, in particular to a method for purifying triptorelin, and belongs to the field of medicinal chemistry. Background technique [0002] Triptorelin, English name: Triptorelin, trade name Tryptorelin, Tabijia, Decapeptyl, etc., is a gonadotropin releasing hormone (GnRH) decapeptide homolog composed of 10 amino acids, and its structure is similar to Ge Serrelin, its peptide sequence is: Pyr-His-Trp-Ser-Tyr-D-Trp-Leu-Arg-Pro-Gly-NH 2 , Its pamoate (storage preparation) is clinically used. [0003] As a gynecological drug, triptorelin is indicated for: 1. Palliative therapy for advanced prostate cancer; 2. Precocious puberty; 3. Endometriosis, female infertility and uterine fibroids. When administered continuously at a therapeutic dose, this product can strongly inhibit the secretion of gonadotropins, and its activity is stronger than that of natural GnRH. After starting the administration, there wi...

Claims

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Application Information

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Patent Type & Authority Patents(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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