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Method for purifying Leuprorelin

A technology for leuprolide and purpose, applied in the field of HPLC, can solve problems such as no large-scale production, and achieve the effect of good yield and high purity

Active Publication Date: 2009-12-09
HYBIO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the published literature and patents, there is no large-scale production and high yield purification process report

Method used

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  • Method for purifying Leuprorelin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Sample treatment: Dissolve each gram of crude peptide with a mixture of ultrapure water, acetonitrile and acetic acid (V water: V acetonitrile: V acetic acid = 85:10:5), and filter the sample after it is completely dissolved, and collect the filtrate spare.

[0024] 2. The first step of purification: 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: A phase: 0.1%-0.3% phosphoric acid aqueous solution with triethylamine to adjust the pH to 2.0-3.0; B phase: acetonitrile and methanol (V acetonitrile: V methanol = 4:1) mixture. Flow rate: 70-80ml / min. Detection wavelength: 280nm. Gradient: B%: 12% to 43% (55min). The injection volume is 1.3-1.5g.

[0025] Purification process: equilibrate the chromatographic column with mobile phase A and load the sample, the sample volume is 13-15ml of sample solution. After...

Embodiment 2

[0028] 1. Sample treatment: Dissolve each gram of crude peptide with a mixture of ultrapure water, acetonitrile and acetic acid (V water: V acetonitrile: V acetic acid = 85:10:5), and filter the sample after it is completely dissolved, and collect the filtrate spare.

[0029] 2. The first step of purification: purification conditions: chromatographic column: a chromatographic column with octaalkylsilane bonded silica gel as the stationary phase, and the diameter and length of the column are: 15cm×25cm. Mobile phase: A phase: 0.1%-0.3% phosphoric acid aqueous solution with triethylamine to adjust the pH to 2.0-3.0; B phase: acetonitrile and methanol (V acetonitrile: V methanol = 4:1) mixture. Flow rate: 450-550ml / min. Detection wavelength: 280nm. Gradient: B%: 18% to 33% (45min). The injection volume is 13-15g.

[0030] Purification process: equilibrate the chromatographic column with mobile phase A and load the sample, the sample volume is 130-150ml of sample solution. Af...

Embodiment 3

[0033] 1. Sample treatment: Dissolve each gram of crude peptide with a mixture of ultrapure water, acetonitrile and acetic acid (V water: V acetonitrile: V acetic acid = 85:10:5), and filter the sample after it is completely dissolved, and collect the filtrate spare.

[0034] 2. The first step of purification: 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: 30cm×25cm. Mobile phase: A phase: 0.1%-0.3% phosphoric acid aqueous solution with triethylamine to adjust the pH to 2.0-3.0; B phase: acetonitrile and methanol (V acetonitrile: V methanol = 4:1) mixture. Flow rate: 1900-2200ml / min. Detection wavelength: 280nm. Gradient: B%: 12% to 53% (65min). The injection volume is 55-75g.

[0035] Purification process: equilibrate the chromatographic column with mobile phase A and load the sample, the sample volume is 550-750ml of sample solution. ...

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Abstract

The invention discloses a method for purifying Leuprorelin, which comprises the following steps: 1) after crude peptide synthesized by a solid phase is dissolved, using reverse-phase silica gel column as the solid phase, flowing-phase phosphate buffer solution as an A phase and mixed solution of chromatographic pure acetonitrile and methanol as a B phase to carry out gradient elution and purification, and collecting peptide solution of a target peak value; and 3) exchanging phosphate into acetate by adopting negative ions. The invention provides the process method which is suitable for industrialized purification of the Leuprorelin; and the method for purifying the Leuprorelin by using reverse-phase efficient liquid chromatography has high purity and good yield, and achieves the industrialized requirement.

Description

technical field [0001] The invention belongs to the technical field of HPLC, in particular to a method for large-scale purification of leuprorelin. Background technique [0002] Leuprorelin, the Chinese name of the preparation is Leuprorelin acetate, Innaton or Leuprolide for short, and the English name is Leuprorelin acetate, Enanton, Lucrin, etc. Its structure is: [0003] [0004] Molecular formula: C 59 h 84 N 16 o 12 [0005] Molecular weight: 1209.41 [0006] CAS accession number: 53714-56-0 [0007] Leuprolide is a GnRH analogue with the same effect as buserelin. Repeated administration of large doses of luteinizing-releasing hormone (LH-RH) or its highly active derivative leuprolide acetate can produce a transient excitatory effect on the pituitary-gonadal system immediately after the first administration (acute effect), It then inhibits the production and release of gonadotropins by the pituitary gland. It also further suppresses the response of the ovar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/06C07K1/16A61P15/00A61P35/00
Inventor 康旭覃亮政李红玲马亚平袁建成
Owner HYBIO PHARMA
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