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Purification method for leuprorelin acetate crude product

A technology of leuprolide acetate and a purification method, which is applied in the field of drug synthesis, can solve problems such as excessive impurities in the purification method, and achieve the effects of improving purity, improving peak shape and low cost

Inactive Publication Date: 2017-09-15
ASYMCHEM LAB TIANJIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The main purpose of the present invention is to provide a kind of purification method of leuprolide acetate crude product, to solve the problem that existing impurity exceeds standard in the purification method of existing leuprolide acetate crude product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Sample handling:

[0040] Each gram of crude leuprolide was dissolved in 20ml of solvent (acetonitrile: acetic acid: water volume ratio: 8:1:1), filtered through a 0.45um membrane to obtain the sample to be tested, and set aside.

[0041] First elution:

[0042] Chromatographic conditions: The chromatographic column uses octadecylsilane and silica gel as the stationary phase. The model of the dynamic axial pressurized column is YMC-ODS-AQ. The diameter and length of the column are 150×250mm; the first mobile phase is 0.05wt% Tri Fluoroacetic acid aqueous solution, the second mobile phase is 0.05wt% trifluoroacetic acid acetonitrile solution, and the detection wavelength is 220nm.

[0043] The above-mentioned chromatographic column is equilibrated using the initial gradient (the second mobile phase is 18wt%), inject 5g of the sample to be tested, and carry out gradient elution under the above-mentioned chromatographic conditions, and the weight percentage of the second ...

Embodiment 2

[0049] The difference from Example 1 is that the weight percentage of the second mobile phase in the first elution step changes positively between 10-20 wt%. The product was leuprolide product with a purity of 99.66wt%, and a yield of 61wt%.

Embodiment 3

[0051] The difference from Example 1 is that the concentration of trifluoroacetic acid in the first mobile phase and the second mobile phase is 0.02wt%. The product was leuprolide product with a purity of 99.46wt%, and a yield of 68wt%.

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Abstract

The invention provides a purification method for a leuprorelin acetate crude product. The purification method comprises performing first elution, namely performing first elution on the leuprorelin acetate crude product by employing a reversed phase chromatographic column, so as to obtain a first elution product, wherein the elution conditions for the first elution comprise that a first mobile phase is an aqueous solution of trifluoroacetic acid, and a second mobile phase is an acetonitrile solution of trifluoroacetic acid; successively performing salt conversion and salt removal on the first elution product, so as to obtain a leuprorelin acetate product. By employing trifluoroacetic acid as the mobile phases, the product purity is improved, chromatographic peak shape tailing is reduced and the peak shape is improved, and then the leuprorelin acetate product is obtained through the processes of salt conversion and salt removal. Additionally, the purification method provided by the invention does not introduce new counter ions, and has the advantages of high product purity, controllable quality, low cost, operation convenience and the like.

Description

technical field [0001] The invention relates to the field of drug synthesis, in particular to a method for purifying a crude product of leuprolide acetate. Background technique [0002] Leuprolide, the Chinese name of the preparation is Leuprolide Acetate, Intraton or Leuprolide for short. 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 ovaries and testes to gonadotropins, thereby reducing the production of estradiol and testosterone (chronic effect). The luteinizing hormone (LH) releasing activity of leuprolide acetate is about 100 times that of LH-RH, and its funct...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/23C07K1/20C07K1/18C07K1/14
CPCC07K7/23
Inventor 卢江平李九远李新勇代洪飞
Owner ASYMCHEM LAB TIANJIN
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