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Preparation method of cetrorelix acetate freeze-dried preparation

A technology of cetrorelix acetate and freeze-dried preparations, applied in the field of pharmaceutical preparations, can solve the problem of high content

Pending Publication Date: 2022-07-08
QILU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yet the applicant finds that the product prepared by this freeze-drying process all easily produces impurity deamidation cetrorelix impurity (D-21739) and acetylated cetrorelix (D-21739) under the accelerated condition of 40 ℃ / 75%RH through repeated tests. -64308), and its high content

Method used

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  • Preparation method of cetrorelix acetate freeze-dried preparation
  • Preparation method of cetrorelix acetate freeze-dried preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Step 1: Preparation of Cetrorelix Acetate Liquid for Injection

[0052] Accurately weigh 28.1mg of cetrorelix acetate, put it in a 50ml beaker, add 30% acetic acid solution, dissolve, transfer to a 100ml beaker containing 50ml water for injection, add 5.48g of mannitol, dissolve and prepare this solution with water for injection. 102g; immediately filter the feed solution with a 0.2μm filter membrane under aseptic conditions and dispense it into a washed colorless 2ml injection bottle and plug it with a sterile freeze-drying stopper, the filling volume is 1.0ml (1.021g).

[0053] Step 2: Freeze-Drying Process

[0054] Specific steps are as follows:

[0055] 1) Freezing stage: 1.0°C / min plate temperature to 0°C, hold for 15min, continue to cool down to -40°C at 1.0°C / min, hold for 2h, and then continue to cool down to -45°C at a cooling rate of 1.0°C / min ℃, keep warm for 0.5h;

[0056] 2) Annealing stage: the temperature of the plate layer is raised to -20°C at 1.0°C / ...

Embodiment 2

[0060] The preparation of cetrelix acetate liquid medicine for injection is the same as the first step of Example 1.

[0061] Step 2: Freeze-Drying Process

[0062] 1) Freezing stage: cool down to -45°C at a temperature of 1.0°C / min and keep the temperature for 3h;

[0063] 2) Annealing stage: the temperature of the plate layer is raised to -10°C at 2.0°C / min, and the holding time is 0.5h; the temperature of the plate layer is lowered to -40°C at 2.0°C / min, and the holding time is 1h;

[0064] 3) sublimation stage: the pressure is 15Pa, the temperature of the plate layer is heated to -10°C at 0.8°C / min, and the holding time is 12h;

[0065] 4) Drying stage: the temperature of the board layer was raised to 15°C at 1.5°C / min, and the holding time was 10h.

Embodiment 3

[0067] The preparation method of cetrorelix acetate liquid medicine for injection is the same as that of the first step of Example 1.

[0068] Step 2: Freeze-Drying Process

[0069] 1) Freezing stage: Decrease the plate temperature to -5°C at 2.0°C / min and keep it for 10min; continue to cool down to -35°C at a cooling rate of 2.0°C / min and keep it for 3h; then continue to cool down to -35°C at 2.0°C / min 40 ℃, heat preservation 0.8h.

[0070] 2) Annealing stage: the temperature of the plate layer is raised to -15°C at 1.5°C / min, and the holding time is 0.7h; the temperature of the plate layer is lowered to -44°C at 1.5°C / min, and the holding time is 0.5h;

[0071] 3) sublimation stage: the pressure is 18Pa, the temperature of the board is heated to -15°C at 0.9°C / min, and the holding time is 11h;

[0072] 4) Drying stage: the temperature of the board layer was raised to 18°C ​​at 1.2°C / min, and the holding time was 9h.

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Abstract

The invention relates to the field of medicinal preparations, in particular to a preparation method of a cetrorelix acetate freeze-dried preparation, which is characterized in that an annealing process is introduced, so that impurities generated in a freeze-drying process can be effectively reduced, particularly deamidated cetrorelix and acetylated cetrorelix, and the content of the deamidated cetrorelix and acetylated cetrorelix is controlled at a lower level. In addition, the pharmaceutical composition prepared by the method has good stability.

Description

technical field [0001] The invention relates to the field of pharmaceutical preparations, in particular to a freeze-drying process for reducing impurities deamidated cetrelix and acetylated cetrelix in freeze-dried preparations of cetrelix acetate. Background technique [0002] Cetrorelix is ​​a GNRH antagonist, which can be used for patients undergoing controlled ovarian stimulation to prevent premature ovulation, and then perform egg collection and assisted reproductive technology treatment. The drug has a good clinical application prospect in assisted reproductive technology. [0003] Cetrorelix is ​​a synthetic decapeptide with five unnatural D-amino acids to enhance activity and resistance to proteolytic enzymes. The marketed product is Cetrorelix acetate for injection, which is a Sterile lyophilized formulation. [0004] At present, there are the following disclosures about the preparation method of cetrorelix acetate freeze-dried preparation: CN1112019A discloses a c...

Claims

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Application Information

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IPC IPC(8): A61K9/19A61K38/09A61K47/26A61P15/08
CPCA61K9/19A61K38/09A61K47/26A61P15/08
Inventor 李明亮黄河青孙彦华杨清敏徐先艳张明会李延志
Owner QILU PHARMA
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