Degarelix acetate lyophilized powder injection and preparation method thereof

[0017] Example 1

[0018]

[0019] Accurately weigh mannitol and sodium acetate, add 90% water for injection, dissolve and stir evenly, then add degarelix acetate, dissolve and stir evenly, adjust the pH to 0.5mol/L acetic acid or 0.1mol/L sodium hydroxide solution 5.0. After passing the intermediate inspection, add water for injection to the full amount. The solution is pumped into a sterile room, filtered through a 0.22μm microporous filter membrane until it is clear, and filled into a 10ml vial with a volume of 4ml per bottle, added with a butyl rubber stopper, and placed on a plate. Put the loaded sample to be freeze-dried in a freeze-drying box, close the door, turn on the machine, and cool down. When the product temperature reaches -40℃, keep it for 3 hours, and then open the condenser valve. When the condenser valve temperature reaches -45 When the temperature is ℃, turn on the vacuum pump, when the vacuum reaches 20Pa or less, start heating and sublimation drying, the final drying temperature is 25℃, keep the temperature for 2 hours, finally press the plug, take out the box, tie the mouth with aluminum-plastic combination, and package after passing the quality inspection , You can.

[0020] Example 2

[0021]

[0022] Accurately weigh mannitol and sodium acetate, add 90% water for injection, dissolve and stir evenly, then add degarelix acetate, dissolve and stir evenly, adjust the pH to 0.5mol/L acetic acid or 0.1mol/L sodium hydroxide solution 7.4. After passing the intermediate inspection, add water for injection to the full amount. The solution is pumped into a sterile room, filtered through a 0.22μm microporous filter membrane until it is clear, and filled into a 10ml vial with a volume of 4ml per bottle, added with a butyl rubber stopper, and placed on a plate. Place the sample to be freeze-dried on the plate in a freeze-drying oven, close the door, turn on, and cool down. When the product temperature reaches -40℃, keep it for 2 hours, and then open the condenser valve. When the condenser valve temperature reaches -45 When the temperature is ℃, turn on the vacuum pump, when the vacuum reaches below 20Pa, start to heat up and sublimate and dry, and finally the drying temperature is 25℃, keep the temperature for 4 hours, finally press the plug, take out the box, tie the mouth with aluminum-plastic combination, and package after passing the quality inspection , You can.

[0023] Example 3

[0024]

[0025]

[0026] Accurately weigh mannitol and sodium acetate, add 90% water for injection, dissolve and stir evenly, then add degarelix acetate, dissolve and stir evenly, adjust the pH to 0.5mol/L acetic acid or 0.1mol/L sodium hydroxide solution 6.5. After passing the intermediate inspection, add water for injection to the full amount. The solution is pumped into a sterile room, filtered through a 0.22μm microporous filter membrane until it is clear, and filled into a 10ml vial with a volume of 4ml per bottle, added with a butyl rubber stopper, and placed on a plate. Put the loaded sample to be freeze-dried in a freeze-drying box, close the door, turn on the machine, and cool down. When the product temperature reaches -40℃, keep it for 3 hours, and then open the condenser valve. When the condenser valve temperature reaches -45 When the temperature is ℃, turn on the vacuum pump, when the vacuum reaches 20Pa or less, start to heat up and sublimate and dry, and finally the drying temperature is 25℃, keep the temperature for 3 hours, finally press the plug, take out the box, tie the mouth with aluminum-plastic combination, and package after passing the quality inspection , You can.