A kind of purification method of carbetocin
A carbetocin and purification method technology, applied in the purification field of carbetocin, can solve the problems such as difficulty in separating and obtaining high-purity products, complicated purification and purification process, high cost and the like, and shorten the purification process. route, improve purification efficiency, reduce the number of purification times and the effect of steps
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Embodiment 1
[0052] (1) Sample treatment: The crude carbetocin peptide with a chromatographic purity of 60% to 70% was prepared by solid-phase synthesis, and 3L of a mixed solution of purified water-acetonitrile (1:1) was used, according to 15g to 20g / L The concentration is dissolved, stirred, and after complete dissolution, filter with a 0.45um water-based filter membrane to remove insoluble matter and obtain the filtrate, which is the crude carbetocin solution.
[0053] The HPLC spectrogram of the obtained carbetocin crude product solution is as follows figure 1 shown.
[0054] (2) Salt precipitation:
[0055] First, add trifluoroacetic acid solution (1.0%) to adjust the pH value of the crude product solution to 2.0-2.5, and place it at 2-8°C for refrigerated storage for 2-4h, filter off the gray precipitate; then adjust the pH value of the crude product solution with alkali (ammonia water) solution The value is 7.5-8.5, and stored at 2-8°C for 2-4 hours, filtered to remove the precipi...
Embodiment 2
[0065] (1) Sample processing:
[0066] 55g of carbetocin crude peptide with a chromatographic purity of 60% was obtained by solid-phase synthesis, dissolved in 3L of purified water-acetonitrile (1:1) mixed solution according to the concentration of 15g-20g / L, stirred, and completely dissolved Afterwards, filter with a 0.45um water-based filter membrane to remove insoluble matter and obtain the filtrate, which is the crude carbetocin solution.
[0067] (2) Salt precipitation:
[0068] First add TFA solution (0.5%) to adjust the pH value of the crude product solution to 2.0-2.5, and place it at 2-8°C for refrigerated storage for 2-4h, filter off the gray precipitate; then use alkali (ammonia) solution to adjust the pH value of the crude product solution. 7.5-8.5, and stored at 2-8°C for 2-4 hours, filtered to remove the precipitate; then use TFA solution (0.5%) to adjust the pH value of the crude product solution to 3.5-4.5, and store at 2-8°C for 2 Filter after -4h.
[0069]...
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