A kind of purification method of glucagon
A technology for glucagon and purification methods, which is applied in the direction of preparation methods, chemical instruments and methods of glucagon and peptides, and can solve the problems that glucagon cannot achieve high production efficiency
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Embodiment 1
[0062] Embodiment 1: purification method of the present invention
[0063] 1. Crude peptide pretreatment
[0064] Dissolve 5 g of crude glucagon peptide synthesized in solid phase with pure water until the sample is dissolved, then slowly add ammonia water to adjust the pH to 10, then raise the temperature of the crude peptide solution to 60 degrees Celsius, and slowly add 100 mmol / 1 of guanidine hydrochloride and 300mmol / l of sodium chloride were kept stirring during the addition process. After 20 minutes of reaction, the reverse phase detection reaction was completed, and the temperature of the crude peptide solution was immediately lowered to 37 degrees Celsius with ice water, the reaction was terminated, and the IM conversion process was over. .
[0065] 2. Gradient elution purification
[0066] Purification conditions: chromatographic column: a chromatographic column with octadecyl bonded silica gel as the stationary phase, and the diameter and length of the column are...
Embodiment 2
[0071] Embodiment 2: purification method of the present invention
[0072] 1. Crude peptide pretreatment
[0073] Dissolve 15 g of the crude glucagon peptide synthesized in the liquid phase with pure water until the sample is dissolved, then slowly add ammonia water to adjust the pH to 9.5, then raise the temperature of the crude peptide solution to 55 degrees Celsius, and slowly add 100 mmol / 1 of guanidine hydrochloride and 200mmol / l of sodium chloride, kept stirring during the addition process, after 20 minutes of reaction, the reverse phase detection reaction was completed, immediately lowered the temperature of the crude peptide solution to 37 degrees Celsius with ice water, the reaction was terminated, and the IM conversion process was over .
[0074] 2. Gradient elution purification
[0075] Purification conditions: chromatographic column: a chromatographic column with octadecyl bonded silica gel as the stationary phase, and the diameter and length of the column are: ...
Embodiment 3
[0080] Embodiment 3: purification method of the present invention
[0081] 1. Crude peptide pretreatment
[0082] Dissolve 15 g of the crude glucagon peptide in Example 2 with pure water until the sample is dissolved, then slowly add ammonia water to adjust the pH to 9.5, then raise the temperature of the crude peptide solution to 55 degrees Celsius, and slowly add 100 mmol The guanidine hydrochloride of / l and the sodium chloride of 300mmol / l, keep stirring during the addition process, after reacting for 20min, the reversed-phase detection reaction is completed, and the temperature of the crude peptide solution is immediately lowered to 37 degrees Celsius with ice water, the reaction is terminated, and the IM conversion process End.
[0083] 2. Gradient elution purification
[0084] Purification conditions: chromatographic column: a chromatographic column with octadecyl bonded silica gel as the stationary phase, and the diameter and length of the column are: 10cm×25cm. Mob...
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Abstract
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