A method for purifying semaglutide
A technology for semaglutide and semaglutide crude peptide, applied in the field of peptide purification, can solve the problems of low yield and low purity of semaglutide samples, and achieve the effect of improving the purity and yield
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Embodiment 1
[0050] Subject
[0051] Sample treatment: 3 g of the mamarut peptide (crude peptide: 4.6 g) sample was dissolved in aqueous acetonitrile solution, and filtered with 0.22 μm filtrate after complete dissolution. The filtered Somalu peptide aqueous solution is collected.
[0052] First step HPLC purification
[0053] Chromatographic conditions: a chromatographic column (30 mm × 250 mm, 10 μm) with a tetrakylsilane bile silica gel (30 mm × 250 mm, 10 μm); with a 0.2% phosphoric acid (taking 1000 ml of water, adding 2 ml of phosphoric acid, mixing uniform, and adjusting pH to 2.3) For mobile phase A; with acetonitrile as mobile phase B; flow rate is 20 ml of per minute; the detection wavelength is 230 nm; the single needle sample is 0.6g. The following table elution gradient was eluted.
[0054]
[0055] The fraction of the Somalu peptide sample having a purity greater than 95% is charged. The water bath temperature was 30 to 35 ° C with a rotary evaporator, and the vacuum was remove...
Embodiment 2
[0062] Subject
[0063] Sample treatment: 8 g of the mamarut peptide crude peptide (crude peptide: 12.2 grams) sample was dissolved in aqueous aqueous acetonitrile, and filtered with 0.22 μm filtration after complete dissolution. The filtered crude peptide solution was collected.
[0064] First step HPLC purification
[0065] Chromatographic conditions: chromatographic columns with tetrakylsilane bile silica gel (50 mm × 250 mm, 10 μm); with 0.2% phosphoric acid (taking 1000 ml of water, adding 2 ml of phosphoric acid, mixing uniform, using ammonia water to adjust pH) to 2.3) For mobile phase a; with acetonitrile as mobile phase B; flow rate is 60 ml of per minute; the detection wavelength is 230 nm; the upper sample is 1.6 g. The following table elution gradient was eluted.
[0066]
[0067] The fraction of the Somalu peptide sample having a purity greater than 95% is charged. The water bath temperature was 30 to 35 ° C with a rotary evaporator, and the vacuum was removed at -0...
Embodiment 3
[0073] Subject
[0074] Sample treatment: 32 g of Somalu peptide crude peptide (crude peptide: 48.8 grams) sample was dissolved in aqueous acetonitrile, and filtered with 0.22 μm filtration after complete dissolution. The filtered crude peptide solution was collected.
[0075] First step HPLC purification
[0076] Chromatographic conditions: a chromatographic column (100 mm × 250 mm, 10 μm) with a tetrakylsilane bilor silica gel (100 mm × 250 mm, 10 μm); with a 0.2% phosphoric acid (taking 1000 ml of water, adding 2 ml of phosphoric acid, mix well, using ammonia water to adjust pH to 2.3) For mobile phase a; with acetonitrile to flow phase B; flow rate of 200 ml of each minute; the detection wavelength is 230 nm; the upper sample is 6.4 g. The following table elution gradient was eluted.
[0077]
[0078] A fraction containing Somalu sample is charged. The water bath temperature was 30 to 35 ° C with a rotary evaporator, and the vacuum was removed at -0.09 MPa or less. The first...
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