Method for preparing octreotide acetate and medicine composition with same
A technology of octreotide acetate and composition, which is applied in the field of preparation method of octreotide acetate and pharmaceutical composition thereof, can solve the problems such as lack of protective measures for products, unfavorable storage and transportation, poor stability and the like
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Embodiment 1
[0042] Step 1: Dissolve 2.2 g of octreotide acetate crude product with 10% acetonitrile aqueous solution according to the concentration of 15 mg / ml, ultrasonically dissolve the sample completely and filter it with a filter membrane, collect the filtrate as a crude product solution, and set aside.
[0043] Step 2: Take the crude product solution and use a C8 chromatographic column with a diameter and length of 50mm×250mm. Use isopropanol aqueous solution containing 0.1% trifluoroacetic acid (85% water / 15% isopropanol by volume) as phase A, acetonitrile containing 0.1% trifluoroacetic acid as phase B, flow rate: 55ml / min, gradient: 40% B → 60% B, linear gradient elution, elution 200min, collect the eluate with a purity of more than 95%, and concentrate the collected eluate from the peak of interest to about 20mg / ml by rotary evaporation under reduced pressure for the second Purify the sample step by step.
[0044] Step 3: Use a C18 reverse-phase chromatographic column, the inje...
Embodiment 2
[0050] Step 1: Dissolve 2.5 g solid octreotide acetate crude product at a concentration of 10 mg / ml with 3% acetonitrile aqueous solution, sonicate to dissolve the sample completely and filter it with a filter membrane, collect the filtrate as a crude product solution, and set aside.
[0051] Step 2: Take the crude product solution and use a C8 chromatographic column with a diameter and length of 50mm×250mm. Use isopropanol aqueous solution containing 0.2% trifluoroacetic acid (volume ratio is 75% water / 25% isopropanol) as phase A, acetonitrile containing 0.2% trifluoroacetic acid as phase B, flow rate: 80ml / min, gradient is 15% B → 30% B, linear gradient elution, elution 180min, collect the eluate with a purity greater than 95%, and concentrate the collected eluate from the peak of interest to about 20mg / ml by rotary evaporation under reduced pressure for the second Purify the sample step by step.
[0052] Step 3: Use a C18 reverse-phase chromatographic column, the injection...
Embodiment 3
[0058] Step 1: Dissolve 3.0 g solid octreotide acetate crude product at a concentration of 20 mg / ml with 8% acetonitrile aqueous solution, sonicate to dissolve the sample completely and filter it with a filter membrane, collect the filtrate as a crude product solution, and set aside.
[0059] Step 2: Take the crude product solution and use a C8 chromatographic column with a diameter and length of 50mm×250mm. Take the isopropanol aqueous solution containing 0.2% trifluoroacetic acid (volume ratio is 60% water / 40% isopropanol) as phase A, and the acetonitrile containing 0.2% trifluoroacetic acid as phase B, the flow rate: 100ml / min, the gradient is 20% B → 50% B, linear gradient elution, elution 160min, collect the eluate with a purity greater than 95%, and concentrate the collected eluate from the peak of interest to about 20mg / ml in a vacuum rotary evaporation for the second Purify the sample step by step.
[0060] Step 3: Use a C18 reverse-phase chromatographic column, the i...
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