Ularitide preparation method
A technology of uralitide and purification method, which is applied in the field of biomedicine, can solve the problems of low purity and long time, and achieve the effect of simplified process technology and easy control
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Embodiment 1
[0009] 1. Take 1g of crude ralitide and dissolve it in water to prepare a saturated solution, put it in a filter device, and filter to remove solid particles;
[0010] 2. Pump the ularitide solution into the dynamic axial compression column to prepare the chromatographic system. The column packing size is Φ50×250mm, the filler is octadecyl silica gel, the particle size is 10um, and the sample volume is 1g. The volume ratio of the mobile phase was 10:90~30:70 for gradient elution for 80 minutes. After ulinaritide was eluted, the mobile phase was switched to acetonitrile with a high proportion to wash out the rear-end impurities, and a separation cycle ended. The detection wavelength of the ultraviolet-visible photometric detector used is 215nm, and the fractions with a retention time of 37-45min are collected, and the purity is ≥98.7% by HPLC analysis.
Embodiment 2
[0012] 1. Take 1.5g of crude ralitide and dissolve it in water to prepare a saturated solution, place it in a filter device, and filter to remove solid particles;
[0013] 2. Pump the ularitide solution into the dynamic axial compression column to prepare the chromatographic system. The column packing size is Φ50×250mm, the packing is octadecyl silica gel, the particle size is 10um, and the sample loading is 1.5g. The volume ratio of the mobile phase was 5:95-30:70 for gradient elution for 80 minutes. After ulinaritide was eluted, the mobile phase was switched to acetonitrile with a high proportion to wash out the rear-end impurities, and a separation cycle ended. The detection wavelength of the ultraviolet-visible photometric detector used was 215nm, and the fractions with a retention time of 42-50min were collected, and the purity was ≥98.5% by HPLC analysis.
Embodiment 3
[0015] 1. Dissolve 2.5g of crude ralitide in water, prepare a saturated solution, put it in a filter device, and filter to remove solid particles;
[0016] 2. Pump the ularitide solution into the dynamic axial compression column to prepare the chromatographic system. The column packing size is Φ150×250mm, the packing is octadecyl silica gel, the particle size is 10um, and the sample loading is 2.5g. The volume ratio of the mobile phase was 5:95-30:70 for gradient elution for 100 minutes. After ulinaritide was eluted, the mobile phase was switched to acetonitrile with a high proportion to wash out the rear-end impurities, and a separation cycle ended. The detection wavelength of the ultraviolet-visible photometric detector used was 215nm, and the fractions with a retention time of 51-59min were collected, and the purity was ≥98.2% by HPLC analysis.
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