Novel process for preparing eptifibatide by purification
A new technique of eptifatid, which is applied in the field of high-purity centrifuged chromatography to prepare high-purity aptiferin, can solve the problems of large investment, expensive production equipment, and difficulty in large-scale production, so as to reduce the difficulty of sample pretreatment, Reduce the loss of samples and the probability of contamination, which is conducive to the effect of industrial scale production
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Embodiment 1
[0018] Adopt Pilot-Scale preparative high-speed centrifugal separation chromatograph (FCPC), the solvent selects dichloromethane-acetonitrile-water system to prepare eptifibatide. Firstly, the above solvent system was arranged in a separatory funnel at a volume ratio of 2:1:3, shaken evenly, and allowed to stand to separate into layers. Separate the upper and lower layers, take the upper phase as the stationary phase, and the lower phase as the mobile phase. Take 100 grams of crude eptifibatide, dissolve it in 1 liter of the above-mentioned mixed system, filter it with a 0.45um organic phase membrane, and wait for purification. A French Kromaton preparative high-speed centrifugal separation chromatograph is used, with a rotor volume of 5 liters. First, the entire column is filled with the stationary phase, the speed of the main engine is adjusted to 1000 rpm, and the mobile phase is pumped into the column at a flow rate of 150 ml. After the whole system is balanced, inject th...
Embodiment 2
[0021] Using Pilot-Scale preparative high-speed centrifugal separation chromatograph (FCPC), the solvent is ethyl acetate-acetonitrile-water (3:1:3) system to prepare aptifertide. The sample load is 150 grams, and the method is the same as in Example 1.
Embodiment 3
[0023] Using Pilot-Scale preparative high-speed centrifugal separation chromatograph (FCPC), the solvent is ethyl acetate-methanol-water (3:1:3) system to prepare aptifertide. The sample load is 150 grams, and the method is the same as in Example 1.
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