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

Inactive Publication Date: 2009-02-25
HYBIO PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this method is that it is simple and versatile, and is suitable for the purification of most peptides, but the disadvantage is that it is not easy to achieve large-scale production, and the production equipment is very expensive, and the investment is very large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention relates to a new technique for purifying and preparing eptifibatide. At present, the eptifibatide is separated, purified and produced by adopting opposite phase high pressure liquid chromatography. However, mass production is not easy to realize, and the equipment are expensive. Separation and purification are carried out by the method by applying two solvent systems which are not dissolved in each other and make epicyclic motion at high speed in a chromatographic column tube; the processing steps comprises: a. synthetic crude product of the eptifibatide is dissolved by solvent; b. the dissolved crude product of the eptifibatide is separated and purified by high-speed centrifugation separation chromatography (FCPC), and is tested by a uv detector from the distance of 230nm, so that target peak is collected by subsection; c. the collected cut fraction is tested by HPLC, wherein, the cut fraction with the purity higher than 98% is bended to be treated by the next step, and the cut fraction with the purity lower than 98% is recycled and purified again; d. ion exchange is carried out on the cut fraction with qualified purity to remove trifluoroacetic acid (TFA), and then the cut fraction is transformed into acetic acid eptifibatide. The new technique has no irreversible adsorption and the advantages of no loss of sample, no pollution, high speed and high efficiency, and is suitable for mass production.

Description

technical field [0001] The invention relates to the field of medicine and chemical industry, in particular to a new process for preparing high-purity eptifibatide by using high-speed centrifugal separation chromatography (FCPC). Background technique [0002] Eptifibatide is a cyclic polypeptide containing mercaptopropionyl and six amino acid residues, the molecular formula is C 32 h 49 N 11 o 9 S 2 , is a platelet glycoprotein GP IIb / IIIa receptor antagonist, can block the platelet aggregation reaction caused by various activators, is the strongest known specific platelet aggregation inhibitor, and is mainly used to prevent myocardial oxygen supply arterial occlusion , Heart attack, unstable angina, non-Q wave myocardial infarction, sudden death caused by coronary intervention. [0003] The polypeptide has undergone multi-step synthesis, oxidation, and cracking processes, and contains a large amount of insoluble impurities, which makes the pre-treatment of the crude pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/06C07K1/16
Inventor 何平袁建成马亚平
Owner HYBIO PHARMA
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