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Method for purifying Eptifibatide

A technology of eptifibatide and phase B, applied in the field of HPLC, can solve the problem of not finding large-scale production and purification process, and achieve the effect of high yield purification and high purity

Active Publication Date: 2009-09-23
HYBIO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the published literature and patents, there is no report or application for large-scale production and a purification process with a higher yield

Method used

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  • Method for purifying Eptifibatide

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Embodiment 1

[0023] 1. The first step of purification: Take a Buchner funnel of appropriate size, put a layer of filter paper, then spread a layer of diatomaceous earth with a thickness of 2cm-3cm, and put a layer of filter paper on top. Pour the oxidized solution of eptifibatide into the funnel for suction filtration under reduced pressure, and collect the filtrate for later use.

[0024] 2. The second step of purification: Purification conditions: chromatographic column: a chromatographic column with alkylsilane bonded silica gel as the stationary phase, and the diameter and length of the column are: 5cm×25cm. Mobile phase: A phase: 0.1% trifluoroacetic acid aqueous solution; B phase: chromatographically pure acetonitrile. Flow rate: 70-80ml / min. Detection wavelength: 280nm. Gradient: B%: 15% ~ 30% (30min), the injection volume is 1.0-1.2g.

[0025] Purification process: equilibrate the chromatographic column with mobile phase A and load the sample, the sample volume is 2.0-2.4L sampl...

Embodiment 2

[0029] 1. The first step of purification: Take a Buchner funnel of appropriate size, put a layer of filter paper, then spread a layer of diatomaceous earth with a thickness of 2cm-3cm, and put a layer of filter paper on top. Pour the oxidized solution of eptifibatide into the funnel for suction filtration under reduced pressure, and collect the filtrate for later use.

[0030] 2. The second step of purification: Purification conditions: chromatographic column: a chromatographic column with alkylsilane bonded silica gel as the stationary phase, and the diameter and length of the column are: 15cm×25cm. Mobile phase: A phase: 0.1% trifluoroacetic acid aqueous solution; B phase: chromatographically pure acetonitrile. Flow rate: 400-500ml / min. Detection wavelength: 280nm. Gradient: B%: 15% to 30% (30min). The injection volume is 15-18g.

[0031] Purification process: equilibrate the chromatographic column with mobile phase A and load the sample, the sample volume is 15-20L samp...

Embodiment 3

[0035] 1. The first step of purification: Take a Buchner funnel of appropriate size, put a layer of filter paper, then spread a layer of diatomaceous earth with a thickness of 2cm-3cm, and put a layer of filter paper on top. Pour the oxidized solution of eptifibatide into the funnel for suction filtration under reduced pressure, and collect the filtrate for later use.

[0036] 2. The second step of purification: Purification conditions: chromatographic column: a chromatographic column with alkylsilane bonded silica gel as the stationary phase, and the diameter and length of the column are: 30cm×25cm. Mobile phase: A phase: 0.1% trifluoroacetic acid aqueous solution; B phase: chromatographically pure acetonitrile. Flow rate: 1500-2000ml / min. Detection wavelength: 280nm. Gradient: B%: 15% to 30% (30min). The injection volume is 60-80g.

[0037] Purification process: equilibrate the chromatographic column with mobile phase A and load the sample, the sample volume is 60-80L sa...

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Abstract

The invention discloses a method for purifying Eptifibatide, which comprises the following steps of: 1) conducting suction filtration with a Buchner funnel containing diatomite to remove slightly soluble impurities; 2) conducting gradient elution and purification with the fixed phase being alkylsilane bonded silica, the phase A of a mobile phase being trifluoroacetic acid aqueous solution and the phase B thereof being chromatographic grade acetonitrile, wherein the mobile phase includes phase A and phase B; and collecting the peptide solution at a target peak value, and conducting reduced pressure distillation and concentration; and 3) using anion exchange method for converting the trifluoroacetate into acetate, thus obtaining the acetic acid Eptifibatide bulk drug which meets the requirement. In the invention, the method which is applicable to the industrialized purification of Eptifibatide is provided; reversed phase high-performance liquid chromatography is used and combined with the anion exchange method for converting the trifluoroacetate into acetate so as to purify the Eptifibatide; and the purity is high, and the purification yield of the yield reaches more than 70 percent and meets the industrialization requirement.

Description

technical field [0001] The invention belongs to the technical field of HPLC, in particular to a method for large-scale purification of Eptifibatide. Background technique [0002] Eptifibatide, also known as Eptifibatide, Eptifibatide, English name: Eptifibatide, molecular formula: C 35 h 49 N 11 o 9 S 2 , CAS accession number 148031-34-9, whose structure is [0003] [0004] Epifibatide is an anti-platelet aggregation agent jointly developed by American COR Therapeutics Company and American Schering-Plough Company. In July 1998, it was first listed in the United States under the trade name Intrifiban by Schering-Plough Company, and in 1999 it was launched in Europe under the trade name Intrifiban. Synonyms IntrifibanTM, Sch-60936, C68-22, SB-1. [0005] Eptifibatide is a cyclic peptide and is a platelet glycoprotein GPIIb / IIIa receptor antagonist, which can block the platelet aggregation reaction caused by various activators, and is the strongest specific platelet ...

Claims

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Application Information

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IPC IPC(8): C07K7/06C07K1/20C07K1/18A61P7/02A61P9/10
Inventor 刘建李红玲马亚平袁建成
Owner HYBIO PHARMA
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