Method for separating and detecting cardio-cerebrovascular drug S-configuration tirofiban

A tirofiban and detection method technology, applied in the field of isomer separation, can solve the problems of increasing tirofiban separation cost, high cost of chiral chromatographic column, short service life, etc.

Active Publication Date: 2017-04-26
上海微谱检测科技集团股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional chiral separation method mostly uses ovomucin chiral chromatographic column for the chiral separation of tirofiban, but the cost of ovomucin chiral chromatographic column is too high and the service life is short, which greatly increases the Therefore, it is urgent to develop a new high-efficiency, low-cost separation and detection method

Method used

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  • Method for separating and detecting cardio-cerebrovascular drug S-configuration tirofiban
  • Method for separating and detecting cardio-cerebrovascular drug S-configuration tirofiban
  • Method for separating and detecting cardio-cerebrovascular drug S-configuration tirofiban

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preparation example Construction

[0040] Preparation of Chitosan Modified Silica Gel Column Stationary Phase

[0041] Soak the silica gel in acid, and reflux, then wash with double distilled water until neutral, wash with acetone three times, bake to remove water and activate, cool and store in a desiccator for later use. Take the activated dry silica gel, add anhydrous dry toluene, and add KH-560 and triethylamine catalyst under stirring. in N 2Heating to reflux under protection, cooling, extracting with toluene, washing with acetone, methanol and acetone in sequence, and drying under vacuum to obtain a coupling agent-bonded silica gel material, and prepare a silica gel precursor.

[0042] Weigh the silica gel precursor, add chitosan, acetic acid and toluene to it under heating and stirring. Perchloric acid was added dropwise as catalyst, in N 2 Heating to reflux under protection, cooling, adjusting the pH to neutral, and precipitating solids to obtain the chitosan-modified silica gel chromatography colu...

Embodiment 1

[0061] Soak 10g of silica gel in 3mol / L hydrochloric acid, heat to reflux for 10h, then wash with twice distilled water until neutral, wash with acetone three times, bake at 150°C to remove water and activate for 8h, cool and store in a desiccator for later use. Take 6.0g of activated dry silica gel, add 100mL of anhydrous dry toluene, add 4.0mL of KH-560 and 3 drops of triethylamine catalyst under stirring. in N 2 Heating to reflux for 24 hours under protection, cooling, extracting with toluene for 24 hours, washing with acetone, methanol and acetone in sequence, and vacuum drying at 80°C for 8 hours to obtain a coupling agent-bonded silica gel material, and prepare a silica gel precursor.

[0062] Weigh 10 g of the silica gel precursor, add chitosan, acetic acid, and toluene therein under heating and stirring. 2 drops of perchloric acid were added dropwise as a catalyst, under N 2 Heating to reflux for 24 hours under protection, cooling, adjusting the pH to neutral, and pr...

Embodiment 2

[0065] Soak 10g of silica gel in 3mol / L hydrochloric acid, heat to reflux for 10h, then wash with twice distilled water until neutral, wash with acetone three times, bake at 150°C to remove water and activate for 8h, cool and store in a desiccator for later use. Take 6.0g of activated dry silica gel, add 100mL of anhydrous dry toluene, add 4.0mL of KH-560 and 3 drops of triethylamine catalyst under stirring. in N 2 Heating to reflux for 24 hours under protection, cooling, extracting with toluene for 24 hours, washing with acetone, methanol and acetone in sequence, and vacuum drying at 80°C for 8 hours to obtain a coupling agent-bonded silica gel material, and prepare a silica gel precursor.

[0066] Weigh 10 g of the silica gel precursor, add chitosan, acetic acid, and toluene therein under heating and stirring. 2 drops of perchloric acid were added dropwise as a catalyst, under N 2 Heating to reflux for 24 hours under protection, cooling, adjusting the pH to neutral, and pr...

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Abstract

A method for separating and detecting a cardio-cerebrovascular drug S-configuration tirofiban includes the steps of (1), weighing tirofiban hydrochloride racemate and subjecting the tirofiban hydrochloride racemate to extraction by a flowing-phase solution so as to obtain an injection sample; (2), adopting high-performance liquid chromatography for chiral separation. The method for separating and detecting the cardio-cerebrovascular drug S-configuration tirofiban has the advantages that the method is excellent in separation degree and capable of reducing chiral separation cost greatly because of cheap and easily available chitosan, thereby being suitable for large-scale industrial production.

Description

technical field [0001] The present invention relates to the separation method of isomer, more specifically, the present invention relates to a kind of separation and detection method of S-configuration of tirofiban, a cardiovascular and cerebrovascular drug. Background technique [0002] Tirofiban hydrochloride (tirofihan hydrochloride), the chemical name is N-(butylsulfonyl)-O-[4-(4-pyridyl)butyl]-L-tyrosine hydrochloride, developed by Merck , is the first marketed non-peptide platelet surface glycoprotein (GP) IIb / IIIa receptor antagonist, which has the advantages of high efficiency, high selectivity, and reversibility. It was first launched in the United States in May 1998, and it was launched in China in August 2004. It is currently the only platelet-type GP IIb / IIIa receptor antagonist in China. It is clinically used for the treatment of acute coronary syndrome, including unstable angina or none. Patients with Q-wave myocardial infarction, as well as patients undergoin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 秦秋明宁飞飞侯小刚贾梦虹姜俊婕
Owner 上海微谱检测科技集团股份有限公司
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