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A kind of high-performance liquid chromatography detection method of saxagliptin intermediate and its isomers

A technology of high-performance liquid chromatography and detection method, which is applied in the field of drug analysis, can solve the problems that have not been reported, and achieve the effect of simple method, good separation effect, good quality and stability

Active Publication Date: 2022-07-29
SYNCOZYMES SHANGHAI
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  • Description
  • Claims
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Problems solved by technology

[0005] The separation of optical isomers of compounds containing multiple chiral carbon atoms has always been a difficult point in drug quality control. However, for (1S,3S,5S)-2-azabicyclo[3.1.0]hexane-3- The chiral analysis and determination of carboxamide methanesulfonate and its isomers has not been reported so far

Method used

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  • A kind of high-performance liquid chromatography detection method of saxagliptin intermediate and its isomers
  • A kind of high-performance liquid chromatography detection method of saxagliptin intermediate and its isomers
  • A kind of high-performance liquid chromatography detection method of saxagliptin intermediate and its isomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 HPLC analysis of (1S,3S,5S)-2-azabicyclo[3.1.0]hexane-3-carboxamidemethanesulfonic acid

[0026] Chromatographic conditions:

[0027] Chromatographic column: Daicel AD-H column, 250mm*4.6mm*5um.

[0028] Mobile phase: ethanol / n-hexane / diethylamine (20 / 80 / 0.1, V / V / V), isocratic elution.

[0029] Flow rate: 1.0 mL / min.

[0030] Wavelength: 215nm.

[0031] Column temperature: 25°C.

[0032] Running time: 20min.

[0033] Diluent and blank: ethanol / mobile phase / diethylamine (25 / 75 / 1, V / V / V).

[0034] Test solution concentration: 10mg / mL.

[0035] Injection volume: 20uL.

[0036] Experimental steps:

[0037] Weigh (1S,3S,5S)-2-azabicyclo[3.1.0]hexane-3-carboxamide methanesulfonate and its three isomers (1R,3R,5R)-2-nitrogen Heterobicyclo[3.1.0]hexane-3-carboxamidemethanesulfonate, (1R,3R,5S)-2-azabicyclo[3.1.0]hexane-3-carboxamidemethanesulfonate and ( 1S, 3S, 5R)-2-azabicyclo[3.1.0]hexane-3-carboxamide methanesulfonate) each 100mg into a 10mL volumetric f...

Embodiment 2

[0038] Example 2 HPLC analysis of (1S,3S,5S)-2-azabicyclo[3.1.0]hexane-3-carboxamidemethanesulfonic acid

[0039] Chromatographic conditions:

[0040] Chromatographic column: Daicel AD-H column, 250mm*4.6mm*5um.

[0041] Mobile phase: ethanol / n-hexane / diethylamine (25 / 75 / 0.1, V / V / V), isocratic elution.

[0042] Flow rate: 0.8 mL / min.

[0043] Wavelength: 215nm.

[0044] Column temperature: 30°C.

[0045] Running time: 30min.

[0046] Diluent and blank: ethanol / mobile phase / diethylamine (25 / 75 / 1, V / V / V).

[0047] Test solution concentration: 10mg / mL.

[0048] Injection volume: 10uL.

[0049] Experimental steps:

[0050] Weigh (1S,3S,5S)-2-azabicyclo[3.1.0]hexane-3-carboxamide methanesulfonate and its three isomers (1R,3R,5R)-2-nitrogen Heterobicyclo[3.1.0]hexane-3-carboxamidemethanesulfonate, (1R,3R,5S)-2-azabicyclo[3.1.0]hexane-3-carboxamidemethanesulfonate and ( 1S, 3S, 5R)-2-azabicyclo[3.1.0]hexane-3-carboxamide methanesulfonate) each 100mg into a 10mL volumetric f...

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Abstract

The invention discloses a high-performance liquid chromatography detection method for (1S,3S,5S)-2-azabicyclo[3.1.0]hexane-3-carboxamide methanesulfonate and its isomers. In this method, Daicel AD-H chromatographic column is selected, and the mixed solution of ethanol and n-hexane added with diethylamine is used as the mobile phase, and isocratic elution is carried out. The present invention can accurately measure (1S,3S,5S)-2-azabicyclo[3.1.0]hexane-3-carboxamide methanesulfonic acid and its isomers through one high-performance liquid chromatography detection. content, can achieve a good separation effect.

Description

Technical field: [0001] The invention belongs to the technical field of drug analysis, in particular to the high-performance liquid chromatography detection of (1S,3S,5S)-2-azabicyclo[3.1.0]hexane-3-carboxamide methanesulfonate and its isomers method. Background technique: [0002] Saxagliptin is a highly potent dipeptidyl peptidase-4 (DPP-4) selective and competitive inhibitor jointly developed by Bristol-Myers Squibb and Astra Zeneca, and is mainly used for the treatment of type 2 diabetes. The main mechanism of action of the drug is through reversible, competitive and selective inhibition of dipeptidyl peptidase-4 (DPP-4), reducing the hydrolysis of glucagon-like peptide-1 (GLP-1), and increasing insulin release. Lower blood sugar. The drug has obvious hypoglycemic effect, small toxic and side effects, and high safety. The chemical name for saxagliptin is (1S,3S,5S)-2-[(2S)-2-amino-2-(3-hydroxytricyclo[3.3.1.1] 3,7 ]decan-1-yl)ethyl]-2-azabicyclo[3.1.0]hexane-3-carbon...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 韦玉娜陈玉玉竺伟
Owner SYNCOZYMES SHANGHAI
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