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Method for measuring optical purity of R-alogliptin benzoate

A technology of alogliptin and optical purity, which is applied in the field of determination of optical purity of R-benzoic acid alogliptin, can solve the problem of low separation efficiency and achieve the effect of improving separation efficiency

Inactive Publication Date: 2015-12-30
DISHA PHARMA GRP +1
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Problems solved by technology

[0008] Purpose of the present invention: in order to solve the problem that separation efficiency is lower, we have developed the chiral chromatography that adopts the mobile phase that adds ion pair to measure R-benzoic acid Alogliptin Optical Purity Method

Method used

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  • Method for measuring optical purity of R-alogliptin benzoate
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  • Method for measuring optical purity of R-alogliptin benzoate

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Embodiment 1

[0033] The determination of the optical purity of embodiment 1R-benzoic acid alogliptin sample

[0034] Instruments and reagents: high performance liquid chromatography (Hitachi, Japan; Thermo Fisher Scientific Co., Ltd.); C18 chromatographic column (250mm×4.6mm, 5μm; Thermo Fisher Scientific Co., Ltd.); AD-H chiral Chromatographic column (250mm×4.6mm, 5μm; Daicel Pharmaceutical Chiral Technology Co., Ltd.); constant temperature water bath (Jiangsu Jintan Kexing Instrument Factory); electronic constant speed stirrer (Shanghai Shensheng Technology Co., Ltd.).

[0035] n-Hexane (chromatographically pure, Tianjin Biaoshiqi Technology Co., Ltd.); absolute ethanol (chromatographically pure, Tianjin Biaoshiqi Technology Co., Ltd.); trifluoroacetic acid (chromatographically pure, Aladdin Reagent Company); diethylamine ( Analytical grade, Tianjin Guangcheng Chemical Reagent Co., Ltd.); R-benzoic acid alogliptin reference substance (purity ≧ 99.9%, Disha Pharmaceutical Group Drug...

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Abstract

The invention relates to a method for measuring the optical purity of R-alogliptin benzoate. The method is characterized in that a chromatographic system is a high performance liquid chromatograph; a chromatographic column filler is amylose-tris(3,5-dimethylphenyl carbamate); the flow velocity is 0.8 ml / min; the column temperature is 25 DEG C; the measurement wavelength is 278 nm; the sample introduction amount is 20 [mu]l; the chromatographic mobile phases are n-hexane and an ethanol solution which contains 0.2% trifluoroacetic acid and 0.1% diethyl amine; the ratio of n-hexane to the ethanol solution is 80:20; sample introduction is conducted on an R,S-alogliptin benzoate reference solution and an S-alogliptin benzoate reference solution respectively for system suitability analysis at first, and then the optical purity of an R-alogliptin benzoate test solution is measured and the optical purity of an R-alogliptin benzoate sample is calculated according to an area normalization method.

Description

technical field [0001] The invention relates to a method for measuring the optical purity of R-benzoic acid alogliptin. Background technique [0002] Alogliptin Benzoate, chemical name 2-[[6-[(3R)-3-amino-1-piperidinyl]-3,4-dihydro-3-methyl-2,4-dioxo Dai-1(2H)-pyrimidinyl]methyl]benzonitrile benzoate is a novel dipeptidyl peptidase-IV (DPP-IV) inhibitor used for the treatment of type Ⅱ diabetes mellitus. The structural formula is shown in formula 1 . [0003] [0004] Formula 1 [0005] R-benzoic acid alogliptin is synthesized by reacting 3-methyl-6-chlorouracil with 2-bromomethylbenzonitrile to generate 2-[(6-chloro-3,4-dihydro-3-methanol Base-2,4-dioxo-1(2H)-pyrimidinyl)methyl]benzonitrile, 2-[(6-chloro-3,4-dihydro-3-methyl-2,4-di Oxo-1 (2H)-pyrimidinyl) methyl] benzonitrile reacts with R-3-aminopiperidine dihydrochloride to generate R-alogliptin, and R-alogliptin reacts with benzoic acid to form salt to obtain R-benzoate alogliptin. [0006] Currently, the optica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 张曼玉付婷婷
Owner DISHA PHARMA GRP
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