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Method for separating alogliptin benzoate and its enantiomers by high performance liquid chromatography

A high-performance liquid chromatography, enantiomer technology, applied in the field of medicine, can solve problems such as low activity, and achieve the effect of ensuring effectiveness and safety

Active Publication Date: 2018-11-23
JIANGSU DEYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Benzyl alogliptin has stereoisomerism. Due to the presence of the amino group at the C18 position, it produces two configurations, R and S. The commercially available strong active substance is the R configuration, and the S-isomer has also been reported. Antagonizes the activity of DDP-4, but the activity is more than 1000 times lower than that of the R configuration, and has no activity against other families

Method used

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  • Method for separating alogliptin benzoate and its enantiomers by high performance liquid chromatography
  • Method for separating alogliptin benzoate and its enantiomers by high performance liquid chromatography

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Embodiment 1

[0018] Embodiment 1, a kind of method of high-performance liquid chromatography resolution alogliptin benzoate and its enantiomer: the alogliptin benzoate containing alogliptin benzoate and its enantiomer The raw material drug is dissolved in the diluent to a concentration of 0.1 mg / mL; cellulose-tris(3,5-dichlorophenylcarbamate) covalently bonded to the surface of silica gel is used as the stationary phase, and n-hexane, ethyl acetate , dehydrated ethanol and triethylamine mixed solution are mobile phases, and alogliptin benzoate and its enantiomers are resolved with a high performance liquid chromatography system; the diluent is selected from one of acetonitrile, methanol and ethanol one or a mixture of several. The cellulose-tris(3,5-dichlorophenylcarbamate) chiral column is a bonded chiral chromatography column CHIRALPAK IC. The flow rate of the mobile phase is 0.5mL / min, the temperature of the chromatographic column is 25°C, and the detection wavelength is 220nm. The in...

Embodiment 2

[0019] Embodiment 2, a kind of method of high-performance liquid chromatography resolution alogliptin benzoate and its enantiomer: alogliptin benzoate containing alogliptin benzoate and its enantiomer The raw material drug was dissolved in the diluent to a concentration of 2 mg / mL; cellulose-tris(3,5-dichlorophenylcarbamate) covalently bonded to the surface of silica gel was used as the stationary phase, and n-hexane, ethyl acetate, The mixed solution of absolute ethanol and triethylamine is the mobile phase, and alogliptin benzoate and its enantiomers are resolved with a high-performance liquid chromatography system; the diluent is selected from one of acetonitrile, methanol, and ethanol. Or a mixture of several components. The cellulose-tris(3,5-dichlorophenylcarbamate) chiral column is a bonded chiral chromatography column CHIRALPAK IC. The flow rate of the mobile phase is 2.0 mL / min, the temperature of the chromatographic column is 45° C., and the detection wavelength is ...

Embodiment 3

[0020] Embodiment 3, a kind of method of high-performance liquid chromatography resolution alogliptin benzoate and its enantiomer: the alogliptin benzoate containing alogliptin benzoate and its enantiomer The raw material drug was dissolved in the diluent to a concentration of 1 mg / mL; the stationary phase was cellulose-tris(3,5-dichlorophenylcarbamate) covalently bonded to the surface of silica gel, and n-hexane, ethyl acetate, The mixed solution of absolute ethanol and triethylamine is the mobile phase, and alogliptin benzoate and its enantiomers are resolved with a high-performance liquid chromatography system; the diluent is selected from one of acetonitrile, methanol, and ethanol. Or a mixture of several components. The flow rate of the mobile phase described in 1 is 1.0mL / min, the temperature of the chromatographic column is 35°C, and the detection wavelength is 270nm. The sample injection volume is 10L. In the mobile phase, calculated by volume ratio, n-hexane: ethyl ...

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Abstract

The invention discloses a method for separating Alogliptin benzoate and an enantiomer thereof through high performance liquid chromatography. The method comprises the following steps: dissolving an Alogliptin benzoate raw material medicine containing Alogliptin benzoate and the enantiomer thereof in a dilution solution until the concentration is 0.1-2mg / mL; and separating Alogliptin benzoate and the enantiomer thereof by using a high performance liquid chromatography system adopting silica with the surface being covalently bonded with cellulose-tri(3,5-dichlorophenylcarbamate) as a stationary phase and an n-hexane, ethyl acetate, anhydrous ethanol and triethylamine mixed solution as a mobile phase, wherein the dilution solution is one selected from or a mixture composed of two or more of acetonitrile, methanol and ethanol. The method effectively realizes separation and determination of Alogliptin benzoate and the enantiomer thereof, and guarantees the effectiveness and the safety of Alogliptin benzoate products.

Description

technical field [0001] The invention relates to a method for resolving alogliptin benzoate and its enantiomers, belonging to the technical field of medicine. Background technique [0002] Alogliptin benzoate (Alogliptin benzoate) is a serine protease dipeptidyl peptidase IV (DPP-4) inhibitor developed by Takeda, Japan, which can maintain glucagon-like peptide 1 (GLP-1) and glucose It depends on the level of insulin-promoting polypeptide (GIP), promotes the secretion of insulin, and thus exerts the hypoglycemic effect. [0003] Benzyl alogliptin has stereoisomerism. Due to the presence of the amino group at the C18 position, it produces two configurations, R and S. The commercially available strong active substance is the R configuration, and the S-isomer has also been reported. Antagonizes the activity of DDP-4, but the activity is more than 1000 times lower than that of the R configuration, and has no activity against other families. In the production process, alogliptin ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/027G01N2030/065
Inventor 陈学民杨汉跃董淑波王建涛郑家通
Owner JIANGSU DEYUAN PHARMA
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