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Analysis method for Vildagliptin intermediate-5 enantiomer detection

A technology for enantiomers and intermediates, which is applied in the field of high-performance liquid chromatography analysis and determination of vildagliptin intermediate-5 enantiomers, and achieves the advantages of simple operation, perfect quality standards, quality assurance and curative effect. Effect

Inactive Publication Date: 2017-04-19
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the process of synthesizing this compound, its enantiomers may affect the purity and quality of vildagliptin intermediate-5 due to incomplete removal. In the later stage of vildagliptin, there is no other refining means to reduce vildagliptin The content of enantiomers, so the enantiomers of vildagliptin can only be controlled by controlling the content of enantiomers of vildagliptin intermediate-5

Method used

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  • Analysis method for Vildagliptin intermediate-5 enantiomer detection
  • Analysis method for Vildagliptin intermediate-5 enantiomer detection
  • Analysis method for Vildagliptin intermediate-5 enantiomer detection

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Experimental program
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Effect test

Embodiment 1

[0021] Instruments and Conditions

[0022] High performance liquid chromatography: Hitachi L-2000

[0023] Column: CHIRALPAK ® AD-H Chiral Chromatographic Column (4.6×250mm)

[0024] Mobile phase: n-hexane-ethanol-methanol=65:25:10

[0025] Flow rate: 0.8mL / min

[0026] Column temperature: 35°C

[0027] Detection wavelength: 210nm

[0028] Injection volume: 10 μL.

[0029] Experimental procedure

[0030] System suitability solution: Take vildagliptin intermediate-5 isomer: 5.1 mg and place it in a 10 mL volumetric flask, dissolve in ethanol to constant volume to obtain impurity stock solution. Take Intermediate-5: 50.2 mg, put it in a 50 mL volumetric flask, add 1.0 mL of impurity stock solution, add ethanol to dissolve, dilute to volume, and shake well to obtain the system suitability solution.

[0031] Take the system suitability solution and carry out high-performance liquid chromatography analysis according to the above-mentioned chromatographic conditions, and con...

Embodiment 2

[0034] Instruments and Conditions

[0035] With embodiment 1.

[0036] Experimental procedure

[0037] Preparation of the test solution: Weigh the samples of 3 batches of Vildagliptin Intermediate-5 small test respectively: small test 1 batch 25.3 mg, small test 2 batches 24.6 mg, small test 3 batches 25.1 mg in 3 In a 25 mL volumetric flask, add ethanol to dissolve and constant volume, shake well as the test solution, take the test sample for high performance liquid chromatography analysis according to the above chromatographic conditions, record the chromatogram, and one batch of small test is used as vildagliptin A typical HPLC chromatogram for the detection of the enantiomers of Intermediate-5 is shown in image 3 , Vildagliptin intermediate-5 enantiomer detection results were normalized according to the area, and the results of the vildagliptin intermediate-5 enantiomer content were shown in Table 1.

[0038] The detection result of table 1 embodiment 2

[0039] ...

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Abstract

The invention relates to a method for analyzing and measuring a Vildagliptin intermediate-5 enantiomer through high performance liquid chromatography. The method comprises the steps that a CHIRALPAK-AD-H type chiral chromatographic column is adopted, and after normal hexane-ethyl alcohol-methyl alcohol is adopted as a flow phase for chromatographic column separation, an ultraviolet detector is used for detecting the Vildagliptin intermediate-5 enantiomer. By means of the method, the enantiomer in Vildagliptin intermediate-5 can be effectively detected, and the quality of the Vildagliptin intermediate-5 can be better ensured. The method has the advantages of being high in specificity, high in accuracy and good in reproducibility.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for analyzing and measuring vildagliptin intermediate-5 enantiomer by high performance liquid chromatography. Background technique [0002] Vildagliptin is a dipeptidyl peptidase Ⅳ inhibitor, which is a new oral drug for the treatment of diabetes. Vildagliptin intermediate-5 is one of the key intermediates in the synthesis of vildagliptin. Its chemical name is: S -1-(2-Chloroacetyl)pyrrolidine-2-carbonitrile. structural formula. [0003] Molecular formula: C 7 h 9 ClN 2 O; molecular weight: 172.61. [0004] In the process of synthesizing this compound, its enantiomers may affect the purity and quality of vildagliptin intermediate-5 due to incomplete removal. In the later stage of vildagliptin, there is no other refining means to reduce vildagliptin Therefore, the enantiomer of vildagliptin can only be controlled by controlling the content of en...

Claims

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Application Information

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IPC IPC(8): G01N30/34G01N30/60G01N30/74
CPCG01N30/34G01N30/60G01N30/74
Inventor 高子彬栗伟娜陈玺孙勇军张丽男张勇翟梦宇刘怡胡佳
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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