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A kind of hplc detection method of vildagliptin intermediate-5

A detection method and intermediate technology, applied in the field of HPLC detection of vildagliptin intermediate-5, can solve the problems such as difficulty in guaranteeing the quality and curative effect of vildagliptin

Active Publication Date: 2022-05-03
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the existing process of synthesizing vildagliptin intermediate-5, impurities such as p-toluenesulfonic acid and intermediate-5 amide will be produced, and the quality and curative effect of vildagliptin synthesized by it are difficult to guarantee. The present invention Provide a kind of HPLC detection method of vildagliptin intermediate-5

Method used

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  • A kind of hplc detection method of vildagliptin intermediate-5
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  • A kind of hplc detection method of vildagliptin intermediate-5

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Instruments and Conditions:

[0033] High performance liquid chromatography: Hitachi L-2000;

[0034] Chromatographic column: AgelaVenusil MP C18 (2) column (4.6mm×50mm, 3μm);

[0035] Mobile phase: Phosphate buffer (take 0.01mol / L potassium dihydrogen phosphate solution, adjust pH to 2.4 with 20% (v / v) phosphoric acid solution)-acetonitrile-methanol (200:3:3) as mobile phase A , using phosphate buffer-acetonitrile-methanol (80:90:30) as mobile phase B;

[0036] Flow rate: 1.7ml / min;

[0037] Column temperature: 35°C;

[0038] Detection wavelength: 210nm;

[0039] Injection volume: 10μl;

[0040] The elution method is gradient elution, and the specific elution conditions are: 0-3min, 90→70vol% of phase A, 10→30vol% of phase B; 3-10min, 70→55vol% of phase A, 30→45vol% of phase B; 10-18min, phase A 55vol%, phase B 45vol%; 18-18.1min, phase A 55→90vol%, phase B 45→10%; 18.1-22min, phase A 90vol%, phase B 10vol%.

[0041] experiment method

[0042] Preparation of di...

Embodiment 2

[0047] Instruments and Conditions:

[0048] High performance liquid chromatography: Hitachi L-2000;

[0049] Chromatographic column: AgelaVenusil MP C18 (2) column (4.6mm×50mm, 3μm);

[0050]Mobile phase: use phosphate buffer (take 0.05mol / L potassium dihydrogen phosphate solution, adjust pH to 2 with 30% (v / v) phosphoric acid solution)-acetonitrile-methanol (200:4:4) as mobile phase A , using phosphate buffer-acetonitrile-methanol (80:95:25) as mobile phase B;

[0051] Flow rate: 1.6ml / min;

[0052] Column temperature: 33°C;

[0053] Detection wavelength: 208nm;

[0054] Injection volume: 8μl;

[0055] The elution method is gradient elution, and the specific elution conditions are: 0-3min, 90→70vol% of phase A, 10→30vol% of phase B; 3-10min, 70→55vol% of phase A, 30→45vol% of phase B; 10-18min, phase A 55vol%, phase B 45vol%; 18-18.1min, phase A 55→90vol%, phase B 45→10%; 18.1-22min, phase A 90vol%, phase B 10vol%.

[0056] experiment method

[0057] Preparation of di...

Embodiment 3

[0062] Instruments and Conditions:

[0063] High performance liquid chromatography: Hitachi L-2000;

[0064] Chromatographic column: AgelaVenusil MP C18 (2) column (4.6mm×50mm, 3μm);

[0065] Mobile phase: use phosphate buffer (take 0.1mol / L potassium dihydrogen phosphate solution, adjust pH to 3 with 40% (v / v) phosphoric acid solution)-acetonitrile-methanol (200:5:5) as mobile phase A , using phosphate buffer-acetonitrile-methanol (80:100:35) as mobile phase B;

[0066] Flow rate: 1.8ml / min;

[0067] Column temperature: 37°C;

[0068] Detection wavelength: 212nm;

[0069] Injection volume: 12μl;

[0070] The elution method is gradient elution, and the specific elution conditions are: 0-3min, 90→70vol% of phase A, 10→30vol% of phase B; 3-10min, 70→55vol% of phase A, 30→45vol% of phase B; 10-18min, phase A 55vol%, phase B 45vol%; 18-18.1min, phase A 55→90vol%, phase B 45→10%; 18.1-22min, phase A 90vol%, phase B 10vol%.

[0071] experiment method

[0072] Preparation of ...

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Abstract

The invention relates to the technical field of drug detection, and specifically discloses an HPLC detection method for vildagliptin intermediate-5. The chromatographic condition of described HPLC: chromatographic column: filling agent is octadecylsilane bonded silica gel; Mobile phase: mobile phase A is the phosphate buffer saline-acetonitrile-methanol that volume ratio is 200:3-5:3-5 ;Mobile phase B is phosphate buffer saline-acetonitrile-methanol with a volume ratio of 80:90-100:25-35; column temperature: 33-37°C; detection wavelength: 208-212nm; flow rate: 1.6-1.8ml / min ; The elution method is gradient elution. Each chromatographic peak in the chromatogram obtained by the present invention can be completely separated, and the degree of separation is good, which can ensure the accuracy of the purity detection of vildagliptin intermediate-5 in the sample, and provide the quality and curative effect of the subsequent synthetic vildagliptin Reliable guarantee.

Description

technical field [0001] The invention relates to the technical field of drug detection, in particular to an HPLC detection method for vildagliptin intermediate-5. Background technique [0002] Vildagliptin (Vildagliptin) is a dipeptidyl peptidase Ⅳ inhibitor, it is a new type of oral treatment of diabetes drugs. 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, and its molecular formula is: C7H9ClN2O; molecular weight: 172.61; the chemical structure of Vildagliptin Intermediate-5 is as follows: [0003] [0004] In the process of synthesizing vildagliptin intermediate-5, along with generating p-toluenesulfonic acid, if the removal of p-toluenesulfonic acid is not complete, it will affect the purity and quality of vildagliptin intermediate-5, moreover, residual The p-toluenesulfonic acid may participate in the subsequent reaction to generate genotoxic impuriti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 高子彬候丽蓓黄德胜霍月香臧香环李玲玲孟思付玉飞李硕张惠敏孙艳平孙勇军
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY