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Analytic method for related substances in raw materials and preparation of trelagliptin succinate

A technology of trelagliptin succinate and related substances is applied in the field of analysis of related substances in raw materials and preparations of trelagliptin succinate, and can solve the problems of inability to judge applicability, inability to cover impurities, not given, etc.

Active Publication Date: 2017-06-27
合肥拓锐生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has the following problems: 1. The patent does not give any known impurities, so the applicability of the method cannot be judged; 2. The wavelength parameter of the modified method is set to 278nm, which cannot cover all impurities

Method used

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  • Analytic method for related substances in raw materials and preparation of trelagliptin succinate
  • Analytic method for related substances in raw materials and preparation of trelagliptin succinate
  • Analytic method for related substances in raw materials and preparation of trelagliptin succinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] High performance liquid chromatography conditions:

[0079] Octadecylsilane bonded silica gel chromatographic column (250×4.6mm, 5μm), with phosphoric acid to adjust pH = 3.5 Potassium dihydrogen phosphate buffer solution and acetonitrile at a volume ratio of 90:10 as mobile phase A, with phosphoric acid to adjust pH =3.5 Potassium dihydrogen phosphate buffered aqueous solution and acetonitrile with a volume ratio of 20:80 is the mobile phase B, the detection wavelength is 220nm, the flow rate is 1.0ml / min, and the column temperature is 35°C. Among them, the potassium dihydrogen phosphate buffered aqueous solution , the concentration of potassium dihydrogen phosphate is 0.025mol / L, and gradient elution is carried out;

[0080] The gradient elution process is: within 0.01-5min, the volume ratio of mobile phase A and mobile phase B is 94:6; within 5-50min, the volume ratio of mobile phase A and mobile phase B is gradually changed from 94:6 to 40:60; within 50-50.01min, t...

Embodiment 2

[0086] High performance liquid chromatography conditions:

[0087] Octadecylsilane bonded silica gel chromatographic column (250×4.6mm, 5μm), with phosphoric acid to adjust pH = 3.3 Potassium dihydrogen phosphate buffer solution and acetonitrile at a volume ratio of 92:8 as mobile phase A, with phosphoric acid to adjust pH =3.3 Potassium dihydrogen phosphate buffered aqueous solution and acetonitrile with a volume ratio of 22:78 is mobile phase B, the detection wavelength is 222nm, the flow rate is 0.95ml / min, and the column temperature is 40°C. Among them, the potassium dihydrogen phosphate buffered aqueous solution , the concentration of potassium dihydrogen phosphate is 0.02mol / L, and gradient elution is carried out; the gradient elution process is the same as in Example 1.

[0088] Sample preparation:

[0089] System suitability solution: same as Example 1.

[0090] Need testing solution: take an appropriate amount of succinate trexagliptin test substance, accurately wei...

Embodiment 3

[0094] High performance liquid chromatography conditions:

[0095] Octadecylsilane bonded silica gel chromatographic column (250×4.6mm, 5μm), with phosphoric acid to adjust pH = 3.7 Potassium dihydrogen phosphate buffer solution and acetonitrile at a volume ratio of 88:12 as mobile phase A, with phosphoric acid to adjust pH =3.7 Potassium dihydrogen phosphate buffered aqueous solution and acetonitrile with a volume ratio of 18:82 is mobile phase B, the detection wavelength is 218nm, the flow rate is 1.05ml / min, and the column temperature is 30°C. Among them, potassium dihydrogen phosphate buffered aqueous solution , the concentration of potassium dihydrogen phosphate is 0.03mol / L, and gradient elution is carried out; the gradient elution process is the same as in Example 1.

[0096] Sample preparation:

[0097] System suitability solution: same as Example 1.

[0098] Need testing solution: with embodiment 2.

[0099] Contrast solution: with embodiment 2.

[0100] Test operat...

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Abstract

The invention discloses an analytic method for related substances in raw material and a preparation of trelagliptin succinate. A high performance liquid chromatography is adopted, and chromatographic conditions include that a chromatographic column is octadecyl silane bonded silica gel chromatographic column, the mixed solution with the pH of 3.3-3.7 and the volume ratio of phosphate buffer aqueous solution to acetonitrile of (88-92):(8-12) is taken as a mobile phase A, the mixed solution with the pH of 3.3-3.7 and the volume ratio of phosphate buffer aqueous solution to acetonitrile of (18-22):(78-82) is taken as a mobile phase B, detection wavelength is 218-222nm and isocratic elution is carried out. The analytic method disclosed by the invention can detect many impurities and can rapidly, effectively and accurately monitor the related substances in trelagliptin succinate.

Description

technical field [0001] The invention relates to the technical field of analytical methods of chemical drugs, in particular to a method for analyzing related substances in trexagliptin succinate raw materials and preparations thereof. Background technique [0002] Trelagliptin succinate, chemical name 2-({6-[(3R)-3-aminopiperidine-1- [0003] base]-3-methyl-2,4-dioxo-3,4-dihydropyrimidin-1(2H)-yl}methyl)-4-fluorobenzonitrile succinate with the formula C 18 h 20 FN 5 o 2 ·C 4 h 6 o 4 , the molecular weight is 475.47, the CAS number is 1029877-94-8, and its structural formula is as follows: [0004] [0005] Trexagliptin is a dipeptidyl peptidase-4 (DPP-4) inhibitor. By inhibiting the activity of DPP-4, the plasma glucagon-like peptide-1 (GLP-1) activity level continues to increase , GLP-1 is an incretin with glucose-dependent insulin-stimulating properties. It can promote insulin secretion from β cells, inhibit inappropriate glucagon secretion from α cells, delay ga...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N21/33
CPCG01N21/33G01N30/02
Inventor 戴德标陆文通单胜男
Owner 合肥拓锐生物科技有限公司
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