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Method for determining enantiomer impurities in trelagliptin crude drug and preparation thereof by utilizing HPLC (High Performance Liquid Chromatography)

A technology of enantiomers and raw materials, which is applied in the field of drug analysis, can solve the problems that the enantiomer impurity separation of trexagliptin succinate cannot be realized, and achieve good tolerance, control of drug quality, and precision high degree of effect

Inactive Publication Date: 2017-09-29
WATERSTONE PHARMA WUHAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing patent CN104237421A proposes a method for detecting related substances of trexagliptin succinate and its preparations, wherein the related substances refer to impurities such as solvents, intermediates, By-products, etc., can not achieve the separation of trexagliptin succinate and its enantiomer impurities, therefore, to create a method for separation and analysis of trexagliptin succinate and its enantiomer impurities The quality control of Gliptin's raw materials and preparations has very important practical significance

Method used

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  • Method for determining enantiomer impurities in trelagliptin crude drug and preparation thereof by utilizing HPLC (High Performance Liquid Chromatography)
  • Method for determining enantiomer impurities in trelagliptin crude drug and preparation thereof by utilizing HPLC (High Performance Liquid Chromatography)
  • Method for determining enantiomer impurities in trelagliptin crude drug and preparation thereof by utilizing HPLC (High Performance Liquid Chromatography)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Instrument: Agilent 1100 HPLC, UV detector

[0048] Chromatographic column: CHIRALPAK AD-H (4.6*250mm, 5μm)

[0049] Mobile phase A: a mixed solution containing n-hexane and diethylamine (containing 0.3% by volume of diethylamine)

[0050] Mobile phase B: a mixed solution containing ethanol and diethylamine (containing 0.3% by volume of diethylamine)

[0051] Isocratic elution: mobile phase A (%): mobile phase B (%) = 55:45

[0052] Mobile phase flow rate: 0.8mL / min

[0053] Detection wavelength: 278nm

[0054] Column temperature: 25°C

[0055] Sample solution injection volume: 10μL

[0056] Solvent: ethanol

[0057] Method validation for enantiomers:

[0058] 1. System suitability

[0059] Trexagliptin succinate enantiomer control solution: Accurately weigh an appropriate amount of trexagliptin succinate enantiomer reference substance, add ethanol to dissolve and quantitatively dilute to make a solution containing 2.5 μg per 1 ml.

[0060] Take trexagliptin su...

Embodiment 2

[0101] Instrument: Agilent 1100 HPLC, UV detector

[0102] Chromatographic column: CHIRALPAK AD-H (4.6*250mm, 5μm)

[0103] Mobile phase A: a mixed solution containing n-hexane and diethylamine (containing 0.3% by volume of diethylamine)

[0104] Mobile phase B: a mixed solution containing ethanol and diethylamine (containing 0.3% by volume of diethylamine)

[0105] Isocratic elution: mobile phase A (%): mobile phase B (%) = 55:45

[0106] Flow rate: 0.8mL / min

[0107] Detection wavelength: 278nm

[0108] Column temperature: 25°C

[0109] Injection volume: 10μL

[0110] experiment procedure:

[0111] Trexagliptin succinate enantiomer stock solution: Accurately weigh about 10 mg of the enantiomer reference substance of trexagliptin succinate, put it in a 50ml measuring bottle, add an appropriate amount of ethanol to ultrasonically dissolve and dilute to the mark, shake uniform.

[0112] Separation test solution: Accurately weigh about 10 mg of trexagliptin succinate raw...

Embodiment 3

[0120] Instrument: Agilent 1100 HPLC, UV detector

[0121] Chromatographic column: CHIRALPAK AD-H (4.6*250mm, 5μm)

[0122] Mobile phase A: a mixed solution containing n-hexane and diethylamine (containing 0.2% by volume of diethylamine)

[0123] Mobile phase B: a mixed solution containing ethanol and diethylamine (containing 0.2% by volume of diethylamine)

[0124] Isocratic elution: mobile phase A (%): mobile phase B (%) = 60:40

[0125] Flow rate: 1.0mL / min

[0126] Detection wavelength: 278nm

[0127] Column temperature: 25°C

[0128] Injection volume: 10μL

[0129] experiment procedure:

[0130] Trexagliptin succinate enantiomer stock solution: Accurately weigh about 10 mg of the enantiomer reference substance of trexagliptin succinate, put it in a 50ml measuring bottle, add an appropriate amount of ethanol to ultrasonically dissolve and dilute to the mark, shake uniform.

[0131] Separation test solution: Accurately weigh about 10 mg of trexagliptin succinate raw...

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Abstract

The invention discloses a method for determining enantiomer impurities in a trelagliptin crude drug and a preparation thereof by utilizing an HPLC (High Performance Liquid Chromatography). The analysis conditions of the method are characterized by adopting a chiral chromatographic column with a silica gel surface being coated with amylose-tri(3,5-dimethylphenyl carbamate) as a stationary phase; adopting a mixed solution containing normal hexane and an alkaline additive as a moving phase A and adopting a mixed solution containing ethyl alcohol and the alkaline additive as a moving phase B for carrying out isocratic elution. By adopting the method, the effective separation and determination of a main drug trelagliptin and the enantiomer impurities thereof can be realized, so that the quality control of the trelagliptin crude drug and the preparation thereof can be ensured.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular, the invention relates to a method for measuring the enantiomer impurities in trexagliptin bulk drug and its preparation by using HPLC (high performance liquid chromatography). Background technique [0002] The chemical name of Trelagliptin sμccinate (compound shown in Formula 1) is 2-((6-((3R)-3-amino-1-piperidinyl)-3,4-dihydro-3- Methyl-2,4-dioxo-1(2H)-pyrimidinyl)methyl)-4-fluoro-benzonitrile succinate is the first product originally developed by Takeda in Japan that can achieve weekly A small-molecule diabetes drug administered once, it is a new type of oral dipeptidyl peptidase IV (DPP-4) inhibitor for the treatment of type 2 diabetes, which controls blood sugar levels by selectively and continuously inhibiting DPP-4 . DPP-4 is a cell surface serine protease that triggers the inactivation of incretins (glucagon-like peptide-1 (GLP-1) and glucose-dependent insulinotropic...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 付美玲杭健钱丽娜
Owner WATERSTONE PHARMA WUHAN
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