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Separation detecting method of trelagliptin succinate and enantiomer thereof

A technology of troxagliptin succinate and enantiomers, which is applied in the field of separation and detection of troxagliptin succinate and its enantiomers, can solve the problems that enantiomers cannot be separated, To achieve the effect of strong specificity and high accuracy

Inactive Publication Date: 2016-12-14
ZHENGZHOU MINGZE MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Enantiomers cannot be separated by conventional high performance liquid chromatography and must be separated using a suitable chiral column
[0006] Therefore, there is no effective method for the accurate and sensitive separation and detection of trexagliptin succinate and its enantiomers reported in the literature at present.

Method used

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  • Separation detecting method of trelagliptin succinate and enantiomer thereof
  • Separation detecting method of trelagliptin succinate and enantiomer thereof
  • Separation detecting method of trelagliptin succinate and enantiomer thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Experimental equipment and conditions:

[0039] Waters 1525 high performance liquid chromatograph, Waters 2487 ultraviolet detector;

[0040] Chromatographic column: polysaccharide coated normal phase chiral column CHIRALCEL OJ-H;

[0041] Mobile phase: n-hexane-isopropanol solution, n-hexane-isopropanol solution contains 0.05% ethylenediamine, and the volume ratio of n-hexane to isopropanol is 70:30;

[0042] Flow rate: 0.5mL / min;

[0043] Detection wavelength: 230nm;

[0044] Column temperature: 28°C;

[0045] Injection volume: 20μL;

[0046] Detector: UV detector is used.

[0047] Experimental steps:

[0048] Step (1), solution preparation

[0049] Blank solution: ethanol with a purity of 99.9%;

[0050] Preparation of the test solution: take by weighing 50 mg of trexagliptin succinate, place in a 50 ml measuring bottle, add 99.9% ethanol to dissolve and dilute to the mark;

[0051] Preparation of system suitability solution: Weigh 50 mg of trexagliptin succ...

Embodiment 2

[0060] Experimental equipment and conditions:

[0061] Waters 1525 high performance liquid chromatograph, Waters 2487 ultraviolet detector;

[0062] Chromatographic column: polysaccharide coated normal phase chiral column CHIRALCEL OJ-H;

[0063] Mobile phase: n-hexane-absolute ethanol solution, n-hexane-absolute ethanol solution contains 0.01% diethylamine, and the volume ratio of n-hexane to isopropanol is 60:40;

[0064] Flow rate: 1.5mL / min;

[0065] Detection wavelength: 230nm;

[0066] Column temperature: 25°C;

[0067] Injection volume: 20μL;

[0068] Detector: UV detector is used.

[0069] Experimental steps:

[0070] Step (1), solution preparation

[0071] Blank solution: ethanol with a purity of 99.9%;

[0072] Preparation of the test solution: take by weighing 50 mg of trexagliptin succinate, place in a 50 ml measuring bottle, add 99.9% ethanol to dissolve and dilute to the mark;

[0073] Prepare system suitability solution: weigh 50 mg of trexagliptin succin...

Embodiment 3

[0078] Experimental equipment and conditions:

[0079] Waters 1525 high performance liquid chromatograph, Waters 2487 ultraviolet detector;

[0080] Chromatographic column: polysaccharide coated normal phase chiral column CHIRALCEL OJ-H;

[0081] Mobile phase: n-hexane-absolute ethanol solution, n-hexane-absolute ethanol solution contains 0.01% triethylamine, and the volume ratio of n-hexane to isopropanol is 60:40;

[0082] Flow rate: 1.0mL / min;

[0083] Detection wavelength: 230nm;

[0084] Column temperature: 35°C;

[0085] Injection volume: 20μL;

[0086] Detector: UV detector is used.

[0087] Experimental steps:

[0088] Step (1), solution preparation

[0089] Blank solution: ethanol with a purity of 99.9%;

[0090] Preparation of the test solution: take by weighing 50 mg of trexagliptin succinate, place in a 50 ml measuring bottle, add 99.9% ethanol to dissolve and dilute to the mark;

[0091] Prepare system suitability solution: weigh 50 mg of trexagliptin suc...

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Abstract

The invention relates to the field of medicine analytical chemistry, in particular to a separation detecting method of trelagliptin succinate and enantiomer thereof. According to the method, a polysaccharide-coating-type normal-phase chiral column serves as a chromatographic column, a normal-hexane-low-alcohol solution serves as a mobile phase material, the content of the trelagliptin succinate and the content of the enantiomer of the trelagliptin succinate can be quantitatively measured, specificity is high, accuracy is high, and the separation detecting method can be used for effectively controlling the mass of trelagliptin succinate raw materials.

Description

technical field [0001] The invention relates to the field of pharmaceutical analytical chemistry, in particular to a method for separating and detecting trexagliptin succinate and its enantiomers. Background technique [0002] Trelagliptin is a once-weekly dipeptidyl peptidase IV (DPP-4) inhibitor that controls blood glucose levels through selective and sustained inhibition of DPP-4. DPP-4 is an enzyme that triggers the inactivation of incretins (glucagon-like peptide-1 (GLP-1) and glucose-dependent insulinotropic polypeptide (GIP), which are It plays an important role in regulation.Inhibition of DPP-4 can increase blood glucose level-dependent insulin secretion, thereby controlling blood glucose levels. [0003] The chemical structural formula of Trexagliptin is as follows: [0004] [0005] Separation of enantiomers containing chiral carbon atoms has always been a difficult point in quality control during the synthesis and preparation of chiral drugs. Trexagliptin su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 王永彬郭海波徐培明
Owner ZHENGZHOU MINGZE MEDICAL TECH