Method for separating ertugliflozin and isomers thereof

A separation method and isomer technology, applied in the field of pharmaceutical analysis, can solve the problems of no separation method, etc., and achieve the effect of low equipment requirements, strong practicability, and strong operability

Active Publication Date: 2020-12-01
上海柏狮生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, there is no separation method for isomeric impurities in epagliflozin products. In summary, it is particularly important to urgently need a separation method for epagliflozin and its isomers

Method used

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  • Method for separating ertugliflozin and isomers thereof
  • Method for separating ertugliflozin and isomers thereof
  • Method for separating ertugliflozin and isomers thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The residence time analysis of the isomers of Egliflozin specifically includes the following steps:

[0046] (1) Preparation of diluent

[0047] Mix acetonitrile and distilled water at a volume ratio of 1:1 to obtain a dilution;

[0048] (2), preparation of Epagliflozin isomer solution

[0049] Accurately weigh 25.0mg of Epagliflozin isomers, in a 50mL volumetric flask, dilute to the 50mL mark with the diluent obtained in step (1), mix well to obtain the Epagliflozin Isomers solution;

[0050] (3), adopt reversed-phase high performance liquid chromatography, carry out chromatographic analysis to the diluent of above-mentioned step (1) gained and the epagliflozin isomer solution of step (2) gained, chromatographic analysis condition is as follows:

[0051] The chromatographic column is Agilent proshell 120 EC-C18 4.6×150mm, 4μm;

[0052] The temperature of the chromatographic column is controlled at 35°C;

[0053] The filler used in the chromatographic column is octa...

Embodiment 2

[0061] A kind of Epagliflozin and the analysis of the residence time and resolution of Epagliflozin isomers in different chromatographic columns, specifically comprise the steps:

[0062] (1) Preparation of diluent

[0063] Mix acetonitrile and distilled water at a volume ratio of 1:1 to obtain a dilution;

[0064] (2), the preparation of Epagliflozin solution

[0065] Accurately weigh 25.0mg of Epagliflozin, in a 50mL volumetric flask, dilute to the 50mL mark with the diluent obtained in step (1), mix well to obtain the Epagliflozin solution;

[0066] (3), preparation of Epagliflozin isomer solution

[0067] Accurately weigh 25.0mg of Epagliflozin isomers, in a 50mL volumetric flask, dilute to the 50mL mark with the diluent obtained in step (1), mix well to obtain the Epagliflozin Isomers solution;

[0068] (4) adopt reverse-phase high-performance liquid chromatography, carry out chromatographic analysis respectively to the epagliflozin solution of step (2) gained and the ...

Embodiment 3

[0073] A mixture of Epagliflozin and its isomers, the analysis of residence time and resolution in different mobile phase ratios, specifically comprises the following steps:

[0074] (1) Preparation of diluent

[0075] Mix acetonitrile and distilled water at a volume ratio of 1:1 to obtain a dilution;

[0076] (2), the preparation of the mixed solution of Epagliflozin and Epagliflozin isomers

[0077] Accurately weigh 25.0mg of Epagliflozin, 0.5mg of Epagliflozin isomers in a 50mL volumetric flask, dilute to the 50mL scale with the diluent obtained in step (1), mix well to obtain Epagliflozin and Epagliflozin A mixed solution in which the net isomers are mixed;

[0078] (3), adopt reverse-phase high-performance liquid chromatography, carry out chromatographic analysis to the mixed solution that the Epagliflozin of step (2) gained and Epagliflozin isomers mix, chromatographic analysis conditions, chromatographic analysis conditions are as follows:

[0079] Chromatographic se...

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Abstract

The invention discloses a method for separating ertugliflozin and an isomer thereof, and belongs to the technical field of pharmaceutical analysis. The separation process comprises the following steps: preparing a diluent, preparing a to-be-separated ertugliflozin product solution, preparing an ertugliflozin isomer positioning solution, preparing an ertugliflozin solution, separating by adopting reversed-phase high-performance liquid chromatography, and the like, wherein the temperature of a chromatographic column is controlled to be 25-40 DEG C and the sample size is controlled to be 10mu L in the separation process of the reversed-phase high performance liquid chromatography; a diode array or ultraviolet absorption unit is used as a detector, the detection wavelength is 210 nm, gradientelution is performed on the chromatographic column by using a mobile phase composed of acetonitrile and distilled water at the mobile phase flow rate of 0.8-1.1 mL/min to realize the separation of theergliflozin and the isomer thereof, and the highest separation degree can reach 6.80. The separating method has the characteristics of high feasibility, strong operability, simplicity and conveniencein operation, good separation effect, low separation cost and the like.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, relates to epagliflozin and its isomers, and in particular to a separation method of epagliflozin and its isomers. Background technique [0002] According to the 2018 Global Diabetes Map (8th Edition) report released by the International Diabetes Federation (IDF), about 425 million adults around the world suffer from diabetes in 2018, and it is estimated that by 2045, the number of diabetic patients may reach 629 million, most of them Diabetes is a growing threat to human health. In recent years, sodium-glucose cotransporter 2 (SGLT2) inhibitors have been developed as a very promising class of drugs for diabetes treatment. SGLT2 is mainly expressed in the proximal convoluted tubule of the kidney. It is a transporter with low affinity and high transport capacity, and about 90% of glucose reabsorption in the human body is completed by it. At present, the SGLT2 inhibitors that have been appr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/89
CPCG01N30/02G01N30/89G01N2030/027
Inventor 王红秀王亚萍宋玉红潘仙华
Owner 上海柏狮生物科技有限公司
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