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Method for separation and determination of Edoxaban tosylate hydrate and isomer impurities thereof by chiral high performance liquid chromatography

A technology of edoxaban tosylate and high-performance liquid chromatography, which is applied in the field of drug analysis, can solve problems such as the detection of edoxaban tosylate hydrate isomers that have not yet been seen, and achieve quality controllability, Easy operation and high sensitivity

Active Publication Date: 2018-01-05
NANJING CHANGAO PHARMA SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The literature "Determination of Enantiomer Content in Rivaroxaban by HPLC" (Chinese Pharmacist, 2014, 17(10): 1629-1631) reported that Zhang Qianru et al. used Chiralpak IA chiral column to separate rivaroxaban and Its enantiomers, but there is no literature report on the detection of isomers of edoxaban tosylate hydrate

Method used

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  • Method for separation and determination of Edoxaban tosylate hydrate and isomer impurities thereof by chiral high performance liquid chromatography
  • Method for separation and determination of Edoxaban tosylate hydrate and isomer impurities thereof by chiral high performance liquid chromatography
  • Method for separation and determination of Edoxaban tosylate hydrate and isomer impurities thereof by chiral high performance liquid chromatography

Examples

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Embodiment 1

[0032] Example 1 Validation of the method for the determination of isomers Edox-II and Edox-III in edoxaban tosylate hydrate according to the present invention.

[0033] Chromatographic column: DAICEL CHIRALCEL OX-H chiral chromatographic column (size 4.6mm×250mm, 5μm);

[0034] Mobile phase: methanol-ethanol-diethylamine (40:60:0.3);

[0035] Detection wavelength: 290nm;

[0036] Flow rate: 1.0mL / min;

[0037] Column temperature: 35°C.

[0038] 1.1 System suitability test

[0039] Take an appropriate amount of Edox reference substance, Edox-II and Edox-III, add mobile phase to dissolve and make a mixed solution containing 1 mg of Edox, 5 μg of Edox-II and 5 μg of Edox-III per 1 ml, accurately measure 20 μl, and follow the above chromatographic conditions Injection analysis, the result shows: Edox-Ⅲ, Edox, Edox-Ⅱ peaks successively, and the resolution between the three is 15.5 and 13.3, reaching the baseline separation (see figure 1 ).

[0040] 1.2 Specificity test

[0...

Embodiment 2

[0063] Example 2 Determination of isomers Edox-II and Edox-III in the Edoxaban Toluenesulfonate Hydrate Tablets of the present invention.

[0064] Take an appropriate amount of Edox reference substance, Edox-II and Edox-III, add mobile phase to dissolve and make a mixed solution containing 1 mg of Edox, 5 μg of Edox-II and Edox-III per 1 ml, as a system suitability solution. Take an appropriate amount of edoxaban tosylate hydrate tablet fine powder, accurately weighed, add mobile phase to dissolve and dilute to make a solution containing about 1.0 mg of edoxaban tosylate hydrate per 1 ml, shake well, filter Then, as the test solution, accurately measure 1.0ml, put it in a 100ml measuring bottle, dilute to the mark with mobile phase, shake well, and use it as a control solution. Take an appropriate amount of blank excipients for Edoxaban Toluenesulfonate Hydrate Tablets, add mobile phase to dissolve and dilute to make a solution of corresponding concentration, as the blank exci...

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Abstract

The invention discloses a method for separation and determination of an Edoxaban tosylate hydrate and isomer impurities thereof by chiral high performance liquid chromatography. The method uses a chiral chromatographic column adopting silica gel coated with cellulose-tri(4-chloro-3-methylphenyl carbamate) as the filler, and takes a methanol-ethanol mixed solution added with an alkaline additive asthe mobile phase. The method provided by the invention can realize complete separation of edoxaban from isomers Edox-II and Edox-III. The method is convenient in operation, and is verified to be goodin specificity, high in sensitivity, precise and accurate. The method provided by the invention can accurately perform quantitative analysis of Edoxaban tosylate hydrate bulk drugs and the isomers Edox-II and Edox-III of preparations thereof, thus guaranteeing the quality controllability of the Edoxaban tosylate hydrate and preparations thereof.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for separating and measuring edoxaban tosylate hydrate and its isomer impurities by chiral high-performance liquid chromatography. Background technique [0002] Edoxaban Toluenesulfonate Hydrate is a small molecule oral anticoagulant developed by Japan's Daiichi Sankyo Co., Ltd., which is a coagulation factor X (FXa) blocker. It was approved by the Japanese Ministry of Health, Labor and Welfare (MHLW) in April 2011. Approved for marketing in Japan, it is used to prevent venous thromboembolism after major orthopedic surgery, including total knee surgery, total hip surgery and hip fracture surgery. It was approved by the US Food and Drug Administration (FDA) in January 2015 as a commodity Savaysa is listed in the United States for reducing the risk of stroke and systemic embolism in patients with non-valvular atrial fibrillation. [0003] The structure of edoxaban tosylate hy...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 范婧王秀云魏伟王益群谢少斐李纬黄海燕朱丽君
Owner NANJING CHANGAO PHARMA SCI & TECH CO LTD
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