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Detection method for effectively separating Lesinurad from main impurities

A detection method and technology for main impurities, which are applied in the field of medicine and biology, can solve the problems such as the failure to achieve the separation degree of Recinade and Impurity I, and achieve the effects of easy adjustment, strong practicability and simple operation.

Inactive Publication Date: 2020-06-02
北京鑫开元医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Since the impurities mainly present in the synthetic sample are similar in polarity to Raysnard and are easily wrapped in the main peak, to achieve complete baseline separation, the high performance liquid chromatography method reported in the literature or the optimization method based on the above method, the Raysnard Sinard and impurity I failed to achieve a certain degree of resolution

Method used

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  • Detection method for effectively separating Lesinurad from main impurities
  • Detection method for effectively separating Lesinurad from main impurities
  • Detection method for effectively separating Lesinurad from main impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Select a sample of Resinard and perform the detection according to the following steps:

[0042] S1. Preparation of mobile phase:

[0043] Take 2.72g of potassium dihydrogen phosphate, add 1000ml of purified water to dissolve, and adjust the pH value to 3.0 with phosphoric acid.

[0044] Mobile phase A: Phosphate buffer at pH 3.0;

[0045] Mobile phase B: Methanol;

[0046] S2. Preparation of the test solution: accurately weigh 10 mg of Resinard sample to a 50ml volumetric flask, add acetonitrile to dissolve and mix evenly, and prepare a solution containing 0.2 mg of Resinard in every 1 ml as the test solution. stand-by;

[0047] S3. Accurately weigh 10mg of impurity I reference substance into a 100ml volumetric flask, add acetonitrile to dissolve and mix evenly, then accurately measure 0.1ml into a 50ml volumetric flask, and then accurately weigh 10mg of Resinard sample into a 50ml volumetric flask , add acetonitrile to dissolve and mix evenly, and prepare a mixed ...

Embodiment 2

[0060] The difference between this example and Example 1 is that the detectors used in the chromatographic conditions are different, and other detection conditions are consistent with Example 1.

[0061] In this embodiment, the detector used is DAD.

[0062] It can be seen from the test that the purity of the Resinard sample and the peak of impurity I are 0.999998 and 0.999991 respectively.

Embodiment 3

[0064] The detection conditions of this embodiment are consistent with those of Embodiment 1.

[0065] In this embodiment, the signal-to-noise ratio of the prepared Leycinard sample solution is 10:1 as the quantification limit, and the signal-to-noise ratio is 3:1 as the detection limit.

[0066] It can be seen from the test that the detection limit of Resinard is 0.019 μg / ml, and the quantification limit is 0.058 μg / ml.

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Abstract

The invention relates to a detection method for effectively separating Lesinurad from main impurities. The detection method comprises a method for separating impurities with polarity close to that ofa main peak in a Lesinurad sample by using high performance liquid chromatography, particularly separating the impurities 2-((5-chloro-4-(4-cyclopropyl-1-naphthalene)-4H-1, 2, 4-triazole-3-yl) thio)acetic acid from the main peak effectively. In the actual detection process, the detection limit of the detection method reaches 0.019 mu g / ml, the impurities with approximate polarities can be effectively separated, the practicability is high, and the detection process is simple and rapid.

Description

technical field [0001] The invention relates to a detection method for effective separation of lecinard and main impurities, which belongs to the field of medical biotechnology. Background technique [0002] Lesinurad (Lesinurad), the chemical name is 2-((5-bromo-4-(4-cyclopropyl-1-naphthalene)-4H-1,2,4-triazol-3-yl)thio ) acetic acid. Resinard is a new type of drug for the treatment of gout, which can reduce uric acid levels by inhibiting urate transporter 1 and promoting uric acid excretion. Clinical studies have shown that Recinard is well tolerated and can reduce the level of uric acid in plasma in a dose-related manner. Combining it with xanthine oxidase inhibitors (allopurinol and febuxostat) can improve The response rate of gout patients who do not respond well to the above drugs can effectively accelerate the elimination of uric acid in gout patients, and it has high safety and good market prospects. The chemical structural formula of Raycinard is: [0003] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/8679G01N2030/047
Inventor 夏中宁吴进王仕伟
Owner 北京鑫开元医药科技有限公司