Reversed-phase high performance liquid chromatography analysis method of fluralana intermediate hydroximic acid

A reversed-phase high-efficiency liquid phase and reversed-phase high-efficiency liquid phase technology, which is applied in the directions of analyzing materials, material separation, measuring devices, etc., to achieve the effects of high number of plates, quality assurance, and high detection sensitivity

Active Publication Date: 2022-03-04
LIVZON NEW NORTH RIVER PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there are no relevant patent literature reports on this compound and its impurity detection method. With the deepening of domestic research on this product, impurities produced in its production process have gradually been discovered. It is necessary to provide a sensitive, stable and reliable detection method for the quality control of its intermediates and impurities

Method used

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  • Reversed-phase high performance liquid chromatography analysis method of fluralana intermediate hydroximic acid
  • Reversed-phase high performance liquid chromatography analysis method of fluralana intermediate hydroximic acid
  • Reversed-phase high performance liquid chromatography analysis method of fluralana intermediate hydroximic acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] Embodiment 1: the reversed-phase high-performance liquid chromatography analysis method of the oxamic acid of Frellaner intermediate:

[0070] Preparation of the standard solution: Weigh about 10 mg of the oxamic acid, an intermediate of Freylan, accurately weigh it in a 25mL volumetric flask, add an appropriate amount of 60% acetonitrile aqueous solution to dissolve and dilute to the mark, and mix well to obtain Freylal The concentration of the sodium intermediate oxamic acid is 0.4 mg / mL.

[0071] Chromatographic determination conditions:

[0072] Chromatographic column: C18, size 4.6×250mm, 5μm;

[0073] Mobile phase: A: acetonitrile, B: 0.1% phosphoric acid solution;

[0074] Flow rate: 0.8mL / min;

[0075] Column temperature: 25°C;

[0076] Injection volume: 15μL;

[0077] Detection wavelength: 205nm;

[0078] Gradient elution program:

[0079] When the time is 0.0min, the volume fraction of A in the mobile phase is 20%, and the volume fraction of B is 80%; ...

Embodiment 2

[0085] Embodiment 2: System suitability test of the determination of the content of oxamic acid in the intermediate of Frellaner

[0086] Preparation of the standard solution: Weigh 10.2 mg of the intermediate oxamic acid of Freylan, accurately weigh it and put it in a 25mL volumetric flask, add an appropriate amount of 60% acetonitrile aqueous solution to dissolve and dilute to the mark, mix well to obtain Freylan The concentration of the sodium intermediate oxamic acid is 0.408mg / mL.

[0087] Chromatographic determination conditions:

[0088] Chromatographic column: C18, size 4.6×250mm, 5μm;

[0089] Mobile phase: A: acetonitrile, B: 0.1% phosphoric acid solution;

[0090] Flow rate: 0.8mL / min;

[0091] Column temperature: 25°C;

[0092] Injection volume: 15μL;

[0093] Detection wavelength: 205nm;

[0094] Gradient elution program:

[0095] When the time is 0.0min, the volume fraction of A in the mobile phase is 20%, and the volume fraction of B is 80%;

[0096] Whe...

Embodiment 3

[0104] Reproducibility Investigation of Flurelaner Intermediate Xamic Acid

[0105] (1) Preparation of the standard reference substance: Weigh 10 mg of the intermediate of frellaner hydroxamic acid, accurately weigh it into a 25mL volumetric flask, add diluent to dissolve and dilute to the mark, mix well, and use it as the standard reference substance solution.

[0106] (2) Preparation of the test product: Weigh 6 parts of the raw material drug samples of Frellaner intermediate xamic acid respectively: (10.2mg, 10.3mg, 10.1mg, 10.33mg, 10.21mg, 10.36mg), each accurately weighed In a 25mL volumetric flask, dissolve with 60% acetonitrile aqueous solution and dilute to the mark, and mix well to obtain different mass concentrations of Frellaner intermediate hydroxamic acid solutions, which correspond to the standard solutions of numbers 1 to 6 respectively: 0.408mg / mL, 0.412mg / mL, 0.404mg / mL, 0.413mg / mL, 0.408mg / mL, 0.414mg / mL.

[0107] Chromatographic determination conditions: ...

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Abstract

The invention belongs to the field of analysis, and discloses a reversed-phase high-performance liquid chromatography analysis method of fluralan intermediate oximic acid, which comprises the following steps: dissolving by using an acetonitrile aqueous solution, and determining a chromatogram under specific reversed-phase high-performance liquid chromatography conditions, and calculating the content of fluralan intermediate oximic acid (4-(hydroxyimino) methyl)-2-methyl benzoic acid in the sample to be detected according to the chromatogram. The high performance liquid chromatography analysis method for the fluralana intermediate oximic acid has the advantages of high detection sensitivity, high stability, high reliability, high number of theoretical plates and relatively simple operation, can effectively detect the content of the fluralana intermediate oximic acid, and is beneficial to guarantee the quality of fluralana intermediate oximic acid bulk drugs and preparations.

Description

technical field [0001] The invention belongs to the technical field of drug analysis and detection, and in particular relates to a reversed-phase high-performance liquid chromatography analysis method for an intermediate of Freylaner, hydroxamic acid. Background technique [0002] The chemical name of Frellana is 4-[5-(3,5-dichlorophenyl)]-4,5-dihydro-5-trifluoromethyl-3-isoxazolyl]-2-methyl -N-[2-oxo-2-[2.2.2-trifluoroethyl)amino]]benzamide, a novel broad-spectrum insecticide, is a ligand-gated chloride ion channel in neurons A potent inhibitor of , with remarkable selectivity for mammalian and arthropod neurons. The successful research and development of Freilaner has created a new research direction of GABA-gated chloride ion channel disruptors, which are similar to the targets of pesticides such as cyclopentadiene, phenylpyrazoles and macrolides , has good insecticidal activity against pests such as ticks, fleas, lice, hemiptera and diptera, and its toxicity is higher ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/065Y02P20/55
Inventor 王婉盈龚俊姜桥李冰冰
Owner LIVZON NEW NORTH RIVER PHARMA
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