Method for detecting related substances in 4-oxime methyl-1-naphthoic acid

A detection method and a technology related to substances, which are applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as no patent literature reports, and achieve the effects of stable durability, good durability, and high sensitivity

Pending Publication Date: 2022-03-01
LIVZON NEW NORTH RIVER PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there is no relevant patent literature report on the compound and its related substance detection method

Method used

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  • Method for detecting related substances in 4-oxime methyl-1-naphthoic acid
  • Method for detecting related substances in 4-oxime methyl-1-naphthoic acid
  • Method for detecting related substances in 4-oxime methyl-1-naphthoic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] S1: Preparation of reference substance solution: Accurately weigh 10mg of 4-oximemethyl-1-naphthoic acid reference substance in a 20mL volumetric flask, then take 1.0mL of this solution in a 50mL volumetric flask, dissolve and dilute to the mark with a solvent , mix well;

[0043] S2: Preparation of the test solution: Accurately weigh 10 mg of the 4-oximemethyl-1-naphthoic acid test product in a 20 mL volumetric flask, dissolve and dilute to the mark with a solvent, and mix well;

[0044] S3: HPLC measurement: Kromasil 100-5-C18 chromatographic column: 4.6mm * 100mm, 5 μ m; Mobile phase is acetonitrile: 0.01% perchloric acid aqueous solution=(30~80):(70~20)(v / v) Carry out gradient elution, the order of the gradient elution time and the volume ratio of mobile phase acetonitrile is: 0min~8min, 30%~70% operation; 8min~12min, 70%~80% operation; 12min~15min, 80% operation ;15.1min~20min, 30% operation; flow rate: 1.2mL / min; column temperature: 30°C; detection wavelength of...

Embodiment 2

[0047] The detection method of embodiment 2 and embodiment 1 is identical, and difference is the chromatographic condition of S2, specifically:

[0048] Mobile phase is acetonitrile:0.1% perchloric acid aqueous solution=(30~80):(70~20) (v / v) carries out gradient elution, and detection result is as follows figure 2 shown.

[0049] Depend on figure 2 It can be seen that each component can be effectively separated, and the content of impurity A in 4-oximemethyl-1-naphthoic acid calculated by the self-contrast method of the principal component is 0.0034%, the content of impurity B is 0.0019%, and the content of impurity C is 0.0611%. The content of impurity D is 1.1368%, the content of impurity E is 0.0486%, and the peak shape is good.

Embodiment 3

[0050] Embodiment 3: specificity test

[0051] S1: Preparation of impurity stock solution: Take impurity A, impurity B, impurity C, impurity D, and impurity E respectively, add solvent to make the concentration 0.10mg / mL, and use it as a stock solution for later use;

[0052] S2: Preparation of impurity limit solution: pipette 0.5 mL of impurity stock solution into a 20 mL volumetric flask to obtain an impurity limit solution with a concentration of 2.50 μg / mL;

[0053] S3: Preparation of system suitability solution: Accurately weigh 10 mg of 4-oximemethyl-1-naphthoic acid reference substance into a 20 mL volumetric flask, add 0.5 mL each of the above impurity stock solution, dissolve with a solvent and dilute to the mark, mix uniform. The concentration of 4-oximemethyl-1-naphthoic acid is 500 μg / mL, and the concentration of each impurity is 2.50 μg / mL;

[0054] S4: Perform measurement according to the high-performance liquid chromatography conditions in Example 1, inject ea...

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Abstract

The invention belongs to the field of pharmaceutical analysis, and discloses a method for detecting related substances in 4-oxime methyl-1-naphthoic acid. The method comprises the following steps: preparing a reference substance solution and a test solution, determining chromatograms of the reference substance solution and the test solution by using high performance liquid chromatography, and determining the content of the related substances according to a main component self-contrast method. The detection method has the advantages of high specificity, high separation degree, excellent linear relation, high sensitivity, short analysis time and the like, can meet the detection requirements of related substances in 4-oxime methyl-1-naphthoic acid, and is suitable for popularization and application.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical analytical chemistry, and specifically relates to a method for detecting related substances in 4-oximemethyl-1-naphthoic acid. Background technique [0002] Afulaner (trade name: Nixor) is the first anthelmintic in China that can effectively kill both ticks and fleas. Its mechanism of action is to inhibit the GABA chloride ion channel, causing arthropod nerves to be overexcited and lethal. In 2017, Boehringer Ingelheim, the world's second largest animal health company, announced that its oral anthelmintic drug for dogs against ticks and fleas, Nixie, was launched in China. It is popular for its fast killing speed and long-lasting effect. [0003] 4-Oximemethyl-1-naphthoic acid As an intermediate in the production process of arfurana raw materials, it has specific research significance in the production of arfurana raw materials. [0004] At present, there are no relevant patent literatu...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/065
Inventor 谢倩玲李冰冰姜桥温军贤陈果
Owner LIVZON NEW NORTH RIVER PHARMA
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