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Method for analyzing related impurities of isoxazoline veterinary drug intermediate ammonium salt

An analytical method and isoxazoline technology, which can be used in analytical materials, material separation, instruments, etc., can solve many problems, and achieve the effect of good separation effect and high sensitivity

Active Publication Date: 2022-04-29
LIVZON NEW NORTH RIVER PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to better control the quality of 2-amino-N-(2,2,2-trifluoroethyl) acetamide and Afraner and Freilaner, the present invention is to self-made and most of the 2- The related substances in amino-N-(2,2,2-trifluoroethyl)acetamide have been systematically studied and found that the main impurities are glycine and trifluoroethylamine salts. There are not many reports on the quality research of (2,2,2-trifluoroethyl)acetamide

Method used

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  • Method for analyzing related impurities of isoxazoline veterinary drug intermediate ammonium salt
  • Method for analyzing related impurities of isoxazoline veterinary drug intermediate ammonium salt
  • Method for analyzing related impurities of isoxazoline veterinary drug intermediate ammonium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 1) Preparation of standard reference substance solution: Accurately weigh 2-amino-N-(2,2,2-trifluoroethyl)acetamide standard substance (hereinafter referred to as AY standard substance) and add diluent (the diluent is every 1ml Containing 20 μg of ascorbic acid solution, the same below) dissolved, and prepared into a reference substance solution containing 15 mg of working standard per milliliter of AY standard substance per 1 mL.

[0044] 2) Preparation of the test solution: Accurately weigh 2-amino-N-(2,2,2-trifluoroethyl)acetamide for the test, add diluent and dissolve to make 75 μg of the test in 1ml The solution.

[0045] 3) Impurity D stock solution: Accurately weigh 10 mg of the impurity D reference substance, put it in a 10 ml volumetric flask, add diluent to dissolve and set the volume to the mark, and make a stock solution containing 1 mg of impurity D in each 1 ml.

[0046] 4) Instrument: high performance liquid chromatography (CAD detector);

[0047] Chrom...

Embodiment 2

[0058] Example 2: Specificity

[0059] Prepare reference substance solution and need testing solution and impurity D stock solution according to embodiment 1;

[0060] Preparation of system suitability solution: prepare a system suitability solution containing 15mg of the test product and 75μg each of impurity A, impurity B, and impurity D per 1ml;

[0061] Take the test solution to prepare various destruction solutions:

[0062] Light damage solution: take the stock solution of the test product into a transparent EP tube and place it under 254nm ultraviolet light for 24 hours;

[0063] Oxidative destruction solution: take the test product stock solution and add 3% H 2 o 2 , placed at room temperature for 4 hours;

[0064] High-temperature destruction solution: take 1ml of the stock solution of the test product, put it in a transparent EP tube, place it in a water bath at 60°C for 3 hours, and then cool it down;

[0065] Acid destruction solution: take the test product stoc...

Embodiment 3

[0074] Embodiment 3: detection limit and quantitative limit

[0075] 1) Impurity D stock solution: Accurately weigh 10 mg of the impurity D reference substance, put it in a 10ml volumetric flask, add diluent to dissolve and set the volume to the mark, and make a stock solution containing 1mg of impurity D in each 1ml.

[0076] According to the chromatogram of each related substance limit solution in Example 2, the signal-to-noise ratio of each component can be preliminarily obtained, and the stock solution is gradually diluted to find out the concentration corresponding to the signal-to-noise ratio of 2 to 4, which is defined as the detection limit concentration; The concentration corresponding to the signal-to-noise ratio of 8 to 12 was defined as the concentration of quantitation limit. The results are shown in Table 4 and Table 5 below.

[0077] Table 4. Results of detection limit of impurity D reference substance

[0078]

[0079] Table 5, results of quantitation limi...

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Abstract

The invention discloses a method for analyzing related impurities of an isoxazoline veterinary drug intermediate ammonium salt, the intermediate is 2-amino-N-(2, 2, 2-trifluoroethyl) acetamide, the related impurities are trifluoroethylamine hydrochloride and glycine, and the method comprises the following steps: dissolving the intermediate ammonium salt and a reference substance by using a diluent to obtain a sample solution and a reference substance solution; a reversed-phase high performance liquid chromatograph is used for detecting glycine, and gas chromatography is used for detecting trifluoroethylamine hydrochloride. The method provided by the invention can effectively separate impurities of 2-amino-N-(2, 2, 2-trifluoroethyl) acetamide, and has the advantages of high efficiency, simplicity, convenience, high sensitivity and good separation effect.

Description

technical field [0001] The invention belongs to the field of analysis of pharmaceutical intermediates, and in particular relates to an analysis method for impurities related to ammonium salts of isoxazoline veterinary drug intermediates. Background technique [0002] Fluralaner (Fluralaner) and Afoxolaner (Afoxolaner) are high-end long-acting antiparasitic drugs, which cause hyperexcitability of the nervous system by interfering with the gamma-aminobutyric acid (GABA)-gated chloride channel of the parasite And die. Fluralaner is the first oral chewable ectoparasiticide for fleas and ticks for up to 12 weeks. One chewable tablet or one dose of topical solution provides broad-spectrum and long-lasting protection, begins to kill fleas within 2 hours, and controls 4 species of ticks (black-legged tick, American dog tick, brown dog tick and Lone star tick ). Afoxolaner is the first oral anthelmintic in China that kills both ticks and fleas at the same time. It can take effect ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679Y02A40/70
Inventor 温军贤李冰冰冯绮晴姜桥
Owner LIVZON NEW NORTH RIVER PHARMA
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