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Method for detecting afoxolaner intermediate by reversed-phase high performance liquid chromatography

A reversed-phase high-performance liquid phase and chromatographic detection technology, which is applied in the field of reversed-phase high-performance liquid chromatography to detect afolana intermediates, and achieves the effects of good chromatographic peak shape, good repeatability and stability

Active Publication Date: 2021-12-31
LIVZON NEW NORTH RIVER PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] At present, there is no relevant report on the quality evaluation method of 4-oximemethyl-1-naphthoic acid. In order to ensure the quality of the afurana raw material synthesized as an intermediate and to ensure the safety of the drug, it is necessary to invent an efficient detection method. Method to determine the purity of the afurana intermediate

Method used

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  • Method for detecting afoxolaner intermediate by reversed-phase high performance liquid chromatography
  • Method for detecting afoxolaner intermediate by reversed-phase high performance liquid chromatography
  • Method for detecting afoxolaner intermediate by reversed-phase high performance liquid chromatography

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Experimental program
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Effect test

Embodiment 1

[0035] S1: Preparation of the test solution: Weigh an appropriate amount of the test product of the intermediate of Afurana in a 20mL volumetric flask, dissolve it with a solvent and dilute to the mark, mix well, and prepare a sample containing 0.5mg of the intermediate per 1mL solution;

[0036] S2: Determination of reverse phase high performance liquid chromatography: YMC-Triart C18 chromatographic column: 4.6mm × 250mm, 5 μ m; mobile phase is acetonitrile: 0.01v / v% trifluoroacetic acid aqueous solution = (40 ~ 65): (60 ~ 35) (v / v) Gradient elution, gradient elution time and volume ratio of mobile phase acetonitrile: 0min~9min, 40%~55% operation; 9min~15min, 55%~65% operation; 15.1min~25min , 40% run. Flow rate: 1.0mL / min; Column temperature: 30°C; Detection wavelength of UV detector: 245nm; Sample volume: 10μL; figure 1 shown.

[0037] Depend on figure 1 It can be seen that the retention time of the main component in the test solution is 6.35min, the number of theoretic...

Embodiment 2

[0038] Embodiment 2: The influence of the volume fraction of trifluoroacetic acid aqueous solution on the detection of afolana intermediate by reversed-phase high-performance liquid chromatography

[0039] S1: according to embodiment 1 preparation need testing solution;

[0040] S2: In the chromatographic conditions of Example 1, keep acetonitrile unchanged, change the volume fraction of trifluoroacetic acid in the mobile phase B, and take the test sample for inspection. The results are shown in Table 1. Wherein, the degree of separation refers to the degree of separation between the afuraner intermediate and adjacent impurities.

[0041] Table 1

[0042] mobile phase B keep time Number of plates Tailing factor Separation Number of impurities 0.01v / v% trifluoroacetic acid in water 6.56min 21148 0.98 4.37 10 0.02v / v% trifluoroacetic acid aqueous solution 6.59min 26453 1.09 4.22 10 0.03v / v% trifluoroacetic acid aqueous solution 6...

Embodiment 3

[0044] Embodiment 3: the impact of column temperature on the detection of Afolana intermediates by reversed-phase high-performance liquid chromatography

[0045] S1: according to embodiment 1 preparation need testing solution;

[0046] S2: On the basis of the chromatographic conditions in Example 1, the column temperature was changed, and the sample solution of the test sample was taken for inspection. The results are shown in Table 2.

[0047] Table 2

[0048] Column temperature keep time Number of plates Tailing factor Separation Number of impurities 20℃ 7.09min 24252 0.97 4.42 8 25℃ 6.82min 27760 0.92 4.48 10 30℃ 6.56min 21148 0.98 4.37 10 35℃ 6.31min 26000 0.95 4.45 10 40℃ 6.09min 25114 0.96 4.28 10

[0049] The test results showed that if the temperature was too low, the detection of the intermediate of Afolana was affected, and the impurities could not be fully detected. When the column temperatu...

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Abstract

The invention discloses a method for detecting an afoxolaner intermediate by reversed-phase high performance liquid chromatography. The arfanaga intermediate is 4-oximidomethyl-1-naphthoic acid. The method comprises the following steps: 1) preparing a test solution; 2) detecting the test solution by using reversed-phase high performance liquid chromatography; and 3) determining the content of the afoxolaner intermediate in the test solution by using an area normalization method. The complete separation of the chromatographic peaks in the test solution can be achieved through a simple mobile phase component, the detection result precision is high, the repeatability is good and stable, and the purity of the afoxolaner intermediate can be accurately controlled.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical analytical chemistry, and in particular relates to a method for detecting an afolana intermediate by reversed-phase high-performance liquid chromatography. Background technique [0002] The isoxazoline insecticide Aflana, as a new generation of oral anthelmintics for dogs, is famous for its rapid drug effect, convenient oral administration and delicious taste. Experiments have proved that because the drug kills fleas quickly and can continuously inhibit the laying of eggs by fleas; it can kill many types of cicadas, and the drug effect usually lasts for more than 4 weeks, and is widely used in environmental management. [0003] The chemical name of the intermediate of Afraner is 4-oxime methyl-1-naphthoic acid, which is a key intermediate of Aflaner API, and its structural formula is as follows: [0004] [0005] At present, there is no relevant report on the quality evaluation method o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027Y02P20/55
Inventor 谢倩玲米俊儒姜桥温军贤陈果
Owner LIVZON NEW NORTH RIVER PHARMA
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