Flusilazole hapten, antigen, antibody, detection device and detection method thereof

A flusilazole and hapten technology, which is applied in the field of antigen, antibody, detection device, and flusilazole hapten, can solve the problems of complex detection process, high cost, and failure to meet supervision and law enforcement, and achieve good specificity and easy operation , the effect of high sensitivity

Active Publication Date: 2022-06-24
广东江门中医药职业学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The detection methods for flusilazole mainly include liquid chromatography and liquid chromatography-tandem mass spectrometry, but the detection process is more complicated, and the solid phase extraction column needs to be purified, the cost is high, and the purpose of rapid detection cannot be achieved. Rapid on-site testing cannot meet the needs of regulatory authorities and testing agencies for on-site supervision and law enforcement

Method used

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  • Flusilazole hapten, antigen, antibody, detection device and detection method thereof
  • Flusilazole hapten, antigen, antibody, detection device and detection method thereof
  • Flusilazole hapten, antigen, antibody, detection device and detection method thereof

Examples

Experimental program
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Embodiment 1

[0023] In this example, the 1.0Msolution in THF specification of 4-fluorophenylmagnesium bromide supplied by Sinopharm Chemical Reagent Co., Ltd. was selected for p-fluorophenylmagnesium bromide, and the analytical purity of cuprous cyanide was selected from Sinopharm Chemical Reagent Co., Ltd. Cuprous cyanide, chloromethyl methyl dichlorosilane select 95% (chloromethyl) methyl dichlorosilane supplied by Sinopharm Chemical Reagent Co., Ltd., and hydrochloric acid select 36%-38% supplied by Sinopharm Chemical Reagent Co., Ltd. Hydrochloric acid, ethyl acetate select analytically pure ethyl acetate supplied by Sinopharm Group Chemical Reagent Co., Ltd., anhydrous sodium sulfate select 99% anhydrous sodium sulfate supplied by Sinopharm Group Chemical Reagent Co., Ltd., 1,2,4-triazole- 97% methyl 1,2,4-triazole-3-carboxylate supplied by Sinopharm Chemical Reagent Co., Ltd., N,N-dimethylformamide selected from Sinopharm Chemical Reagent Co., Ltd. The analytically pure N,N-dimethylf...

Embodiment 2

[0025] Example 2 Synthesis of flusilazole hapten for immunization

[0026] The preparation method of flusilazole hapten for immunization comprises the following steps:

[0027] S1. Take a 100ml single-neck bottle, measure 17ml of p-fluorophenylmagnesium bromide, add 9mg of cuprous cyanide, stir for 5min in an ice-water bath, add 3.9ml of chloromethylmethyldichlorosilane dropwise, and then transfer to 30°C oil Continue the reaction under the bath for 1h, then in an ice-water bath for 10min, dropwise add 5ml of 1M hydrochloric acid, stir for 0.5h, keep the ice-water bath, add an appropriate amount of distilled water and ethyl acetate, stir well, separate the liquid, dry with anhydrous sodium sulfate, concentrate, mix The first intermediate was obtained by passing a column with a filler of 200 mesh silica gel powder;

[0028] S2. Take another 100ml single-neck bottle, put all the first intermediates in a total of 2.4g, take by weighing 1.19g 1,2,4-triazole-3-carboxylate methyl e...

Embodiment 3

[0029] Example 3 Coating with flusilazole hapten synthesis

[0030] The preparation method of flusilazole hapten for coating comprises the following steps:

[0031] A1. Take a 100ml single-neck bottle, weigh 1g of flusilazole technical drug, 0.82g of sublimation sulfur, add 20ml of DMF, react in an oil bath at 156°C overnight, concentrate the reaction solution, dilute with water, extract with ethyl acetate, and dry with anhydrous sodium sulfate, Concentrate to obtain the second intermediate;

[0032] A2. Take another 100ml single-neck bottle, load all the second intermediates, weigh 1.5eq potassium carbonate, 1.2eq t-butyl 4-bromobutyrate, add 15ml DMF, react in an oil bath at 80°C for 3h, cool the reaction solution and concentrate , diluted with water, extracted with ethyl acetate, directly mixed with samples and purified by a column filled with 200-mesh silica gel powder to obtain the third intermediate. In this step, 1eq is calculated as the original drug of flusilazole; ...

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Abstract

The invention discloses flusilazole hapten, antigen, antibody, detection device and detection method thereof, and relates to flusilazole hapten for immunization, flusilazole hapten for coating, flusilazole antigen, flusilazole antibody and fluorine A silazole colloidal gold chromatography detection device and a method for detecting flusilazole residues. The flusilazole colloidal gold chromatography detection device of the present invention can quickly detect flusilazole residues in fruits, vegetables and grains, and does not need to purify the solid-phase extraction column during application to achieve the purpose of rapid detection. The detection method is dedicated to the detection of flusilazole residues, which has the advantages of good specificity, high sensitivity, easy operation, and rapid on-site detection, etc., and can better meet the needs of on-site supervision and law enforcement by regulatory authorities and testing institutions The department quickly detects whether flusilazole residues in fruits, vegetables, and grains exceed the standard to provide technical support.

Description

technical field [0001] The invention relates to the field of pesticide safety detection, in particular to a flusilazole hapten, an antigen, an antibody, a detection device and a detection method thereof. Background technique [0002] The chemical name of Flusilazole is bis(4-fluorophenyl)methyl (1H-1,2,4-triazol-1-ylmethyl)silane, which is a new type of triazole fungicide containing silicon. Mainly as a sterol demethylation inhibitor, it can disrupt the formation of cell membranes and cause bacterial death. Flusilazole has a good control effect on diseases caused by Ascomycetes, Basidiomycetes and Deuteromycetes, such as Botrytis cinerea, scab, and stoloniferous leaf spot. [0003] The maximum residue limit standard for flusilazole pesticides in fruits formulated in my country is 0.2 mg / kg, but there is no standard for the detection method of flusilazole at present. The detection methods for flusilazole mainly include liquid chromatography and liquid chromatography-tandem ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08C07K14/765C07K14/77C07K14/795C07K14/79C07K16/44C07K16/06G01N33/558G01N33/58G01N33/53
Inventor 李拥军熊文明周昱良温宝莹莫婷筠余廉柱李斌陈文浩
Owner 广东江门中医药职业学院
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