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Preparation method and application of dicofol hapten

A technology of dicofol and hapten, which is applied in the field of dicofol hapten preparation, can solve the problems of unsuitable basic-level laboratory batches, rapid detection of samples, difficulty in batch detection of samples, and complicated detection steps, etc. Short, accurate effects

Inactive Publication Date: 2018-04-13
吴鹏
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the methods for testing the drug are mainly instrumental methods such as mass spectrometry. The accuracy of the instrumental detection method is high, but the instrument is expensive, requires professional technicians, and the detection steps are complicated. , rapid detection of samples

Method used

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  • Preparation method and application of dicofol hapten
  • Preparation method and application of dicofol hapten
  • Preparation method and application of dicofol hapten

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1 Preparation of dicofol detection test strips (time-resolved fluorescent test strips, colloidal gold immunochromatography test strips)

[0042] 1. Preparation of dicofol hapten

[0043] Pour 20ml of DMF into a single-necked bottle, add 3.7g of dicofol, add 2.76g of potassium carbonate, stir at room temperature for 20min; add 1.2g of succinic anhydride, slowly heat up to 60°C, react for 10h, cool down, add 50ml of water, transfer to a separatory funnel, Ethyl acetate extraction. After drying, the solvent was evaporated to dryness, and purified by column chromatography to obtain 3.8 g of the target compound with a yield of 82%.

[0044] From the dicofol hapten proton nuclear magnetic resonance spectrum, it can be seen that the carboxyl peak at 12.7, the hydrogen peak on the aromatic ring at 7-8, and the methylene peak on the succinic anhydride at about 2.7 exist, indicating that the connection between dicofol and succinic anhydride has been completed. The targe...

Embodiment 2

[0067] Example 2 Detection of Dicofol Residues in Samples

[0068] 1. Sample processing

[0069] (1) Cabbage / tea pretreatment method

[0070] Homogenize the sample with a homogenizer; weigh (1.00±0.05)g of the homogenized sample into a 10mL polystyrene centrifuge tube, add 2mL of 0.1mol / L sulfuric acid, then add 5mL of methanol, and vortex for 5min with a vortexer ;, Centrifuge at 1000r / min for 5min at room temperature; Take 200μL of the supernatant, add it to 800μL of 0.01M PBS, mix well, take 50μL for analysis.

[0071] (2) Rice pretreatment method

[0072] Homogenize the sample with a homogenizer; weigh (2.00±0.05)g of the homogenized sample into a 10mL polystyrene centrifuge tube, add 4mL 10% sodium chloride and 2mL methanol respectively, and vibrate with a vortexer for 5min; room temperature Centrifuge at 4000r / min for 5min; take 100μL of the supernatant, add it to 900μL 0.01M PBS, mix well, take 50μL of it for analysis.

[0073] (3) Vegetable oil pretreatment method ...

Embodiment 3

[0085] Embodiment 3 sample detection example

[0086] 1. Time-resolved fluorescent test strips to detect samples

[0087] (1) Detection limit test

[0088] Take blank tea / cabbage / rice / vegetable oil / fish / shrimp samples, add dicofol to the final concentration of 5ng / ml, 10ng / ml, 100ng / ml, 600ng / ml, 1200ng / ml, 1800ng / ml, 2000ng / ml ml, 2200ng / ml, take a test strip for detection, and repeat the measurement three times for each sample.

[0089] When testing samples such as tea / cabbage / rice / vegetable oil / fish / shrimp with test strips, determine the detection limit range according to the results displayed on the test strips, indicating that the detection limit range of this test strip is: 10ng / ml-2000ng / ml.

[0090] (2) Sample precision and accuracy test

[0091] The recovery rate was used as the accuracy evaluation index, and the relative standard deviation (RSD%) of the test results of repeated determination of a certain concentration sample was used as the precision evaluation in...

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Abstract

The invention discloses a method for preparing a hapten for detecting dicofol and its application in time-resolved fluorescent test strips and colloidal gold immunochromatographic test strips. The time-resolved fluorescent test strip and the colloidal gold immunochromatographic test strip of the present invention have high sensitivity, high accuracy, high precision, low cost, simple operation, short detection time, suitable for use by various units, simple storage, and long shelf life It has the advantage of being long, and can quickly detect a large number of samples at the same time, and can realize high-throughput rapid detection on site. The time-resolved fluorescent test strip and the colloidal gold immunochromatographic test strip provided by the invention are suitable for determining the residual amount of dicofol in samples such as tea, cabbage, rice, vegetable oil, fish meat and shrimp meat.

Description

technical field [0001] The invention relates to a method for preparing dicofol hapten and its application, such as the application in time-resolved fluorescent test strips and colloidal gold immunochromatography test strips, belonging to the field of rapid detection technology, used for tea, cabbage, rice, vegetable oil The content detection of dicofol in samples such as meat, fish meat and shrimp meat. Background technique [0002] Dicofol is a low toxicity acaricide, insoluble in water, soluble in various organic solvents. Stable in acidic solution, easy to decompose in alkaline medium. my country mainly allows the use of citrus, apples, pears and cotton. Since its raw material comes from DDT, industrial products of dicofol may contain a certain amount of DDT, which will lead to a significant increase in the residues of agricultural products using this agent. Therefore, my country currently prohibits its use on tea trees and vegetables. In addition, the drug was also f...

Claims

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Application Information

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IPC IPC(8): G01N33/577G01N33/558G01N33/533
CPCG01N33/577G01N33/533G01N33/558
Inventor 吴鹏
Owner 吴鹏
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