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Preparation method and application of amitraz molecular imprinting monolithic column

A technology of molecular imprinting and amitraz, which is applied in the field of analytical chemistry, can solve the problems of complex antibody preparation process, poor tolerance to environmental conditions, cumbersome sample processing process, etc., and achieve simple preparation process, strong tolerance, Inexpensive effect

Active Publication Date: 2014-12-10
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Gas chromatography needs to derivatize amitraz, and the sample processing process is cumbersome; gas chromatography-mass spectrometry requires high equipment and is expensive, and the general laboratory cannot bear it; while liquid chromatography pretreatment is relatively simple, but It is necessary to purchase a specific chromatographic column, and the price is relatively high. Although the chromatographic column of biological antibodies can specifically recognize the target molecule, the preparation process of the antibody is complicated, the cost is high, the preparation cycle is long, and the tolerance to environmental conditions poor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0024] A method for preparing an amitraz molecularly imprinted monolithic column, comprising the following steps:

[0025] (1) Dissolve the template molecules in the porogen, add functional monomers, mix them with ultrasonic treatment for 5 minutes, put them in a refrigerator at 4°C for prepolymerization for 24 hours, and obtain a prepolymerization system;

[0026] The template molecule is amitraz, the porogen is a mixed solvent composed of acetonitrile and dodecanol with a volume ratio of 1: 2-5, and the functional monomer is methacrylic acid, trifluoro A combination of any one or both of methacrylic acid, acrylamide, 4-vinylpyridine and methacrylate; the molar ratio of the template molecule to the functional monomer is 1: 3-8, and the template molecule is in The molar concentration in the porogen is 30mmol / L-70mmol / L;

[0027] (2) Add cross-linking agent and initiator to the pre-polymerization system prepared in step (1), ultrasonicate for 5 minutes, mix thoroughly, and the...

Embodiment 1

[0035] (1) Preparation of Amitraz Molecularly Imprinted Monolithic Column

[0036]Weigh 0.3 mmol of the template molecule (Amitraz) and dissolve it in 6 mL of porogen mixed solution of acetonitrile and dodecanol (1 : 2, V / V), add 0.9 mmol of functional monomer methacrylic acid, and store in a refrigerator at 4 °C Leave it for 24 hours to allow the monomers to fully interact with the template molecules to complete the pre-polymerization process and obtain a pre-polymerization system. Then add cross-linking agent trimethylolpropane trimethacrylate 4.5mmol and initiator benzoyl peroxide and N, N-dimethyl aniline each 0.18mmol, pass into nitrogen gas 30min after ultrasonic 5min, mix solution Inject into an empty chromatographic column tube with the bottom capped, then seal the other end of the column. Place the formed mixed solution at 30°C to initiate polymerization for 24 hours. After the polymerization is completed, open the seals at both ends of the column, cover the sieve pl...

Embodiment 2

[0051] (1) Preparation and Characterization of Amitraz Molecularly Imprinted Monolithic Column

[0052] The basic process is the same as in Example 1, the porogen is a mixed solution of 5mL acetonitrile and dodecanol (1:3, V / V), the pre-polymerization time is 48h, the functional monomer trifluoromethacrylic acid is 2.4mmol, cross-linked Agent trimethylolpropane trimethacrylate 12mmol, initiator benzoyl peroxide and N,N-dimethylaniline 0.24mmol each, polymerization temperature is 35°C, time is 20h, template molecule eluent is methanol -Acetic acid mixture (8:2, V / V), the capacity factor and imprinting factor of the obtained monolithic column are shown in Table 3, the obtained standard curve equation is: Y=94.23X+0.35, and the correlation coefficient r is 0.99996.

[0053] Table 3 Capacity factor and imprinting factor of molecularly imprinted monolithic columns

[0054] k MIP k NIP IF Amitraz 2.37 0.95 2.49

[0055] (2) Detection of actual ...

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PUM

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Abstract

The invention discloses a preparation method and application of an amitraz molecular imprinting monolithic column. The preparation method comprises the following steps: by taking amitraz as a template molecule, dissolving the template molecule into a mixed solution of acetonitrile and dodecyl alcohol, adding a functional monomer, pre-polymerizing at a low temperature, further adding a cross-linking agent and an initiator, introducing nitrogen, filling into a chromatographic column hollow tube of which the lower end is already sealed, sealing the upper end of the chromatographic column hollow tube, and initializing polymerization, thereby obtaining the molecular imprinting monolithic column. After the functional monomer, a pore-foaming agent and the template molecule which are not polymerized are washed off from the column by using a mixed solution of methanol and acetic acid, the molecular imprinting monolithic column which has a good adsorption effect and an enrichment effect on amitraz is obtained. Compared with a conventional body polymerization method, the preparation method has the characteristics that the preparation method is simple and convenient, the aftertreatment is simple, the recognition property is good, the cost is low, required instruments and reaction conditions are easy to achieve, and the like. The molecular imprinting monolithic column prepared by using the preparation method is capable of separating and detecting residual amitraz in foods.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for preparing an amitraz molecularly imprinted monolithic column and its application in the analysis of amitraz residues in food. Background technique [0002] Amitraz is a broad-spectrum acaricide with moderate toxicity. It mainly inhibits the activity of monoamine oxidase. It has contact killing, antifeedant and repellent effects, and also has certain systemic and fumigation effects. Acaricide-resistant mites are also effective, and the number of harmful mites can be controlled for a long time after treatment. Amitraz is widely used in the prevention and control of harmful mites on fruit trees, vegetables, tea, cotton, soybeans, sugar beets and other crops. systemic and fumigation effects. It also has good medicinal effect on Homoptera pests, and can also be used to control pests such as aphids, cotton bollworms, and red flies. It also has a good control effect o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/56
Inventor 李道敏李兆周高红丽曹力李智丽陈秀金侯玉泽李松彪张腊梅王慧娟王芳俞嘉伟唐淑阁
Owner HENAN UNIV OF SCI & TECH
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