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Preparation method and application of amitraz molecularly imprinted monolithic column

A molecular imprinting and amitraz technology, applied in the field of analytical chemistry, can solve the problems of cumbersome sample processing process, poor environmental condition tolerance, complex antibody preparation process, etc. Inexpensive effect

Active Publication Date: 2015-09-30
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 preparation method of bisformamidine molecularly imprinted monolithic column includes the following steps:

[0025] (1) Dissolve the template molecule in the porogen, add the functional monomer, ultrasonically treat for 5 minutes and mix well, then put it in a refrigerator at 4°C for pre-polymerization for 24 hours to obtain a pre-polymerization system;

[0026] The template molecule is bisformamidine, the porogen is a mixed solvent composed of acetonitrile and dodecanol in a volume ratio of 1: 2-5, and the functional monomer is methacrylic acid, trifluoromethyl Any one or a combination 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 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), sonicate for 5 minutes, and after mixing thoroughly, ...

Embodiment 1

[0035] (1) Preparation of bisformamidine molecularly imprinted monolithic column

[0036] Weigh 0.3 mmol of template molecule (bisformamidine) and dissolve it in 6 mL of porogen acetonitrile and dodecanol mixed solution (1: 2, V / V), add 0.9 mmol of functional monomer methacrylic acid, and refrigerate at 4°C Leave it for 24 hours to make the monomer and template molecule fully interact, complete the pre-polymerization process, and obtain the pre-polymerization system. Then add the cross-linking agent trimethylolpropane trimethacrylate 4.5mmol and the initiator benzoyl peroxide and N,N-dimethylaniline each 0.18mmol, sonicate for 5min and bubbling with nitrogen for 30min, and the mixed solution Inject into an empty column tube with a closed bottom end, and then seal the other end of the column. Place the resulting 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 plate, t...

Embodiment 2

[0051] (1) Preparation and characterization of bisformamidine 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 prepolymerization time is 48h, the functional monomer trifluoromethacrylic acid 2.4mmol, crosslinking Trimethylolpropane trimethacrylate 12mmol, initiator benzoyl peroxide and N,N-dimethylaniline each 0.24mmol, polymerization temperature is 35℃, time is 20h, template molecule eluent is methanol -Acetic acid mixture (8: 2, V / V), the volume 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 factors and imprinting factors of molecularly imprinted monolithic columns

[0054] k MIPk NIP IF Amitraz2.370.952.49

[0055] (2) Detection of actual samples by molecularly imprinted monolithic ...

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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 Patents(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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