Preparation method of halofuginone molecularly-imprinted solid-phase extraction small column and application

A solid-phase extraction column and molecular imprinting technology, applied in the field of analytical chemistry, can solve the problems of cumbersome detection methods and sample pretreatment, complicated preparation process, and low precision, and achieve simple and easy preparation process, large adsorption capacity, The effect of high precision

Inactive Publication Date: 2012-07-04
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the instrumental methods in the detection methods of fushenone residues are mainly high-performance liquid chromatography and high-performance liquid chromatography-mass spectrometry. Although their detection capabilities are strong, the detection methods and sample pretreatment are cumbersome, time-con

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (one). Preparation of Molecularly Imprinted Polymer of Hemosanone

[0021] Weigh 6g of polyvinyl alcohol 400 into 150mL of double distilled water, dissolve in hot water at 90°C-95°C, cool to room temperature, and then transfer to a 250mL three-necked flask. Accurately weigh 0.5mmol of the template molecule (hemosanone) and dissolve it in 150mL of acetonitrile, then add 2mmol of the functional monomer methacrylic acid to make it fully dissolved, then ultrasonicate for 5min, and then place it in a refrigerator at 4°C for 24h to form a stable complex That is, the pre-polymerization is completed. Then add 10 mmol of trimethylolpropane trimethacrylate as a cross-linking agent, 0.4 mmol of benzoyl peroxide as an initiator, and 0.4 mmol of N,N-dimethylaniline, and slowly drop after ultrasonic treatment for 5 minutes (to remove oxygen). The above-mentioned three-neck flask was stirred at 400 rpm and heated at a temperature of 20° C., and a milky white microsuspension emulsion...

Embodiment 2

[0038] (one). Preparation of Molecularly Imprinted Polymer of Hemosanone

[0039] The basic process of preparation is the same as in Example 1, the concentration of polyvinyl alcohol 400 used is 6%, the amount of porogen used is 200mL, the functional monomer is 3mmol of acrylamide, and the crosslinking agent trimethylolpropane trimethacrylate is 15mmol. The initiators benzoyl peroxide and N,N-dimethylaniline are 0.6 mmol each, the polymerization initiation temperature is 25° C., the polymerization time is 12 hours, and the Soxhlet extraction elution time is 15 hours.

[0040] (two). Characterization of Molecularly Imprinted Polymers of Hemosanone

[0041] The characterization method is the same as in Example 1, and the results show that there are two types of adsorption sites in the template molecularly imprinted polymer, one is a highly selective binding site, and the other is a low-selective binding site (its K D1 =2.6×10 -2 mu mol / L, Q max1 =135.4 mu mol / g; K D2 =0....

Embodiment 3

[0049] (one). Preparation of Molecularly Imprinted Polymer of Hemosanone

[0050] The basic process of preparation is the same as in Example 1, the concentration of polyvinyl alcohol 400 used is 5%, the amount of porogen used is 100mL, the functional monomer 4-vinylpyridine is 1.5mmol, and the crosslinking agent trimethylolpropane trimethacrylic acid 7.5 mmol of ester, 0.3 mmol of benzoyl peroxide and 0.3 mmol of N, N-dimethylaniline as initiators, polymerization initiation temperature of 18°C, polymerization time of 24 hours, and Soxhlet extraction and elution time of 12 hours.

[0051] (two). Characterization of Molecularly Imprinted Polymers of Hemosanone

[0052] The characterization method is the same as in Example 1. The results show that there are two types of adsorption sites in the template molecularly imprinted polymer, one is the binding site with high binding energy and high selectivity, and the other is the binding site with low binding energy and low selectivit...

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Abstract

The invention provides a preparation method of a halofuginone molecularly-imprinted solid-phase extraction small column and an application and relates to the field of analytical chemistry. The preparation method comprises the following steps of: taking halofuginone as a template molecule, dissolving the template molecule into a porogen and adding a functional monomer at a low temperature for prepolymerization; then, mixing according to the molar ratio of the template molecule: the functional monomer: a cross-linking agent of 1:3-6:15-30, and preparing molecularly-imprinted polymer micro-spheres in a manner of initiated polymerization at a low temperate by adopting a suspension polymerization method and filling the rinsed, sieved, eluted and dried micro-spheres in an empty column tube of the solid-phase extraction column by adopting a wet process; and later, using the micro-spheres rinsed by acetone and methanol in sequence into selective adsorption, enrichment and purification of the halofuginone remained in animal derived foods. Compared with the existing solid-phase extraction column, the halofuginone molecularly-imprinted solid-phase extraction column prepared by the invention has the characteristics of strong specificity, convenience and simplicity in preparation, good recognition performance, low cost, easiness for realization of required instruments and reaction conditions and the like.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for preparing a hemosanone molecularly imprinted solid-phase extraction column and the purification and enrichment of samples during residue analysis in animal foods. Background technique [0002] Changshanone is a derivative of Changshanjing extracted from Changshan, a traditional Chinese medicine. It is a broad-spectrum antiparasitic drug. Effective, it has obvious inhibitory effect on sporozoites, first and second generation schizonts of coccidia; it is also effective on most Gram-positive bacteria, and has no cross-resistance. Changshanone hydrobromide is widely used as a feed additive to control poultry coccidiosis. In my country, hemosanone hydrobromide is allowed to be added to the feed at a concentration of 3 mg / kg, and the drug withdrawal period is 4 days. In order to avoid the residues of fushenone, many countries have established their residue detection m...

Claims

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Application Information

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IPC IPC(8): G01N30/08
Inventor 李兆周徐航李文荣李道敏侯玉泽张敏李志康刘世磊
Owner HENAN UNIV OF SCI & TECH
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