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Molecularly imprinted polymers (MIPs) for inspecting melamine and preparation method thereof

A technology of molecular imprinting and melamine, which is applied in the field of material chemistry, can solve the problems of template leakage and difficulty in obtaining molecularly imprinted polymers, and achieve the effect of improving specificity, high affinity and selectivity, and increasing specific recognition ability

Inactive Publication Date: 2009-10-21
SOUTH CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Melamine is a water-soluble polar substance. Using melamine itself as a template to prepare molecularly imprinted polymers for pretreatment of melamine, on the one hand, there is no suitable porogen, and on the other hand, there is a problem of template leakage, which has high specificity for melamine. Permanent molecularly imprinted polymers are difficult to obtain

Method used

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  • Molecularly imprinted polymers (MIPs) for inspecting melamine and preparation method thereof
  • Molecularly imprinted polymers (MIPs) for inspecting melamine and preparation method thereof
  • Molecularly imprinted polymers (MIPs) for inspecting melamine and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1 Molecularly imprinted polymer for detecting melamine

[0050] The synthesis and preparation steps of the molecularly imprinted polymer in this example are as follows:

[0051] (1) Preparation of prepolymer

[0052] Weigh 0.166g (1mmol) of cyromazine simulation template in a test tube, add 5.0mL methanol / water (10 / 1, V / V), after ultrasonic dissolution, add functional monomer methacrylic acid 0.690mL (8mmol), Sonicate for 5 minutes, and stand overnight at 4°C to form a prepolymer;

[0053] (2) Photopolymerization

[0054] Add 5.00mL (25mmol) of ethylene glycol dimethacrylate and 30mg of azobisisobutyronitrile to the above prepolymer, sonicate for 5min, blow nitrogen for 5min, seal, and polymerize at 4°C under 365nm ultraviolet light for 24h;

[0055] (3) Polymerization curing

[0056] The above photopolymerization product was transferred into a water bath at 60° C. and then polymerized for 12 hours to obtain a block polymer, which is the molecularly imprinte...

Embodiment 2

[0059] Example 2 Determination of the performance of molecularly imprinted polymers for detecting melamine

[0060] In this example, the molecularly imprinted polymer (with a particle size of 38.5 μm to 75 μm) prepared in Example 1 was selected to be filled in a 3 mL solid-phase extraction empty cartridge (200 mg / column), and activated with 3 mL of methanol and 3 mL of water in sequence.

[0061] The samples in this example are melamine aqueous solutions with serial concentrations of 0.5, 2, 10 and 50 μg / mL. Take 2-5 mL of the sample and load it, wash with 3 mL of water and 3 mL of methanol, press dry, and elute with 5 mL of 5% ammoniated methanol. Blow dry carefully with nitrogen, dissolve with mobile phase, centrifuge at high speed, and detect with HPLC-UV. The detection results are as follows: figure 1 As shown, the AU on the ordinate in the figure is the absorbance unit, m=millimeters, and the abscissa represents the time in minutes (min).

[0062] figure 1 Provide two c...

Embodiment 3

[0063] Example 3 Determination of the performance of molecularly imprinted polymers used to detect melamine as a template and cyromazine as a template

[0064] In this example, the molecularly imprinted polymer (with a particle size of 38.5 μm to 75 μm) prepared in Example 1 was selected to be filled in a 3 mL solid-phase extraction empty cartridge (200 mg / column), and activated with 3 mL of methanol and 3 mL of water in sequence.

[0065] The samples in this example are 0.5 and 10 μg / mL melamine aqueous solutions. Take 2 mL of the sample for loading, wash with 3 mL of water and 3 mL of methanol, press dry, and elute with 5 mL of 5% ammoniated methanol. Blow dry carefully with nitrogen, dissolve with mobile phase, centrifuge at high speed, and detect with HPLC-UV. The detection results are as follows: figure 2 shown.

[0066] figure 2 Provide two chromatographic curves in, wherein 1 is the chromatographic curve that the MIPs solid-phase extraction small column of template ...

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Abstract

The invention discloses molecularly imprinted polymers (MIPs) for detecting melamine and a preparation method thereof. The MIPs are prepared by the steps as follows: cyromazine is used as a virtual moulding board and is polymerized with a functional monomer, a cross linker agent, a pore-foaming agent and an initiator at the temperature from 50 to 80 DEG C to obtain a bulk polymer; and after being processed by the operations of pulverization, screen separation, moulding board removal by acetic acid methanol and methanol, the bulk polymer is processed by vacuum drying to prepare the MIPs which have high cross reaction and outstanding selectivity to melamine. The invention selects the cyromazine as the virtual moulding board to prepare the MIPs, and avoids the problem that the melamine is hard to dissolve in a polymerization system and the problem that when the MIPs prepared by using the melamine as the moulding board is used for solid phase extraction of fill materials, moulding board leakage can lead to an inaccurate result; the invention selects the mixed system of methanol and water as the pore-foaming agent, and the prepared MIPs have high compatibility with the melamine in an aqueous solution; and used as a sample pre-processing material for analyzing the melamine, the prepared MIPs have broad application prospect.

Description

technical field [0001] The invention relates to the technical field of material chemistry, in particular to a molecularly imprinted polymer for detecting melamine and a preparation method thereof. Background technique [0002] Melamine, also known as melamine, cyanuramide, tripolyamide, protein essence, chemical name is 2,4,6-triamino-1,3,5-triazine, is an important organic chemical raw material , Widely used in the production of plastics, coatings, adhesives and food packaging materials. Because the nitrogen content of melamine is as high as 66%, it contains a higher proportion of nitrogen atoms than protein (average nitrogen content 16%), so it is used by some counterfeiters to add it to feed and food to create the illusion of higher protein content. , thus causing serious food safety incidents such as the 2007 American pet food contamination incident and the 2008 Chinese poisoned milk powder incident and poisoned egg incident. [0003] In response to the above situation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/285
Inventor 贺利民曾振灵郑亚秋丁焕中刘雅红沈祥广苏贻娟
Owner SOUTH CHINA AGRI UNIV
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