Dual-template molecule amino functionalized metal organic framework imprinted polymer as well as synthesis method and application thereof

A metal-organic framework and imprinted polymer technology, which is applied in the field of analytical chemistry, can solve the problems of not being able to adsorb multiple types of mycotoxins at the same time, and achieve the effects of rapid adsorption equilibrium, cost reduction, and stable and reliable methods

Active Publication Date: 2020-07-31
HENAN VOCATIONAL COLLEGE OF WATER CONSERVANCY ANDENVIRONMENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are also related reports on surface molecularly imprinted polymers, but the selectivity for mycotoxins is relatively strong and relat

Method used

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  • Dual-template molecule amino functionalized metal organic framework imprinted polymer as well as synthesis method and application thereof
  • Dual-template molecule amino functionalized metal organic framework imprinted polymer as well as synthesis method and application thereof
  • Dual-template molecule amino functionalized metal organic framework imprinted polymer as well as synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The preparation of embodiment 1CPT-MIPs

[0036] 1.1 Experimental reagents

[0037] Aminoterephthalic acid (NH 2 -H 2 BDC) (98%, McLean); aflatoxins (AFB1, AFB2, AFG1, AFG2) (98%, Aladdin); warfarin (98%, Adamas Reagent Co. Ltd); 7-acetoxy - 4-Methylcoumarin (98%, Adamas); glycidyl methacrylate (GMA) (AR, McLean).

[0038] 1.2 Preparation of CPT-MIPs

[0039] (1) MIL-101(Cr)-NH 2 Synthesis

[0040] Add 3.2g (10mmol) Cr(NO 3 )9H 2 O, 1.5g (8.28mmol) NH 2 -H 2 BDC and 60mL deionized water were stirred at room temperature for 1 hour, and then the jacket of the stainless steel reactor was tightened. Using the hydrothermal synthesis method, the oven is controlled by a program to control the temperature, within 30 minutes, the temperature is raised from 50°C to 150°C, and kept at 150°C for 12h. After cooling to room temperature, the product was separated by centrifugation, and the unreacted NH 2 -H 2 BDC. The product was dried overnight in a vacuum oven at 100 °...

Embodiment 2

[0053] Example 2 CPT-MIPs adsorption performance experiment

[0054] 2.1 Preparation of double substituted template standard solution

[0055] Warfarin and 7-acetoxy-4-methylcoumarin concentrations were 0.5, 1.0, 2.0, 3.0, 5.0, 10, 15, 20, 30, 40 and 50 μg mL -1 standard solution, using methanol: water (1:9, V / V) preparation, ready to use.

[0056] 2.2 Static adsorption experiment

[0057]Weigh 10 mg of the eluted and dried CPT-MIPs and mix them with 5 mL of the above-mentioned double substitution template standard solutions of different concentrations in a 10 mL centrifuge tube, shake at 90 rpm for 1 h with an oscillator, and filter the supernatant with a filter membrane. Determine the concentration of the double template in the solution, and calculate the adsorption amount of CPT-MIPs to warfarin sodium and 7-acetoxy-4-methylcoumarin according to formula 3.1:

[0058] Q=(C 0 -C t )*V / m (3.1)

[0059] in,

[0060] Q is the adsorption capacity of CPT-MIPs, (mg g -1 ); ...

Embodiment 3

[0087] Application in embodiment 3 actual samples

[0088] 3.1 Actual sample pretreatment

[0089] Rice samples were purchased from local supermarkets (Henan, Zhengzhou), crushed, and passed through a 40-mesh sieve. Weigh 40g of the above sample, 4gNaCl and 100mL extract (acetonitrile:water=9:1) into a 250mL Erlenmeyer flask and shake for 1h. After filtering with glass fiber filter paper, dilute 20 mL with distilled water 4 times, filter the mixed solution until clear, collect and set aside.

[0090] 3.2 Preparation of CPT-MIPs solid phase extraction column

[0091] Weigh 200 mg of CPT-MIPs after elution and drying, transfer to the SPE small column with the lower sieve plate, add 5 mL of methanol dropwise to wet it, use a capillary glass tube to stir out the air bubbles in the adsorbent, place the upper sieve Plate and ensure that the adsorbent in the column does not leak, ready for use.

[0092] 3.3 Optimization of SPE process of CPT-MIPs column

[0093] (1) Selection ex...

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Abstract

The invention belongs to the field of analytical chemistry, and discloses a dual-template molecule amino functionalized metal organic framework imprinted polymer. MIL-101(Cr)-NH2 is adopted as a carrier, double bonds of a functional monomer that is glycidyl methacrylate are modified to the carrier, then a precipitation polymerization reaction is carried out under the initiation of an initiator through the cross-linking action of a cross-linking agent, and the surface molecularly imprinted polymer is synthesized on the periphery of the carrier in a chemical bond grafting mode. By combining thesynthesized CPT-MIPs with an SPE technology, a solid-phase extraction small column is self-made and is applied to separation and enrichment pretreatment of zearalenone and aflatoxin in grains. Practical application shows that the disclosed polymer is high in sensitivity, high in precision, low in detection limit and quantification limit, good in recovery effect and stable in recovery rate. The method is stable and reliable, and can be used for quantitative analysis of actual samples. The CPT-MIPs column can be regenerated through elution and can be repeatedly used.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and relates to a metal-organic framework imprinted polymer, in particular to a double-template molecule amino functionalized metal-organic framework imprinted polymer and its synthesis method and application. Background technique [0002] Mycotoxins exist in a wide range and may exist in corn, wheat, soybeans, rice, oats and other food crops. During the planting, transportation, storage and processing stages of food, under certain temperature and humidity conditions, food crops will produce mycotoxins. There are many kinds of mycotoxins, including zearalenone toxin (Zearalenone, ZEN), aflatoxins (Aflatoxins, AFs), ochratoxin, deoxynivalenol and so on. It has strong thermal stability, and it is difficult to be degraded or destroyed in the general cooking process (such as frying, frying, steaming, boiling), so these toxins enter through direct or indirect ways after being processed into food or...

Claims

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Application Information

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IPC IPC(8): C08F290/06C08F222/14C08F2/00C08J9/26C08G83/00B01J20/26B01J20/30C08L51/08
CPCC08F290/06C08F2/00C08J9/26C08G83/008B01J20/268C08J2351/08C08J2201/0422
Inventor 宋立新何娟黄志鹏程勇王慧格游利琴
Owner HENAN VOCATIONAL COLLEGE OF WATER CONSERVANCY ANDENVIRONMENT
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