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Rice hull-based magnetic mesoporous silica adsorption material and solid-phase extraction column prepared from same

A mesoporous silica, solid-phase extraction column technology, applied in material separation, analytical materials, solid adsorbent liquid separation, etc. Purity, high recovery rate, high detection cost, etc., to enhance the mass transfer and adsorption capacity, reduce the influence of the system, and accelerate the mass transfer process.

Pending Publication Date: 2022-01-04
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the commonly used mycotoxin detection method in the laboratory is chromatographic detection method. This method needs to be extracted and purified. The analysis method sample pretreatment is cumbersome, complicated, time-consuming and labor-intensive. The sample pretreatment steps have also undergone continuous updates and improvements; convenient and sensitive solid-phase extraction columns have been applied to the enrichment of toxins in samples to replace expensive immunoaffinity columns
[0003] But in the final analysis, immunoaffinity columns are based on the highly specific antigen-antibody binding theory, and solid-phase extraction columns are still difficult to match the sensitivity, specificity and accuracy of immunoaffinity columns, and the recovery rate is low
Most of the existing solid-phase extraction columns on the market adopt the one-column-one-sample mode, which causes serious waste, high testing costs, high technical requirements for operators, and low accuracy of results; and the traditional adsorbent used in traditional solid-phase extraction columns is only Relying on non-specific adsorption to separate different compounds, it is difficult to achieve high purity and high recovery at the same time; with the continuous pursuit of timeliness, accuracy, speed, and popularity of mycotoxin detection, this situation also urgently needs the emergence of new technologies. Continuous improvement and progress

Method used

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  • Rice hull-based magnetic mesoporous silica adsorption material and solid-phase extraction column prepared from same
  • Rice hull-based magnetic mesoporous silica adsorption material and solid-phase extraction column prepared from same
  • Rice hull-based magnetic mesoporous silica adsorption material and solid-phase extraction column prepared from same

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A rice husk-based magnetic mesoporous silica adsorption material and a solid-phase extraction column prepared therefrom. The specific preparation method includes the following steps:

[0038] (1) Preparation of rice husk-based magnetic mesoporous silica

[0039] The rice husk is washed with tap water and deionized water, dried, crushed and passed through an 80-mesh sieve, washed with water and centrifuged after boiling with 2M hydrochloric acid for 2 hours. ℃ for 6 hours to obtain solid rice husk ash; the particle size is about 80 μm.

[0040] According to the ratio of solid rice husk ash to NaOH mass ratio of 5:4, the solid rice husk ash and 0.8M NaOH aqueous solution were heated and dissolved at 100°C for 20 minutes and mixed to prepare the rice husk ash solution;

[0041] 0.2g Fe 3 o 4 Mix with 100mL of 0.02M cetyltrimethylammonium bromide solution by ultrasound for 30min, stir and heat at 80°C for 30min, add 50mL of the above rice husk ash solution dropwise, adju...

Embodiment 2

[0052] A rice husk-based magnetic mesoporous silica adsorption material and a solid-phase extraction column prepared therefrom. The specific preparation method includes the following steps:

[0053] (1) Preparation of rice husk-based magnetic mesoporous silica

[0054] The rice husk is washed with tap water and deionized water, dried, crushed and passed through an 80-mesh sieve, washed with water and centrifuged after boiling with 2M hydrochloric acid for 2 hours. ℃ for 6 hours to obtain solid rice husk ash; the particle size is 100 μm.

[0055] According to the mass ratio of solid rice husk ash to NaOH of 1:1, the solid rice husk ash and 0.7M NaOH aqueous solution were heated and dissolved at 100°C for 20 minutes and mixed to prepare the rice husk ash solution;

[0056] 0.4g Fe 3 o 4 Mix with 100mL of 0.05M cetyltrimethylammonium bromide solution by ultrasonic for 30min, stir and heat at 80°C for 30min, add 50mL of the above rice husk ash solution dropwise, adjust the pH t...

Embodiment 3

[0065] A rice husk-based magnetic mesoporous silica adsorption material and a solid-phase extraction column prepared therefrom. The specific preparation method includes the following steps:

[0066] (1) Preparation of rice husk-based magnetic mesoporous silica

[0067] The rice husk is washed with tap water and deionized water, dried, crushed and passed through an 80-mesh sieve, washed with water and centrifuged after boiling with 2M hydrochloric acid for 2 hours. ℃ for 5 hours to obtain solid rice husk ash; the particle size is 75 μm.

[0068] According to the ratio of solid rice husk ash to NaOH mass ratio of 5:4, the solid rice husk ash and 1M NaOH aqueous solution were heated and dissolved at 100°C for 20 minutes and mixed to prepare the rice husk ash solution;

[0069] 0.2g Fe 3 o 4 Mix with 100mL of 0.04M cetyltrimethylammonium bromide solution by ultrasound for 30min, stir and heat at 80°C for 30min, add 50mL of the above rice husk ash solution dropwise, adjust the p...

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Abstract

The invention discloses a rice hull-based magnetic mesoporous silica adsorption material and a solid-phase extraction column prepared from the same. A preparation method of the adsorption material comprises the following steps of: (1) preparing a rice hull ash solution; (2) preparing magnetic mesoporous silica; (3) dissolving a virtual template into a reaction solvent dimethyl sulfoxide, then sequentially adding a functional monomer, a cross-linking agent and the magnetic mesoporous silica prepared in the step (2), and performing ultrasonic mixing to obtain a prepolymerization solution; and (4) preparing a molecularly imprinted material, namely the adsorption material. According to the invention, an environment-friendly material prepared from a rice husk base is used as a carrier, a molecularly imprinted polymer is prepared by using a covalent and non-covalent hybridization method, a bifunctional monomer and a double-template means, the molecularly imprinted polymer is used for filling to obtain a solid-phase extraction column for specifically adsorbing fungaltoxin, and the effects of specificity, rapidness and accuracy can be achieved in a fungaltoxin detection process.

Description

technical field [0001] The invention relates to the technical field of food detection, in particular to a rice husk-based magnetic mesoporous silica adsorption material and a solid-phase extraction column prepared therefrom. Background technique [0002] Mycotoxins are toxic secondary metabolites produced by fungi during their growth and reproduction. They can easily contaminate food crops and are not easily damaged by cooking, heating or processing. They have reproductive toxicity, nephrotoxicity, neurotoxicity, immunotoxicity, teratogenic toxicity and carcinogenicity. Sex, etc., causing serious damage to humans and animals. The comprehensive prevention and accurate monitoring of mycotoxin contamination is a necessary means to effectively ensure food security and maintain citizens' health, and the detection of mycotoxin content is an important part of it. At present, the detection technology of mycotoxins has developed rapidly, and has developed from traditional thin-layer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/28B01J20/10B01J20/06B01J20/02B01J20/30B01J20/281B01J20/283B01D15/10G01N30/06
CPCB01J20/28009B01J20/28083B01J20/10B01J20/02B01J20/06B01J20/3085B01J20/30B01J20/281B01J20/283B01D15/10G01N30/06
Inventor 罗小虎刘为芝王韧李亚男翟羽恒程淼淼何巧艳
Owner JIANGNAN UNIV
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