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Preparation method of okadaic acid toxin molecularly imprinted-quantum dot polymer and application

A quantum dot polymer, soft sponge acid technology, applied in the fields of material science and analytical chemistry, can solve the problems of expensive equipment, high operator requirements, high pretreatment requirements, and achieve less sample requirements, less organic solvent consumption, and choice high sex effect

Active Publication Date: 2017-06-13
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although instrumental detection methods usually have high sensitivity, they have high requirements for pretreatment, expensive equipment, and high requirements for operators.

Method used

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  • Preparation method of okadaic acid toxin molecularly imprinted-quantum dot polymer and application
  • Preparation method of okadaic acid toxin molecularly imprinted-quantum dot polymer and application
  • Preparation method of okadaic acid toxin molecularly imprinted-quantum dot polymer and application

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Effect test

specific Embodiment 1

[0022] A method for preparing the molecularly imprinted-quantum dot polymer of halicic acid toxin, comprising the following steps: taking haicic acid as a template molecule, adding quantum dot fluorescent nanomaterials, and adding a cross-linking agent tetraethyl orthosilicate TEOS and a functional monomer Under existing conditions, after initiating the polymerization, the template molecules in the obtained polymer are removed by an ultrasonic-assisted extraction method, and the halicic acid toxin molecular imprint-quantum dot polymer that can specifically recognize the haicic acid toxin is obtained. Specific steps are as follows:

[0023] (1) After mixing 7.5 mL cyclohexane and 1.8 mL Triton X-100 and stirring for 15 min, add 500 μg of quantum dot fluorescent nanomaterial QDs, 50 μL of tetraethyl orthosilicate (TEOS ) and 100 μL of ammonia water, and stir for 2 h , and finally add 156 μL of halicic acid toxin solution with a concentration of 1 μg / mL, functional monomer 3-amin...

specific Embodiment 2

[0030] Utilize the molar imprinting-quantum dot polymer of the halicic acid toxin prepared in the above specific embodiment 1 to detect the content of haiconic acid, the specific steps are as follows:

[0031] (1) Weigh 0.02-0.05 mg of Molecularly Imprinted Molecularly Imprinted-Quantum Dot Polymer of Halicic Acid Toxin and dissolve it in 0.5-1.0 mL of ethanol to obtain a homogenate, and transfer the homogenate into a polypropylene Spin solid-phase extraction chamber under vacuum. In the column, the halicic acid toxin molecularly imprinted-quantum dot polymer is compressed through the upper sieve plate and the lower sieve plate to obtain the halicic acid Spin solid phase extraction column; then the halicic acid Spin solid phase extraction column is sequentially washed with ethanol 0.5-1mL, 10wt% ethanol aqueous solution 0.5-1mL rinse activation;

[0032](2) Accurately weigh 1.0 g shellfish sample, add 2.0 mL methanol, homogenate at 12000 rpm for 30 s, vortex shake for 5 min, c...

specific Embodiment 3

[0034] 1. High selectivity (specificity)

[0035] Molecular imprinting of soft spongy acid toxin-quantum dot polymer synthesized by using soft spongy acid (OA) toxin as a template molecule, select fin toxin 1 (DTX1), fin toxin 1 (DTX2), orthopolygalginic acid (AZA1) , saxitoxin (STX) as a structural analogue, the specificity of the obtained MIP-QDs was analyzed (the fluorescence quenching system is represented by the equation, F 0 / F =1+ Ksv [Q], F 0 and F represent the initial fluorescence value of MIP-QDs and the fluorescence value after adding cypermethrin, respectively, Ksv is a constant parameter in the Stem-Volmer equation and [Q] is the concentration of the quencher. ( F 0 -F ) represents the fluorescence quenching value before and after adding cypermethrin, ( F 0 -F ) / F is the imprinting efficiency of MIP-QDs. MIP-QDs and NIP-QDs Ksv The ratio of values ​​represents the imprinting factor ( IF ), used to evaluate the selectivity of MIP-QDs). Expe...

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Abstract

The invention discloses a preparation method of an okadaic acid toxin molecularly imprinted-quantum dot polymer and an application. The preparation method comprises the steps of taking okadaic acid as a template molecule and adding a quantum dot fluorescent nanomaterial; and initializing polymerization in the presence of a cross-linking agent tetraethylortho silicate and a functional monomer, and then removing the template molecule in the obtained polymer by adopting an ultrasonic-assisted extraction method to obtain the okadaic acid toxin molecularly imprinted-quantum dot polymer. The application method comprises the steps of sampling a sample extract solution to an okadaic acid Spin solid-phase extraction column; centrifuging, collecting an eluent and filtering the eluent through a 0.22-micron filter membrane; and measuring the content of okadaic acid toxin by adopting an LC-MS / MS. The method has the advantages of being high in sensitivity, good in stability, high in selectivity, simple in method and convenient to operate, and the targets of simply and efficiently achieving selective separation, purification an enrichment of okadaic acid saxitoxin in a shell sample are achieved.

Description

technical field [0001] The invention relates to the technical fields of analytical chemistry and material science, in particular to a preparation method and application of a halicic acid toxin molecularly imprinted-quantum dot polymer. Background technique [0002] Okadaic acid (OA) is a kind of long-chain fatty acid, belonging to polyether toxins. In 1976, poisoning caused by eating blue mussels occurred in Japan. The poisoning was mainly caused by diarrhea, so it was called diarrhea shellfish poison (DSP). However, okadaic acid has long-lasting toxicity and strong carcinogenicity. Pay attention to. At present, the United States, Canada and most European and American countries have a maximum limit of 80 μg / 100g for PSP in fresh shellfish, and Canada, Japan, and the United Kingdom require that DSP not exceed 20 μg / 100g in shellfish meat. [0003] Among all marine toxins, OA has the widest distribution range and the highest incidence rate. OA toxin can cause poisoning sympt...

Claims

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Application Information

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IPC IPC(8): C08G77/26C08G77/14C08J9/26B01J20/26B01J20/30
CPCB01J20/268B01J2220/4812C08G77/14C08G77/26C08J9/26C08J2383/06C08J2383/08
Inventor 史西志肖婷婷孙爱丽李逊甲李德祥陈炯
Owner NINGBO UNIV
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