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Preparation method and application of a saxitoxin molecularly imprinted nano-fluorescent material

A saxitoxin and molecular imprinting technology, applied in the fields of analytical chemistry and material science, can solve the problems of unsuitable STX molecularly imprinted polymers, difficult to obtain STX structural analogs, and high synthesis costs, and achieve good fluorescence stability and specificity. Selectivity, rapid specific identification and detection, the effect of reducing the cost of preparation

Active Publication Date: 2020-04-17
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high cost of clamshell toxins, conventional molecular imprinting techniques require a large amount of template molecules, and STX structural analogues are not easy to obtain, resulting in high synthesis costs, which are not suitable for the preparation of STX molecularly imprinted polymers.

Method used

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specific Embodiment 1

[0025] A preparation method of saxitoxin molecularly imprinted nano fluorescent material, including the following steps: using saxitoxin as a template molecule, adding quantum dot fluorescent nano material, in the presence of crosslinking agent ethyl orthosilicate and functional monomer After the polymerization is initiated, the template molecule in the obtained polymer is removed by the ultrasonic-assisted extraction method to obtain the saxitoxin molecularly imprinted nano fluorescent material that can specifically recognize the saxitoxin. Specific steps are as follows:

[0026] (1) Stir 7.5mL cyclohexane and 1.8mL Triton X-100 for 15min, then add 500μg quantum dot fluorescent nano material, 50μL tetraethylorthosilicate TEOS, 100μL ammonia water, stir for 2h, and finally add a concentration of 1mg / mL of saxitoxin solution 156μL and functional monomer 3-aminopropyltriethoxysilane (APTES) or methacryloxypropyltris(trimethylsiloxy)silane (MPTES) 22.8μL, Stir the room temperature...

specific Embodiment 2

[0032] Combining the new sample pretreatment method QuEChERS and the detection method based on saxitoxin molecularly imprinted nano-fluorescent materials (STX-MIP-QDs), a rapid and highly sensitive detection method for saxitoxin in shellfish samples was established. The specific process is as follows :

[0033] 1. Pretreatment method for shellfish samples based on QuEChERS

[0034] Accurately weigh 1.00 g of scallop meat, add 2 mL of acetonitrile water extract containing 0.1wt% formic acid, vortex for 1 min and then ultrasonically extract for 10 min in ice water, centrifuge at 4500 rpm for 10 min at 15℃ or below, and take precipitation Acetonitrile water extract containing 0.1wt% formic acid (the volume ratio of acetonitrile to water is 80:20) was repeatedly extracted twice with ultrasound, the supernatants obtained after centrifugation were combined, frozen at -20 ℃ for 1 h, and then removed at 1 The upper organic phase was quickly discarded within minutes, and the lower layer wa...

specific Embodiment 3

[0039] 1. Specificity

[0040] Using OA toxin as a template molecule to synthesize OA toxin molecular imprinting-quantum dot polymer, select Saxitoxin dihydrochloride (STX), Anemonetoxins (ATX-a), Gonospora Toxin (Gonyautoxin, DTX), Neosaxitoxin (Neosaxitoxin, NEO) as structural analogs, the specificity of the obtained MIP-QDs was analyzed (the fluorescence quenching system is expressed by the equation, F 0 / F =1+ Ksv [Q], F 0 with F Respectively represent the initial fluorescence value of MIP-QDs and the fluorescence value after adding cypermethrin, 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 blotting efficiency of MIP-QDs. MIP-QDs and NIP-QDs Ksv The ratio of the values ​​represents the imprinting factor ( IF ) To evaluate the selectivity of MIP-QDs. ).

[0041] Result from figure 2 It can be seen tha...

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Abstract

The invention discloses a preparation method of a saxitoxin molecularly-imprinted nano fluorescent material and an application. The preparation method comprises the steps of taking saxitoxin 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 3-aminopropyltriethoxysilane or 3-(tri(trimethsilyl)silyl)propyl methacrylate, and then removing the template molecule in the obtained polymer by adopting an ultrasonic-assisted extraction method to obtain the saxitoxin molecularly-imprinted nano fluorescent material capable of specifically identifying the saxitoxin. The saxitoxin molecularly-imprinted nano fluorescent material can be used for detecting the content of the saxitoxin in a shell sample, and has the advantages of uniform particle sizes, good selectivity and excellent fluorescent stability; and fast and high-sensitivity detection of the saxitoxin in the shell sample can be achieved.

Description

Technical field [0001] The invention relates to the technical fields of analytical chemistry and material science, in particular to a preparation method of a saxitoxin molecularly imprinted nano fluorescent material. Background technique [0002] Saxitoxin dihydrochloride (STX) is currently one of the most toxic marine biotoxins known. It was first discovered in California mussels and later isolated from gonyaulax catenella. The chemical structure is similar to STX Of the substance. STX is a derivative of tetrahydropurine, which is a marine vibramine toxin. STX blocks Na on neuronal cells and cell membranes + Passage, obstructing Na + Inflow, and then the neuromuscular conduction process is disturbed, and the voluntary muscles relax and paralyze, so STX is classified as paralytic shellfish poison. Saxitoxin dihydrochloride (Saxitoxin dihydrochloride, STX) is currently known as one of the most toxic marine biological toxins. It can inhibit the conduction of nerves by affecting s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/26C08G77/14C08G77/02C08G77/04C08J9/26G01N21/64C09K11/02C09K11/88B01J20/26B01J20/28
CPCB01J20/268B01J20/28004C08G77/02C08G77/04C08G77/14C08G77/26C08J9/26C08J2201/0424C08J2383/06C08J2383/08C09K11/025C09K11/883G01N21/6428G01N2021/6432
Inventor 史西志肖婷婷孙爱丽王琳李德祥陈炯李逊甲
Owner NINGBO UNIV
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