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

A technology of saxitoxin and molecular imprinting, which is applied in the field of analytical chemistry and material science, can solve the problems of unsuitable STX molecularly imprinted polymers, difficulty in obtaining STX structural analogues, high synthesis costs, etc., and achieve good fluorescence stability and specificity Selectivity, rapid specific identification and detection, and the effect of reducing preparation costs

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

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

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specific Embodiment 1

[0025] A preparation method of saxitoxin molecularly imprinted nano-fluorescent material, comprising the following steps: taking saxitoxin as a template molecule, adding quantum dot fluorescent nano-materials, in the presence of cross-linking agent orthosilicate and functional monomers Next, after the polymerization is initiated, the template molecules in the obtained polymer are removed by ultrasonic-assisted extraction, and the saxitoxin molecularly imprinted nano-fluorescent material that can specifically recognize saxitoxin is obtained. Specific steps are as follows:

[0026] (1) Stir 7.5mL cyclohexane and 1.8mL Triton X-100 for 15min, then add 500μg of quantum dot fluorescent nanomaterials, 50μL of tetraethyl orthosilicate TEOS, 100μL of ammonia water, stir for 2h, and finally add the concentration of 1mg / 156 μL of saxitoxin solution in mL and 22.8 μL of functional monomer 3-aminopropyltriethoxysilane (APTES) or methacryloxypropyl tris(trimethylsiloxane) silane (MPTES), ...

specific Embodiment 2

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

[0033] 1. QuEChERS-based shellfish sample pretreatment method

[0034] Accurately weigh 1.00 g of shellfish meat, add 2 mL of acetonitrile water extract containing 0.1 wt% formic acid, vortex for 1 min, then ultrasonically extract in ice water for 10 min, centrifuge at 4500 rpm for 10 min below 15 °C, and take the precipitate for The acetonitrile water extract containing 0.1wt% formic acid (the volume ratio of acetonitrile and water is 80:20) was repeatedly ultrasonically extracted twice, and the supernatants obtained after centrifugation were combined, frozen at -20°C for 1 hour, and taken out at 1 The upper organic phase was quickly discarded within 1 min, and the lower laye...

specific Embodiment 3

[0039] 1. Specificity

[0040] Synthesize Molecularly Imprinted-Quantum Dot Polymers of Soft Spongy Acid Toxins Using Soft Spongy Acid (OA) Toxins as Template Molecules, Selecting Saxitoxin dihydrochloride (STX), Anemonetoxins (ATX-a), and Ginophyllum 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 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 selectiv...

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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 method for preparing a saxitoxin molecularly imprinted nanometer fluorescent material. Background technique [0002] Saxitoxin dihydrochloride (STX) is one of the most toxic marine biotoxins known so far. It was first discovered in California mussels and later isolated from gonyaulax catenella. Its chemical structure is similar to STX substance. STX is a derivative of tetrahydropurine, which is a marine arcamine toxoid. STX blocks Na on neuronal cells and cell sarcolemma ＋ channel, blocking Na ＋ Inward flow, and then the neuromuscular conduction process is disturbed, causing voluntary muscle relaxation and paralysis, so STX is classified as paralytic shellfish poisoning. Saxitoxin dihydrochloride (STX), as one of the most toxic marine biotoxins known so far, can inhibit nerve conduction by affecting sodium ion channels. difficult. In par...

Claims

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Application Information

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Patent Type & Authority Applications(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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