Preparation method of nano-gold immobilized beads and its application in thiram detection

A technology of immobilizing small balls and nano-gold, which is applied in the direction of analysis by chemical reaction of materials and material analysis by observing the influence of chemical indicators, which can solve the problems of limited repeatability and reliability of test results, and test results. Problems such as poor repeatability and reliability, poor stability of the detection system, etc., to achieve the effect of easy on-site detection, improved storage stability, and less sample volume

Active Publication Date: 2019-12-24
CHINA UNIV OF PETROLEUM (EAST CHINA)
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Problems solved by technology

[0008] The preparation of nano gold generally adopts the reduction method, which requires not only a variety of reagents, such as: raw materials (chloroauric acid), reducing agents (sodium citrate, ascorbic acid, sodium borohydride, etc.), but also high temperature conditions (120°C) , the reaction process is relatively complicated, and it is not safe, which limits the application of nano gold in on-site detection to a certain extent, and is very inconvenient to use
[0009] (2) The stability of the detection system is poor, and the repeatability and reliability of the detection results are limited
[0010] In a solution environment, the aggregates formed after the interaction of nano-gold and ziram cannot exist stably, and are prone to sedimentation. Therefore, during detection, the colorimetric result must be read immediately after the interaction of nano-gold and ziram, otherwise it will Causes inaccurate reading of results, poor repeatability and reliability of test results

Method used

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  • Preparation method of nano-gold immobilized beads and its application in thiram detection
  • Preparation method of nano-gold immobilized beads and its application in thiram detection
  • Preparation method of nano-gold immobilized beads and its application in thiram detection

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preparation example Construction

[0037] The embodiment of the present invention provides a preparation method of nano-gold immobilized beads, comprising the following steps:

[0038] Step 1: Weigh di-tert-butyl dicarbonate tyrosine, N-hydroxysuccinimide and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, add 2 - (N-morpholine) ethanesulfonic acid aqueous solution was stirred and dissolved, reacted for 96-144min, then added chitosan solution and stirred overnight, and the reacted solution was placed in an ultrafiltration tube for centrifugal ultrafiltration to obtain chitosan graft Tyrosine solution.

[0039] In this step, N-hydroxysuccinimide (NHS) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) activate di-tert-butyldicarbonate The carboxyl group of ester tyrosine, 2-(N-morpholine) ethanesulfonic acid aqueous solution (being MES damping fluid) is used for providing the acidic environment required for activation reaction, the di-tert-butyl dicarbonate tyrosine through activ...

Embodiment 1

[0065] A preparation method for nano-gold immobilized beads, comprising the steps of:

[0066] Step 1: Weigh 0.5g chitosan, add 19.4g water and 0.63g acetic acid, mix well to obtain chitosan solution; weigh 7.67mg di-tert-butyl dicarbonate tyrosine, 8mg N-hydroxysuccinyl imine and 34mg of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, add 5.6mL of 1mol / L 2-(N-morpholine)ethanesulfonic acid aqueous solution and stir to dissolve, With 1200r / min rotating speed stirring reaction 120min, then add the prepared chitosan solution stirring reaction overnight, the solution after the reaction is placed in the ultrafiltration tube (molecular weight cut-off is 10kDa), with the speed centrifugation ultrafiltration of 11000r / min 7min, And repeat 2-4 times to obtain chitosan grafted tyrosine solution.

[0067] Step 2: Add 40 mL of 0.5 mmol / L chloroauric acid aqueous solution to the chitosan-grafted tyrosine solution obtained in step 1, and adjust the pH value of the solution to...

Embodiment 2

[0070] Step 1: Weigh 0.4g chitosan, add 15.5g water and 0.504g acetic acid, mix well to obtain chitosan solution; weigh 6.13mg di-tert-butyl dicarbonate tyrosine, 6.4mg N-hydroxybutanediol imide and 27.2mg of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, add 5.15mL of 0.87mol / L 2-(N-morpholine)ethanesulfonic acid aqueous solution Stir and dissolve, stir and react with 1100r / min rotating speed for 96min, then add the prepared chitosan solution and stir to react overnight, the solution after the reaction is placed in an ultrafiltration tube (molecular weight cut-off is 10kDa), and centrifuged at a speed of 10000r / min Filter for 5 minutes, and repeat 2-4 times to obtain chitosan grafted tyrosine solution.

[0071] Step 2: Add 35.56mL of 0.45mmol / L chloroauric acid aqueous solution to the chitosan grafted tyrosine solution obtained in step 1, and adjust the pH value of the solution to 11.5, shake it up, and let it stand at 37°C for reaction 24min, the chitosan-nano...

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Abstract

The invention provides a preparation method of nano gold immobilized pellets and application of the nano gold immobilized pellets to ziram detection. The preparation method comprises the following steps: weighing ditert-butyl bicarbonate, NHS and EDC, adding the ditert-butyl bicarbonate, the NHS and the EDC into an MES buffer solution for stirring reaction, adding a chitosan solution for reactionover night, and placing the solution in an ultrafiltration pipe for centrifugal ultrafiltration, thereby obtaining a chitosan grafted tyrosine solution; then adding a chloroaurate aqueous solution into the chitosan grafted tyrosine solution, adjusting the pH value, uniformly shaking the mixed solution, and stewing to obtain a chitosan-nano gold solution; mixing the obtained chitosan-nano gold solution with epoxy chloropropane, dropwise adding the mixture into a sodium hydroxide solution, filtering out suspended pellets in the solution, and drying the pellets, thereby obtaining the nano gold immobilized pellets. The nano gold immobilized pellets prepared by the preparation method provided by the invention are easy to store and high in stability, do not need to be prepared for instant use, and is convenient to use; when the nano gold immobilized pellets are applied to the ziram detection, a detection system is high in stability, and a detection result is high in repetitiveness and reliability.

Description

technical field [0001] The invention belongs to the field of pesticide residue detection, and in particular relates to a preparation method of nano-gold immobilized balls and its application in thiram detection. Background technique [0002] Zirconia dithiocarbamate (zinc dimethyl dithiocarbamate) is a dithiocarbamate fungicide that can prevent and treat various fungal plant diseases. It has high efficiency, low toxicity, and is not easy to induce pathogen resistance. It is relatively safe for humans, animals and plants, and has a broad-spectrum bactericidal effect on plant diseases, and is widely used in agricultural production. However, zirconium moves quickly in the soil and easily enters groundwater, and its metabolites (ethylenethiourea and propylenethiourea) also have carcinogenic, mutagenic and teratogenic effects. Therefore, the detection of ziram should be strengthened very important. [0003] At present, traditional methods such as chromatography and capillary el...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/78
Inventor 杨丽敏张晓慧姜磊王金鑫
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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