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Method for detecting luteolin by combining solid-phase extraction and electrochemical sensor

A technology of luteolin and solid-phase extraction column, which is applied in the field of analytical chemistry, can solve the problems of high equipment requirements, cumbersome detection methods, and low sensitivity, and achieve low cost, improved detection sensitivity and accuracy, and low matrix interference. Effect

Active Publication Date: 2020-12-01
QINGDAO AGRI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] For the problems existing in the prior art, one of the purposes of the present invention is to provide a kind of ZrO 2 Nanoparticle and chitosan doped graphene airgel and the preparation method of this airgel; Two of purpose of the present invention is to provide above-mentioned ZrO 2 Nanoparticle and chitosan-doped graphene airgel modified glassy carbon electrode; The third object of the present invention is to provide a kind of ZrO 2 Nanoparticles and chitosan doped graphene airgel modified silica gel and preparation method thereof; The fourth object of the present invention is to provide the above-mentioned ZrO 2 Nanoparticles and chitosan-doped graphene airgel modified silica gel as the solid-phase extraction column of the extraction material; the fifth object of the present invention is to provide a method for detecting luteolin in conjunction with solid-phase extraction and electrochemical sensors; In order to solve the problems of low sensitivity, cumbersome detection methods and high requirements for equipment in the existing detection technology of luteolin

Method used

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  • Method for detecting luteolin by combining solid-phase extraction and electrochemical sensor
  • Method for detecting luteolin by combining solid-phase extraction and electrochemical sensor
  • Method for detecting luteolin by combining solid-phase extraction and electrochemical sensor

Examples

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Effect test

Embodiment 1

[0070] ZrO 2 The preparation of nanoparticles and chitosan doped graphene airgel, the specific steps are as follows:

[0071] (a) Take graphite powder, adopt Hummers method to prepare graphene oxide suspension, in 5mL 0.1wt% graphene oxide suspension, add 0.005g chitosan and 0.05g ZrOCl successively 2 ·8H 2 O, stirring and dispersing;

[0072] (b) Add 1 mL of hydrazine hydrate to the dispersion (a), transfer the mixed solution to the reaction kettle immediately, react at 180°C for 12 hours, cool, and centrifuge;

[0073] (c) put the product obtained in (b) into a freeze dryer, and obtain ZrO after 10h 2 Nanoparticles and chitosan doped graphene airgel.

[0074] figure 2 graphene airgel and ZrO 2 Scanning electron microscope images of nanoparticles and chitosan doped graphene airgel, the thinner and wrinkled structure of graphene airgel can be seen from a, and the ZrO at 10μm and 100nm scales in b and c, respectively 2 SEM images of nanoparticles and chitosan-doped grap...

Embodiment 2

[0077] ZrO 2 A glassy carbon electrode modified by nanoparticles and chitosan-doped graphene airgel, the specific preparation method is:

[0078] (1) First, the bare glassy carbon electrode (the diameter of the bare glassy carbon electrode used in this embodiment is 3 mm) is polished to a mirror surface with 1.0, 0.3 and 0.05 μm alumina powder respectively, and then respectively in 50% nitric acid solution, Sonicate in ethanol and water for 5 minutes;

[0079] (2) 5wt% Nafion solution is diluted to 0.5% solution with N,N-dimethylformamide, the ZrO prepared by 1mg embodiment 1 2 Nanoparticles and chitosan-doped graphene airgel were added to 1mL of 0.5% Nafion solution, ultrasonicated for half an hour, and dispersed evenly;

[0080] (3) Take 1-5 μL of the dispersion solution in step (2) with a pipette gun, drop-coat it on the surface of the glassy carbon electrode treated in step (1), dry it at room temperature before use.

Embodiment 3

[0082] ZrO 2 Nanoparticles and chitosan doped graphene airgel modified silica gel, prepared by the following method:

[0083] ①Add 2g aminopropyl silica gel to 10mL 0.1wt% graphene oxide suspension, add 0.001g N,N-hydroxysuccinimide and 0.001g 1-(3-dimethylpropyl)-3-ethyl Carbodiimide, stir evenly;

[0084] ②Add 0.01g chitosan and 0.1g ZrOCl to ① 2 ·8H 2 O, react at 180°C for 12 hours, and centrifuge;

[0085] ③ Put the product obtained by centrifugation in ② into a freeze dryer, and after 10 hours, ZrO 2 Silica gel modified with nanoparticles and chitosan-doped graphene airgel.

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Abstract

The invention discloses a method for detecting luteolin by combining solid-phase extraction and an electrochemical sensor, and belongs to the technical field of analytical chemistry. According to themethod, ZrO2 nanoparticle and chitosan doped graphene aerogel modified silica gel is used as a solid phase extraction column of an extraction material to extract luteolin in a to-be-detected sample, and ZrO2 nanoparticle and chitosan doped graphene aerogel modified glassy carbon electrode is used as an electrochemical sensor platform to detect the luteolin in the extract liquor. According to the invention, the ZrO2 nanoparticle and chitosan doped graphene aerogel is used as electrode materials, and the ZrO2 nanoparticle and chitosan doped graphene aerogel modified silica gel is used as the extraction material, so that the adsorption selectivity is high, and detection signal amplification is realized; the preparation method is simple and easy to implement and relatively low in cost; and thesolid-phase extraction and the electrochemical sensor are combined, so that the interference of a sample matrix is avoided, the detection sensitivity and accuracy of the method are improved, and theoperation is simple.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, in particular to a method using ZrO 2 Nanoparticles and chitosan-doped graphene airgel-modified glassy carbon electrode combined with solid-phase extraction cartridges to detect luteolin. Background technique [0002] Luteolin is an important flavonoid compound widely present in celery, pepper, wild chrysanthemum, honeysuckle, mint, basil and other plants. Luteolin can produce many biochemical and pharmacological effects on human health. Such as inhibition of cancer cell activity, inhibition of bacterial activity, reduction of retinal damage, anti-allergic activity, anti-inflammatory and antioxidant activity, etc. At present, some studies have shown that excessive luteolin content may cause some side effects. Therefore, it is particularly important to establish a fast, simple and convenient method to determine the content of luteolin in some actual samples. [0003] In recent yea...

Claims

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Application Information

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IPC IPC(8): G01N27/327G01N27/48
CPCG01N27/3277G01N27/3278G01N27/48
Inventor 侯秀丹杨庆利吴薇解万翠
Owner QINGDAO AGRI UNIV
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