Magnetic dextrin microspheres, preparation method and application in determination of residual quantity of chlorpyrifos in oyster mushrooms

A subtle and magnetic technology, applied in the field of detection of plant pesticide residues, can solve the problems of physical injury of test personnel, consumption of large organic solvents, cumbersome operation steps, etc., and achieve high accuracy, low solvent toxicity, and high enrichment multiples.

Active Publication Date: 2021-07-23
SHANXI AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In the prior art, liquid chromatography (LC), liquid chromatography-mass spectrometry (LC-MS), gas chromatography (GC), gas chromatography- Mass spectrometry (GC-MS), LC-MS and GC-MS are used to determine the amount of chlorpyrifos pesticide residues. These determination methods all need pretreatment, and liquid phase extraction and solid phase extraction are routinely used, but these two methods are not only operation steps It is cumbersome and time-consuming, and consumes a large amount of organic solvents, so it is gradually replaced by the dispersion liquid-liquid microextraction method in the development process, but the general dispersion liquid-liquid microextraction method uses halogenated hydrocarbons and other toxic substances. Solvent is easy to cause harm to the body of the tester. In summary, there are certain defects in the pretreatment method of the prior art

Method used

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  • Magnetic dextrin microspheres, preparation method and application in determination of residual quantity of chlorpyrifos in oyster mushrooms
  • Magnetic dextrin microspheres, preparation method and application in determination of residual quantity of chlorpyrifos in oyster mushrooms
  • Magnetic dextrin microspheres, preparation method and application in determination of residual quantity of chlorpyrifos in oyster mushrooms

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] A preparation method of magnetic dextrin microspheres, comprising the following steps:

[0059] S1, preparation of water phase:

[0060] Accurately weigh 4g of dextrin and 0.6g of NaOH into a 250mL conical flask, add 200mL of distilled water, and gelatinize at 85°C for 30min;

[0061] S2, preparation of oil phase:

[0062] Accurately weigh 6.6g of Span 60, 13.2g of Tween 80, and 100mL of n-hexane in a 250mL Erlenmeyer flask, and dissolve in a 50°C water bath, then add 0.01g of sodium trimetaphosphate and 0.01g of ferric iron tetroxide Powder, 18mL n-pentanol, mixed evenly to obtain the oil phase;

[0063] S3, preparation of magnetic nano-dextrin microspheres:

[0064] Add the water phase to the oil phase drop by drop and keep stirring. After the water and oil phases are mixed, stir with a high-speed homogenizer for 10 minutes, then place them in a water bath at 60°C for 3 hours, then break the emulsion at 85°C for 30 minutes, and remove the upper layer The oil phase...

Embodiment 2

[0074] A preparation method of magnetic dextrin microspheres, comprising the following steps:

[0075] S1, preparation of water phase:

[0076] Accurately weigh 4g of dextrin and 0.4g of NaOH into a 250mL Erlenmeyer flask, add 180mL of distilled water, and gelatinize at 80°C for 33min;

[0077] S2, preparation of oil phase:

[0078] Accurately weigh 6.6g of Span 60, 0.6g of Tween 80, and 80mL of n-hexane in a 250mL Erlenmeyer flask, dissolve them in a 45°C water bath, then add 0.03g of sodium trimetaphosphate and 0.02g of ferric oxide Powder, 20mL n-pentanol, mix well to get the oil phase;

[0079] S3, preparation of magnetic nano-dextrin microspheres:

[0080] Add the water phase to the oil phase drop by drop and keep stirring. After the water and oil phases are mixed, stir with a high-speed homogenizer for 10 minutes, then place them in a water bath at 55°C for 3.5 hours, then break the emulsion at 80°C for 30 minutes, and remove the upper layer The oil phase was alterna...

Embodiment 3

[0090] A preparation method of magnetic dextrin microspheres, comprising the following steps:

[0091] S1, preparation of water phase:

[0092] Accurately weigh 4g of dextrin and 0.8g of NaOH into a 250mL conical flask, add 200mL of distilled water, and gelatinize at 90°C for 30min;

[0093] S2, preparation of oil phase:

[0094] Accurately weigh 6.6g of Span 60, 9.9g of Tween 80, and 100mL of n-hexane in a 250mL Erlenmeyer flask, and dissolve in a 55°C water bath, then add 0.02g of sodium trimetaphosphate and 0.015g of ferric iron tetroxide Powder, 15mL n-pentanol, mix well to get the oil phase;

[0095] S3, preparation of magnetic nano-dextrin microspheres:

[0096] Add the water phase to the oil phase drop by drop and keep stirring. After the water and oil phases are mixed, stir with a high-speed homogenizer for 10 minutes, then place them in a 65°C water bath for 3 hours, then break the emulsion at 90°C for 30 minutes, and remove the upper layer The oil phase was washe...

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Abstract

The invention relates to the technical field of detection of plant pesticide residues, in particular to a magnetic dextrin microsphere, a preparation method and application of the magnetic dextrin microsphere to determination of the residual quantity of chlorpyrifos in oyster mushrooms. According to the method for determining the residual quantity of the organophosphorus pesticide chlorpyrifos in the oyster mushrooms by combining a convertible hydrophilic solvent, magnetic solid-phase extraction, nano magnetic dextrin microspheres, a dispersive liquid-liquid microextraction technology and high performance chromatography, hexanoic acid is fully contacted with a sample to be detected for extraction, then the magnetic nano dextrin microspheres are used for adsorbing the hexanoic acid, and eluting the sample to be detected for detection. The prepared magnetic microspheres are used as a magnetic solid phase carrier, the magnetic microspheres for adsorbing the poisonous dead Japanese premna herb can be rapidly separated through an external magnetic field, the pretreatment time is obviously shortened, the solvent consumption is greatly reduced, the detection efficiency is greatly improved, meanwhile, low-toxicity caproic acid is used as a solvent, and the detection cost is reduced. The method has a great application value for detecting the chlorpyrifos residues in the oyster mushrooms.

Description

technical field [0001] The invention relates to the technical field of detection of plant pesticide residues, in particular to a magnetic dextrin microsphere, a preparation method and an application in the determination of chlorpyrifos residues in oyster mushrooms. Background technique [0002] Edible fungus is a large edible or medicinal fungus, commonly known as mushroom, and is an important vegetable. It has nutritional properties such as high protein content, low fat content, and a large amount of polysaccharides. It has the effects of enhancing immunity, anti-tumor, and lowering blood sugar and blood lipids for the human body. [0003] Organophosphorus pesticides are widely used as a class of pesticides. They are widely used in agriculture, horticulture, and medical treatment because of their high activity, low residue, variety, easy decomposition, and difficult accumulation in animals and humans. Organophosphorus compounds have many advantages, but their disadvantages...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/08G01N30/88
CPCG01N30/08G01N30/88
Inventor 张素敏冯翠萍荆旭陈振家
Owner SHANXI AGRI UNIV
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