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Magnetic nano material for magnetic solid phase extraction and preparation method thereof

A technology of magnetic nanometer and nanometer microspheres, which can be used in material separation, material analysis, material inspection products, etc.

Active Publication Date: 2018-12-07
武汉谱信环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The problem of pesticide residues in agricultural products and the environment has always attracted people's attention. At present, the detection of pesticide residues in domestic agricultural products generally refers to "Determination of Pesticide Residues in Fruits and Vegetables GB / T5009.218-2008" or "National Standard for Agricultural Product Safety Determination of 500 Pesticides and Related Chemical Residues in Fruits and Vegetables by Gas Chromatography-Mass Spectrometry GB23200.8-2016 and Determination of 51 Pesticides in Vegetables and Fruits by Gas Chromatography-Mass Spectrometry NY / T 1380~2007 》, the pretreatment process of these reference standards generally has many steps, and there are two obvious disadvantages: one disadvantage is that the extraction process needs to use a large amount of high-purity organic reagents, and these reagents are not only expensive, but also harmful to the experimenters. Health causes different degrees of harm; another disadvantage is that the purification process requires the use of various expensive solid-phase adsorption columns, and these reagents and columns must be properly disposed of after use, which is generally time-consuming, laborious, and expensive. expensive
This also poses a great challenge to the guarantee of liquid nitrogen and other refrigerants.
In addition, this jet refrigerant modulation technology requires a period of preparation when the equipment is turned on and off, which affects work efficiency.
Therefore, limited to the current conditions, this technology is currently difficult to promote and apply in ordinary laboratories

Method used

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  • Magnetic nano material for magnetic solid phase extraction and preparation method thereof
  • Magnetic nano material for magnetic solid phase extraction and preparation method thereof
  • Magnetic nano material for magnetic solid phase extraction and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0089] Utilize magnetic solid-phase extraction technique to the detection method of fruit, vegetable pesticide residue, comprise the following steps:

[0090] (1) Homogenize 100g of corn kernels with a homogenizer at 9500 rpm for 1 minute to obtain a slurry; take 5g of the slurry in a 50mL centrifuge tube with a stopper, then add 20mL of deionized water and 2mL of acetonitrile, and dissolve at 1800 rpm Shake for 2 minutes;

[0091] (2) Add 50 mg of magnetic nanomaterials to the centrifuge tube with stopper in step (1), and continue to shake at 1800 rpm for 4 minutes;

[0092] (3) The magnet is placed on the side wall of the centrifuge tube, the magnetic nanomaterials fully absorb the pesticides in the agricultural products, the magnetic magnetic nanomaterials are adsorbed on the side wall close to the magnet, and the mixed solution of agricultural products, acetonitrile and water is discarded, Wash the magnetic nanomaterials 3 times with 2 mL deionized water each time, and di...

Embodiment 2

[0130] Substantially the same as Example 1, the difference is only that the preparation method of the magnetic nanomaterial is:

[0131] S1 with 1.35g FeCl 3 ·6H 2 O and 75mL of ethylene glycol were mixed, stirred at 260 rpm for 0.5 hour under the action of a magnetic stirrer, then added 3.6g of sodium acetate, and continued to stir for 1 hour at 260 rpm; continued to add 2.2g of ethylenediamine, at 260 The mixture was stirred at rpm for 15 minutes to obtain a mixed solution; the mixed solution was transferred to a polytetrafluoroethylene-lined stainless steel autoclave with a capacity of 200 mL, and heated and reacted at 200 °C for 12 hours; the reaction product was separated and collected under the action of an external magnetic field, And wash with anhydrous ethanol 60 times the weight of the reaction product, and dry in vacuum at 50°C and a vacuum of 0.07MPa for 8 hours to obtain a black solid Fe 3 o 4 nanospheres;

[0132] S2 will 50mg Fe 3 o 4 The nano-microspheres...

Embodiment 3

[0139] Substantially the same as Example 1, the difference is only that the preparation method of the magnetic nanomaterial:

[0140] S1 with 1.35g FeCl 3 ·6H 2 O and 75mL of ethylene glycol were mixed, stirred at 260 rpm for 0.5 hour under the action of a magnetic stirrer, then added 3.6g of sodium acetate, and continued to stir for 1 hour at 260 rpm; continued to add 2.2g of ethylenediamine, at 260 The mixture was stirred at rpm for 15 minutes to obtain a mixed solution; the mixed solution was transferred to a polytetrafluoroethylene-lined stainless steel autoclave with a capacity of 200 mL, and heated and reacted at 200 °C for 12 hours; the reaction product was separated and collected under the action of an external magnetic field, And wash with anhydrous ethanol 60 times the weight of the reaction product, and dry in vacuum at 50°C and a vacuum of 0.07MPa for 8 hours to obtain a black solid Fe 3 o 4 nanospheres;

[0141] S2 will 50mg Fe 3 o 4 The nano-microspheres we...

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Abstract

The invention discloses a magnetic nano material for magnetic solid phase extraction and a preparation method thereof. The preparation method comprises the following steps: S1, preparing black solid Fe3O4 nano microspheres; S2, preparing Fe3O4@SiO2; S3, weighing dopamine hydrochloride and a Tris buffer solution, the molar concentration of which is 10 mM, and mixing; then adding the Fe3O4@SiO2 andstirring the mixture to react for 16-20 hours; after reaction, centrifugalizing a reaction liquid, collecting bottom solid, and washing and drying the solid to obtain the magnetic nano material. The magnetic nano material combines a conventional mesoporous material with the magnetic nano material, and has properties of the two and has a relatively large specific surface area. Pretreatment is carried out in pesticide extraction of fruits and vegetables by adopting a magnetic solid phase extraction technology, extraction and purification steps are finished by one time of operation, and the method is simple to operate, labor and time saving and low in cost. A complex matrix can be separated efficiently, and various pesticide residues in the complex matrix can be fed at one time and analyzed simultaneously.

Description

technical field [0001] The invention belongs to the technical field of magnetic nanomaterials, and relates to a magnetic nanomaterial for magnetic solid-phase extraction and a preparation method thereof. Background technique [0002] The problem of pesticide residues in agricultural products and the environment has always attracted people's attention. At present, the detection of pesticide residues in domestic agricultural products generally refers to "Determination of Pesticide Residues in Fruits and Vegetables GB / T5009.218-2008" or "National Standard for Agricultural Product Safety Determination of 500 Pesticides and Related Chemical Residues in Fruits and Vegetables by Gas Chromatography-Mass Spectrometry GB23200.8-2016 and Determination of 51 Pesticides in Vegetables and Fruits by Gas Chromatography-Mass Spectrometry NY / T 1380~2007 》, the pretreatment process of these reference standards generally has many steps, and there are two obvious disadvantages: one disadvantage ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30G01N30/06G01N33/88
CPCB01J20/06B01J20/103B01J20/22B01J20/28007B01J20/28009B01J20/28019B01J20/3085G01N30/06G01N33/88G01N2030/062
Inventor 赵之骏郑锦彪周新光宋国新王升
Owner 武汉谱信环保科技有限公司
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