Carbon nanotube surface molecularly-imprinted solid phase extraction column for carbofuran

A technology of surface molecular imprinting and solid phase extraction column, which is applied in separation methods, solid adsorbent liquid separation, preparation of test samples, etc., can solve the problem of low density of effective imprinting sites, small binding capacity of target molecules, binding kinetics, etc. Slow and other problems, to achieve the effect of high column capacity, good selectivity, and simple analysis process

Inactive Publication Date: 2019-04-19
CHINA CRIMINAL POLICE UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the molecularly imprinted materials currently widely used have a low density of effective imprinting sites, a small binding capacity for target molecules, and slow binding kinetics.

Method used

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  • Carbon nanotube surface molecularly-imprinted solid phase extraction column for carbofuran
  • Carbon nanotube surface molecularly-imprinted solid phase extraction column for carbofuran
  • Carbon nanotube surface molecularly-imprinted solid phase extraction column for carbofuran

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1 Preparation of Molecularly Imprinted Polymer on the Surface of Carbofuran Carbon Nanotubes (SPE Column Packing)

[0028] Add 0.5g multi-walled carbon nanotubes to 100ml concentrated HNO 3 The solution was ultrasonically treated for 1 h, and then refluxed at 80° C. for 24 h under magnetic stirring. Afterwards, filter the dispersion with a 0.22 μm filter membrane, wash the obtained particles repeatedly with distilled water to neutrality, and dry them under vacuum at 65°C overnight for later use; In the mixed solution of chloroform, reflux at 60°C for 24h under magnetic stirring. After cooling, the mixture was dispersed through a 0.22 μm filter membrane with anhydrous tetrahydrofuran, and washed with distilled water several times until neutral, dried in vacuum at 65°C overnight, and set aside; Mix 0.15 g of the above-prepared carbon nanotubes with 0.87 g of allyl alcohol, 0.18 g of 4-DMAP and 4.5 g of triethylamine, add 20 ml of anhydrous THF, reflux at 50 ° C f...

Embodiment 2

[0029] Example 2 Preparation of Carbofuran Carbon Nanotube Surface Molecularly Imprinted Solid Phase Extraction Column

[0030] 1. Empty column material and specification

[0031] The size of the empty column of the existing solid phase extraction column varies from 1cm to 5cm. The empty column is made of polypropylene, and there are polyethylene sieve plates with 20 μm pore size on the upper and lower sides of the small column. The above-mentioned empty columns can all be used in the present invention, but the 3cm specification is adopted in the following examples.

[0032] 2. Packing of solid phase extraction column

[0033] The filler of the solid phase extraction column is molecularly imprinted polymer on the surface of carbofuran carbon nanotubes.

[0034] 3. Filling volume and filling height

[0035] Fill a 3cm solid-phase extraction column with the molecularly imprinted polymer on the surface of carbofuran carbon nanotubes prepared above, as shown in the attached fi...

Embodiment 3

[0036] Example 3 Separation and purification of carbofuran in biological samples by solid phase extraction

[0037] 4LD 50 (44 mg / kg) for intragastric administration. After the rat died, 1 g of its liver was taken, cut into pieces, added with 2 μg of carbaryl and 2 mL of water, and homogenized at 15,000 rpm for 3 min. The obtained carbofuran carbon nanotube surface molecularly imprinted solid-phase extraction column was completely infiltrated with 4ml of methanol and kept for 5min, and then let off the liquid at a rate of 1 drop / second. After the treatment, the small column was in an activated state; The sample flows through the extraction column at a speed of 2 ml / min, and the solvent component is removed by suction filtration, and then the solid-phase extraction column is eluted with methanol / acetic acid (90:10), and the qualitative and quantitative analysis is performed by high-performance liquid chromatography to obtain the liver The carbofuran content is 0.1-10 μg / g.

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Abstract

The invention discloses a carbon nanotube surface molecularly-imprinted solid phase extraction column for carbofuran. A carbon nanotube surface molecularly-imprinted material for selectively extracting and separating carbofuran from a biological sample is used as a filler to prepare the solid phase extraction column. The matrix of the solid phase extraction column is a carbon nanotube surface molecularly-imprinted polymer for carbofuran, the carbon nanotube surface molecularly-imprinted polymer for carbofuran is prepared through a molecular imprinting polymerization reaction on the surface ofthe carbon nanotubes and elution of template molecules, the volume of the empty tube of the solid phase extraction column is 1-5 ml, the filling height is 0.5-2.0 cm, and the empty tube is made from polypropylene. The carbon nanotube surface molecularly-imprinted solid phase extraction column has the characteristics of high selectivity to the target substance, high column capacity (20 [mu]g/g), good recovery rate (80-102%), low preparation cost, easily available materials, and suitableness for mass production, and has a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of the application of molecular imprinting technology on the surface of carbon nanotubes in the pretreatment of poisoned biological inspection materials, and relates to the preparation of molecularly imprinted polymers on the surface of carbofuran carbon nanotubes and the preparation of nano The tube surface molecularly imprinted solid phase extraction column is used to separate, extract and purify carbofuran in biological samples. Background technique [0002] Carbofuran is a carbamate insecticide, the pure product is white crystal, and it is mainly used for seed coating treatment in demand. According to China's pesticide toxicity classification standards, carbofuran is a highly toxic pesticide and cannot be used on vegetables and fruit trees. In recent years, my country has strictly prohibited its use on vegetables, restricted the scope of application, and prohibited the registration of pesticides contain...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/22B01J20/26B01J20/30C08J9/26C08F120/14C08K9/02C08K9/04C08K3/04G01N1/34
CPCB01D15/22B01J20/20B01J20/261B01J2220/4806B01J2220/4812C08F120/14C08J9/26C08J2333/12C08K3/041C08K9/02C08K9/04C08K2201/011G01N1/34
Inventor 张文骥郑吉龙姜兆林许英健李栋王鹏陈洋
Owner CHINA CRIMINAL POLICE UNIV
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