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Solid-phase extraction column and preparation method thereof

A solid-phase extraction column and extraction column technology, applied in chemical instruments and methods, other chemical processes, material separation, etc., can solve the problems of low sample matrix selectivity and poor purification effect, so as to increase accuracy and improve cleanliness. , the effect of low selectivity

Inactive Publication Date: 2013-04-17
吉林出入境检验检疫局检验检疫技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention discloses a solid-phase extraction column, which solves the disadvantage of poor purification effect of traditional solid-phase extraction products, improves the cleanliness of samples, increases the accuracy of sample detection, and has versatility. Low sensitivity, applicable to the detection of most food samples

Method used

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  • Solid-phase extraction column and preparation method thereof
  • Solid-phase extraction column and preparation method thereof
  • Solid-phase extraction column and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Preparation of graphitized carbon black

[0033] Take carbon powder and wash away metal and other organic impurities with sulfuric acid, hydrochloric acid, water, methanol, acetone and other organic solvents, dry it, add 0.1mol / L NaOH quantitatively, and place it in a high-temperature reforming furnace under the protection of high-purity helium. 10°C / min to raise the temperature to 1000°C, keep it warm for 12 hours, and quickly add 0.1mol / L K quantitatively after cooling down to room temperature 2 HPO 4 , heat up to 2000°C at 20°C / min, keep it warm for 12 hours, add K repeatedly after cooling down 2 HPO 4 Step, the product is washed with a large amount of water, washed and dried with acetone to obtain the product; tested by a specific surface area analyzer, the pore volume is 0.8-1.2 cm3 / g, and the specific surface area is 250-400 m2 / g.

Embodiment 2

[0035] Preparation of Polyaminated Fillers

[0036] Add porous polystyrene microspheres, concentrated hydrochloric acid (50:1, mass ratio), 2mol zinc chloride, and 1mol paraformaldehyde into the reactor, heat to 70°C, react for 24 hours, filter the product, wash with water until neutral, and then bake Dry, add concentrated ammonia water, ethylenediamine, and trimethylamine aqueous solution with a molar ratio of 3:2:1 into the reactor, react at 60°C for 48 hours under nitrogen protection, filter the product, wash with a large amount of water until it is neutral, and then dry it to obtain: Tested by the specific surface area analyzer, the specific surface area is 1000 m 2 / g.

Embodiment 3

[0038] Preparation of Hydrophobic Group Bonded Silica Gel

[0039] Use sodium citrate to reduce chloroauric acid to obtain gold nanoparticles with a diameter of 10-15nm. Another 50um fully porous silica gel is added to the reactor, and then 30ml of xylene, 20ml of mercaptosilane reagent, and 15ml of pyridine are added in order to react under reflux for 24 hours. Then cool down, wash the product with toluene, dichloromethane, methanol, and acetone, then dry it, add it to another reactor, add the gold nanoparticles prepared at the beginning, then add an excess of n-octadecyl mercaptan, and heat and reflux for 48 hours. The product was filtered and washed with methanol and acetone and then dried to obtain the obtained product.

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Abstract

The invention provides a solid-phase extraction column and a preparation method thereof. At the bottom of a column tube, the following operations are carried out in sequence: an outlet sieve plate is pressed in, a graphitized carbon black layer is filled in, a layer of insulating sieve plate is pressed in, a multi-amination packing layer is filled in, a hydrophobic group bonded silica gel resin layer is filled in after being pressed into the insulating sieve plate, and an inlet sieve plate is finally pressed in; and an outlet of the extraction column is arranged at the bottom of the column tube. The solid-phase extraction column provided by the invention is a pesticide residue detection special column and is made of a three-layer adsorbing material. Impurities, such as amino acid microelements, and heavy metal, can be removed by selectively adsorbing and selectively eluting and purifying a matrix of a complex sample, so that the defect of poor purification effect of the conventional solid-phase extraction product can be avoided, the cleaning degree of the sample is greatly improved, an analyzer is effectively protected, the accuracy of sample detection is improved, the detection sensitivity is improved, the time is saved, and the working efficiency of detectors can be improved. Furthermore, the solid-phase extraction column has the advantages of generality, and low selectivity of a matrix of the sample to be detected, and can be applicable to detection of most food samples.

Description

technical field [0001] The invention provides a solid-phase extraction column, which is used for sample extraction and purification in the detection of pesticide residues in food. The invention also discloses a preparation method of the solid-phase extraction column, which belongs to the technical field of analytical chemical materials. Background technique [0002] In recent years, the problem of pesticide residues in food has been widely concerned, and related researches are increasing day by day. There are many types of pesticides. The commonly used pesticides in my country include organochlorines, organophosphorus, carbamates, and pyrethroids. Organochlorines include HCH, DDT, etc. These pesticides were banned in my country in 1983, but due to their long half-life, they still remain in soil and groundwater. They are easy to accumulate in the human body and cause chronic poisoning, seriously endangering human health. Organophosphorus and carbamates can inhibit the activi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02B01J20/282B01J20/283B01J20/285B01J20/30
Inventor 王明泰李爱军牟峻张代辉康明琴胡婷婷牛茜张勋
Owner 吉林出入境检验检疫局检验检疫技术中心
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