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Solid phase dispersion microwave extraction method of sample residues matrix and extraction stuffing and solvent

A matrix solid-phase and solid-phase dispersion technology, applied in solid solvent extraction and other directions, can solve the problems of low recovery rate, difficult and complicated extraction, and achieve high extraction efficiency, good extraction effect, and wide application.

Inactive Publication Date: 2006-07-19
林黎明
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Some of the existing sample pretreatment methods require complex instruments and equipment; some have unsatisfactory extraction effects on complex biological samples; some are difficult to simultaneously extract multiple target compounds with different chemical properties, especially those exceeding In the case of simultaneous determination of more than 20 kinds of residues, reaching hundreds of kinds and hundreds of residues, it is difficult to achieve a balanced extraction effect in the same polar solvent and the same pH range; it is difficult to extract substances or metabolites with strong protein binding large, low recovery

Method used

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Examples

Experimental program
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Effect test

specific Embodiment approach 1

[0094] Rapid Extraction and Determination of 24 Sulfa Residues in Animal Tissues

[0095] Weigh 1g of the animal sample, put it in a mortar, add 3g of C18 solid phase extraction filler, mix and grind it with the animal sample thoroughly, then put it into a 50mL polytetrafluoroethylene test tube, add 30mL of acetonitrile, tighten the test tube cap, and shake Mix for 2 minutes, then put it into a microwave generator, select the appropriate energy, and microwave for 30 seconds, take out the test tube and shake it for 5 minutes, then centrifuge at 3000 rpm for 5 minutes, transfer the supernatant to the Erlenmeyer flask, Rotary evaporate at 40°C to near dryness, blow dry with nitrogen flow, add 1mL mobile phase to dissolve the residue, shake and dissolve on a vortex shaker for 1 minute, transfer the solution into a 5mL glass test tube, add 1mL mixed purification solution, and shake for 2 minutes , centrifuge at 3000 rpm for 3 minutes, pipette the upper layer solution through a butt...

specific Embodiment approach 2

[0096] Rapid Extraction and Determination of 250 Pesticide Residues in Vegetables and Fruits

[0097]Weigh 2g of the sample, put it in a mortar, add 5g of C18 and PSA special mixed solid-phase extraction filler, mix and grind it thoroughly, then put it into a 50mL polytetrafluoroethylene test tube, add 30mL of acetonitrile-acetone mixed extract, and tighten Cover the test tube, shake and mix for 2 minutes, then put it into the microwave generator, select the appropriate energy, microwave radiation for 30 seconds, take out the test tube and shake for 5 minutes, then centrifuge at 3000 rpm for 5 minutes, transfer the supernatant into the cone Rotary evaporate at 40°C until nearly dry, blow dry with nitrogen flow, add 1mL of n-hexane to dissolve the residue, shake and dissolve on a vortex shaker for 1 minute, pass through a button-type filter membrane into a 2mL injection vial, and supply air Phase chromatography / mass spectrometry.

specific Embodiment approach 3

[0098] Rapid extraction and determination of toxins (tetramine, heroin, barbiturate, chlorpromazine, etc.) in biological samples (blood, urine, liver)

[0099] Weigh 1 g of blood sample, put it in a mortar, add 3 g of C18 and PSA (1:3) special mixed solid phase extraction filler, mix and grind thoroughly, then put it into a 50 mL polytetrafluoroethylene test tube, add 30 mL of dichloromethane- Benzene mixed extract (7:3), tighten the test tube cap, shake and mix for 2 minutes, then put it into a microwave generator, select appropriate energy, microwave radiation for 30 seconds, take out the test tube and shake for 5 minutes, and then turn it at 3000 rpm / Centrifuge for 5 minutes, transfer the supernatant into a round bottom flask, rotatably evaporate at a temperature of 40°C until nearly dry, blow dry with nitrogen flow, add 1 mL of methanol to dissolve the residue, shake and dissolve on a vortex shaker for 1 minute, pass through a button-type The filter membrane is placed in...

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Abstract

The invention discloses a solid-phase dispersed microwave extraction method of residual sample base and solid-phase dispersed microwave extraction filler and extraction solvent, which comprises the following steps: 1) mixing the detected sample and solid-phase dispersed microwave extraction filler; grinding evenly; 2) adding the extraction solvent in the microwave generator to proceed the microwave radiation; 3) removing the solid impurity to obtain the extract with residue; removing the solid impurity through eccentric action; proceeding rotary evaporation condensation for the extract; dissolving fitful residue as solvent; purifying through the special right mixed purifying agent to analyze the sampling usage for instrument. The invention can extract object compound with different chemical properties effectively.

Description

technical field [0001] The invention relates to the extraction and purification technology of sample residues in analytical chemistry, and is specifically designed to be used for the detection of pesticide residues, veterinary drug residues, biotoxins, and organic pollutants in animal source foods, plant source foods, and other biological samples. Dispersive microwave extraction method; the present invention further relates to a solid phase dispersion extraction filler and an extraction solvent used in a sample residue matrix solid phase dispersion microwave extraction method. Background technique [0002] The analysis of pesticide residues, veterinary drug residues, pollutants, biotoxins, and human drugs and poisons in animal-derived products, plant-derived products or other biological samples, such as gas chromatography, liquid chromatography, gas chromatography, etc. Chromatography / mass spectrometry, liquid chromatography / mass spectrometry, etc. must undergo complicated s...

Claims

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Application Information

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IPC IPC(8): B01D11/02
Inventor 林黎明
Owner 林黎明
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