Method for processing Chinese herbal medicine sample containing several pesticide residues before determination

A technology of pesticide residues and treatment methods, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of not being detected, and achieve the effects of low matrix interference, high stability and reliability, and simple treatment process

Inactive Publication Date: 2012-09-26
CENT LAB TIANJIN ACADEMY OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The sample pretreatment method established in this patent is a method developed by our unit, and no relevant reports have been found in domestic public literature

Method used

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  • Method for processing Chinese herbal medicine sample containing several pesticide residues before determination
  • Method for processing Chinese herbal medicine sample containing several pesticide residues before determination
  • Method for processing Chinese herbal medicine sample containing several pesticide residues before determination

Examples

Experimental program
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Effect test

Embodiment 1

[0041] (1) Accurately weigh 2 g of the pulverized Chinese herbal medicine Astragali (accurate to 0.01 g), add 20 mL of acetonitrile to a centrifuge tube, vortex for 2 min, centrifuge at 4000 rpm for 5 min, take the supernatant, repeat extraction of the residue once with 20 mL of acetonitrile, vortex Spin for 2 minutes, centrifuge at 4000rpm for 5 minutes, and combine the supernatant;

[0042] (2) Evaporate the extract to dryness at 40°C, dissolve the residue in 5 mL of acetone-n-hexane with a volume ratio of 20:80, and wait for purification;

[0043] (3) Activate the PSA solid phase extraction column with 6mL acetone, 6mL acetone / n-hexane volume ratio 20 / 80, and connect the PSA column with a 25mL syringe with a solid phase extraction column adapter;

[0044] (4) Transfer the sample liquid to the syringe, and then wash the sample bottle with acetone / n-hexane with a volume ratio of 1 / 4, 5 mL each time, wash twice, and transfer all the washing liquid to the syringe, collect all t...

Embodiment 2

[0046] (1) Accurately weigh 2g of the crushed Chinese herbal medicine Semen Cassiae, add 250mL of acetonitrile to a centrifuge tube, vortex for 2min, centrifuge at 4000rpm for 5min, take the supernatant, repeat extraction of the residue once with 15mL of acetonitrile, vortex for 2min, and centrifuge at 4000rpm for 5min , combined supernatant;

[0047] (2) Evaporate the extract to dryness at 40°C, dissolve the residue in 5 mL of acetone / n-hexane with a volume ratio of 20 / 80, and wait for purification;

[0048] (3) Activate the PSA solid phase extraction column with 6mL acetone, 6mL acetone / n-hexane volume ratio 20 / 80, and connect the PSA column with a 25mL syringe with a solid phase extraction column adapter;

[0049] (4) Transfer the sample liquid to a syringe, then wash the sample vial with acetone / n-hexane with a volume ratio of 1 / 4, 5 mL each time, wash twice, transfer all the washing liquid to the syringe, and collect all the effluent; After the sample liquid is completel...

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Abstract

The invention discloses a method for processing a Chinese herbal medicine sample containing carbamate pesticide residues before determination, comprising the following steps: accurately weighing 2g of a smashed Chinese herbal medicine sample; adding 30ml of acetonitrile in a centrifuge tube; eddying for 2 minutes; centrifuging for 5 minutes at 4000 rmp; taking a supernate; repeatedly extracting residues by 10-20ml of acetonitrile once; eddying for 2 minutes; centrifuging for 5minutes at 4000 rmp; combining supernates; drying the extracting solution by evaporation at 40DEG C; dissolving the residues by 5ml of acetone-normal hexane at the volume ratio of 20:80; standing to be purified; activating a PSA (pressure swing adsorption) solid phase extraction column; connecting the PSA column withan injector with the volume of 25ml by an adapter of a solid phase extraction column; restoring the volume by 2ml of methyl alcohol and 0.1% methanoic acid water; performing sampling introduction after passing through a 0.22mu m filter membrane; and determining by an ultrahigh-performance liquid phase-mass spectrum / mass spectrometer. The processing method which is disclosed by the invention has the advantages of high determination speed, simple equipment, low determination cost, and high accuracy, stability and reliability.

Description

Technical field: [0001] The invention belongs to the technical field of determination of pesticide residues, and relates to a method for determining Chinese herbal medicine samples containing carbamate pesticide residues, more specifically, a method for treating Chinese herbal medicine samples containing 15 kinds of carbamate pesticide residues before determination. Background technique: [0002] Pesticide residues refer to the phenomenon that a part of pesticides directly or indirectly remain in grains, vegetables, fruits, livestock products, aquatic products, soil and water after pesticides are applied in agricultural production. The problem of pesticide residues arises with the mass production and widespread use of pesticides. Some of the currently used pesticides can be biodegraded into harmless substances in a relatively short period of time, while some organochlorine pesticides are difficult to degrade and are pesticides with strong residues. Vegetable pesticide resid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/08G01N30/12G01N30/02
Inventor 李娜刘磊李辉邵辉张玉婷郭永泽
Owner CENT LAB TIANJIN ACADEMY OF AGRI SCI
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