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

A technology for pesticide residues and treatment methods, which is applied in measurement devices, instruments, scientific instruments, etc., can solve problems such as not being found, and achieve the effects of small matrix interference, high stability and reliability, and simple treatment process.

Inactive Publication Date: 2011-07-13
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 (accurate to 0.01 g) of the crushed sample of Chinese herbal medicine Astragalus, add 20 mL of acetonitrile to a centrifuge tube, vortex for 2 min, and centrifuge at 4000 rpm for 5 min. Spin for 2min, centrifuge at 4000rpm for 5min, and combine the supernatant;

[0042] (2) The extract was evaporated to dryness at 40°C, and the residue was dissolved in 5mL of acetone-n-hexane with a volume ratio of 20:80, to be purified;

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

[0044] (4) Transfer the sample solution 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, transfer all the washing solution to the syringe, and collect all the outflows After the sample liquid was completely drained, it was elu...

Embodiment 2

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

[0047] (2) The extract was evaporated to dryness at 40°C, and the residue was dissolved in 5mL of acetone / n-hexane with a volume ratio of 20 / 80, to be purified;

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

[0049] (4) Transfer the sample solution to the syringe, and then wash the sample bottle with acetone / n-hexane of 1 / 4 volume ratio, 5 mL each time, wash twice, and transfer all the washing solution to the syringe, and collect all the...

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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 with an 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 pesticide residue determination, and relates to a method for determining Chinese herbal medicine samples containing carbamate pesticide residues, more specifically, a method for processing Chinese herbal medicine samples containing 15 carbamate pesticide residues before determination. Background technique: [0002] Pesticide residues refer to the phenomenon that a part of pesticides remains directly or indirectly in grains, vegetables, fruits, livestock products, aquatic products, soil and water bodies after the application of pesticides 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. Excessive pesticide r...

Claims

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Application Information

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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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