Method for detecting organic copper pesticide residue in fruits and vegetables

A pesticide residue, organic copper technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of low detection sensitivity, cumbersome operation process, easy to be interfered by impurities, etc., and achieve good purification effect, accurate measurement, and improved use. effect of life

Inactive Publication Date: 2015-01-14
TOBACCO RES INST CHIN AGRI SCI ACAD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The detection practice found that this method of residue analysis has the following disadvantages: 1) The solvent is seriously wasted and pollutes the environment; 2) The operation process is cumbersome, time-consuming and labor-intensive; 3) The extraction rate is low; 4) The detection sensitivity is low, Susceptible to impurities

Method used

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  • Method for detecting organic copper pesticide residue in fruits and vegetables
  • Method for detecting organic copper pesticide residue in fruits and vegetables
  • Method for detecting organic copper pesticide residue in fruits and vegetables

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Embodiment 1: the detection of copper quinoline residual amount in tomato

[0059] (1) extraction

[0060] Weigh 5.0g tomato sample in a 50mL centrifuge tube, add 1g Na 2 S, fully vortexed on a vortex oscillator for 2 minutes, then added 15 mL of methanol, vortexed for 2 minutes, ultrasonically extracted for 1 hour (during ultrasonication, shaking once every 20 minutes), and centrifuged at 4000 rpm for 10 minutes. Add 5 mL of methanol and repeat the extraction once. Combine the two extracted supernatants, dilute to volume in a 25ml volumetric flask, and mix well.

[0061] (2) purification

[0062] Take 1 mL of the extract in a 2 mL centrifuge tube, add 50 mg of PSA and 50 mg of C18 adsorbent, and centrifuge at 13000 rpm for 10 min in an ultra-high speed centrifuge. Take the supernatant, pass through a 0.45 μm filter membrane, and wait for the test.

[0063] (3) UPLC-MS / MS detection

[0064] UPLC detection conditions are:

[0065] Thermo Scientific TSQ Quantum Ultra...

Embodiment 2

[0099] Embodiment 2: the detection of nonyl copper residue in cucumber

[0100] (1) extraction

[0101] Weigh 5.0g cucumber sample in a 50mL centrifuge tube, add 1g Na 2 S, fully vortexed on a vortex oscillator for 2 minutes, then added 15 mL of methanol, vortexed for 2 minutes, ultrasonically extracted for 1 hour (during ultrasonication, shaking once every 20 minutes), and centrifuged at 4000 rpm for 10 minutes. Add 5 mL of methanol and repeat the extraction once. Combine the two extraction supernatants, dilute to volume in a 25mL volumetric flask, and mix well.

[0102] (2) purification

[0103] Take 1 mL of the extract in a 2 mL centrifuge tube, add 50 mg of PSA and 50 mg of C18 adsorbent, and centrifuge at 13000 rpm for 10 min in an ultra-high speed centrifuge. Take the supernatant, pass through a 0.45 μm filter membrane, and wait for the test.

[0104] (3) UPLC-MS / MS detection

[0105] UPLC detection conditions are:

[0106] Thermo Scientific TSQ Quantum Ultra;

...

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Abstract

The present invention provides a method for detecting organic copper pesticide residue in fruits and vegetables, wherein a dispersive solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry method is adopted to detect. The method specifically comprises: (1) preparing standard solutions; (2) adding a complexation breaking agent to a sample to carry out complexation breaking, adding methanol, and carrying out vortex vibration and ultrasonic extraction; (3) purifying; (4) detecting with an instrument, wherein the standard work solutions with a series of concentrations in the steps (1) are subjected to sample injection, UPLC-MS / MS detection is performed, and UPLC-MS / MS detection is performed on the purified sample collected in the step (3); (5) establishing a standard curve; and (6) analyzing the result, and calculating the organic copper pesticide content in the sample. With the method, organic copper pesticide residue in fruits and vegetables can be rapidly and accurately detected, the method has characteristics of simpleness, rapidness, accuracy and reliability, and important values are provided for guidance of safe and rational organic copper pesticide use and control of organic copper residue in fruits and vegetables.

Description

technical field [0001] The invention belongs to the technical field of trace analysis, and in particular relates to a method for detecting residual organic copper pesticides in fruits and vegetables by using dispersive solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry (QuEChERS-UPLC-MS / MS). Background technique [0002] As a multi-site fungicide, the copper preparation mainly depends on the concentration of copper ions released from the preparation. After the copper salt is sprayed on the surface of the crops, under the action of the organic acid secreted by the plant or the carbonic acid formed by the carbon dioxide released by the respiration and the carbonic acid formed by the water, it can be gradually decomposed, and the copper ions are slowly released to play a bactericidal effect. [0003] Copper preparations include organic copper preparations and inorganic copper preparations. Since inorganic copper fungicides cannot be mi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 王秀国李义强闫晓阳宋超
Owner TOBACCO RES INST CHIN AGRI SCI ACAD
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