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Method for detecting residual quantity of pesticides in vegetable sample by utilizing liquid chromatogram-high resolution mass spectrometer

A high-resolution mass spectrometry and pesticide multi-residue technology, which is applied in the field of liquid chromatography high-resolution mass spectrometry to detect multi-pesticide residues in vegetable samples, can solve non-target compound interference, reduce the impact on qualitative and quantitative, qualitative and quantitative problems, etc., Achieve the effects of reducing pesticide misjudgment, simplifying sample purification, and rapid analysis

Inactive Publication Date: 2011-10-19
CHINA NAT RICE RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the differences in geographical conditions and the matrix of the vegetables themselves, the actual samples are interfered by non-target compounds during the determination, which has a great impact on the givenness and quantification.
[0005] At present, there are few domestic studies on avoiding interference by extracting the accurate mass of pesticides. Most of the established detection standards for pesticide residues in agricultural products focus on gas chromatography and liquid chromatography-tandem mass spectrometry. Extracting the accurate mass of pesticides to detect pesticide residues and reducing the problem of qualitative and quantitative interference has not attracted attention in the detection industry. Only in the petrochemical industry has a patent for the detection of carbazole compounds in crude oil by gas chromatography-high resolution time-of-flight mass spectrometry

Method used

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  • Method for detecting residual quantity of pesticides in vegetable sample by utilizing liquid chromatogram-high resolution mass spectrometer
  • Method for detecting residual quantity of pesticides in vegetable sample by utilizing liquid chromatogram-high resolution mass spectrometer
  • Method for detecting residual quantity of pesticides in vegetable sample by utilizing liquid chromatogram-high resolution mass spectrometer

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Experimental program
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Effect test

Embodiment 1

[0033] 1. Instruments and reagents

[0034] Instruments: Thermo Scientifc LTQ-Orbitrap XL combined high-resolution mass spectrometer (Thermo Electric Company, USA), SURVEYOR-HPLC liquid chromatograph (Thermo Electric Company, USA), high-speed dispersing machine (IKA Company, Germany).

[0035]Reagents: acetonitrile (chromatographically pure, Merck, Germany); acetone, toluene, formic acid (chromatographically pure, Tedia, USA); PSA and C18 packing (particle size 40 μm, Varian); anhydrous magnesium sulfate (analytical pure, Sigma - Aldrich Company); sodium chloride (analytical grade, Shanghai Shisi Hewei Chemical Co., Ltd.), ammonium acetate (analytical grade, American Fluka Company); water is Milli-Q high-purity water; 5mmol / L ammonium acetate containing 0.1% formic acid : Dissolve 0.385g of ammonium acetate in water, then add 1mL of formic acid and dilute to 1000mL with water. 80 kinds of pesticide standard products (purity not less than 95%, Dr Ehrenstorfer Company), were pr...

Embodiment 2

[0053] 1. Sample processing

[0054] (1) Sample extraction: Weigh 30 g of a uniform sample (vegetable matrix) and place it in a 200 mL plastic centrifuge tube, add 35 mL of acetonitrile, place it in a high-speed disperser at 8000 r / min for 3 min, and then add 20g compound salt (mass ratio of anhydrous magnesium sulfate and sodium chloride 10:1), homogenate at 10000 r / min for 2 minutes, and finally, place the centrifuge tube in a centrifuge and centrifuge at 5000 r / min for 6 minutes.

[0055] (2) Sample purification: Take 2mL of the upper acetonitrile phase into a 20mL centrifuge tube, add 0.6g of anhydrous magnesium sulfate, 0.05g of PSA, and 0.05g of C18, shake on a vortex shaker for 2min, then place the centrifuge tube in a centrifuge Centrifuge at 8000 r / min for 3 min. The supernatant was passed through a 0.22 μm organic filter membrane for testing.

[0056] 2. Preparation of standard working solution

[0057] Accurately weigh standard products: methamidophos, acephate, ...

Embodiment 3

[0068] 1. Sample processing

[0069] (1) Sample extraction: Weigh 50g of a uniform sample (Chinese cabbage matrix) and place it in a 200mL plastic centrifuge tube, add 50mL of acetonitrile, place it in a high-speed disperser at 12000 r / min and homogenize for 3min, then pour it into the centrifuge tube Add 25g of compound salt (mass ratio of anhydrous magnesium sulfate and sodium chloride 10:1), homogenize at 12000 r / min for 3 minutes, and finally place the centrifuge tube in a centrifuge and centrifuge at 3000 r / min for 4 minutes.

[0070] (2) Sample purification: Take 6mL of the upper acetonitrile phase into a 20mL centrifuge tube, add 1.8g of anhydrous magnesium sulfate, 0.2g of PSA, and 0.2g of C18, shake on a vortex shaker for 1.5min, then place the centrifuge tube in a centrifuge In the machine, centrifuge at 12000 r / min for 4 minutes. The supernatant was passed through a 0.22 μm organic filter membrane for testing.

[0071] 2. Preparation of standard working solution ...

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Abstract

The invention relates to a method for detecting the residual quantity of pesticides in a vegetable sample by utilizing a liquid chromatogram-high resolution mass spectrometer, which belongs to the technical field of a food safety detecting. The method provided by the invention comprises the following steps: 1) extracting the residual acetonitrile in the sample; 2) carrying out the dispersion solid-phase extraction and purification on a sample extraction solution; 3) detecting by utilizing the liquid chromatogram-high resolution mass spectrometer; and 4) analyzing the result. In the method provided by the invention, the quality accuracy of 27 pesticides is less than 1ppm; the detection limit is 0.01-0.05mg / kg; the addition recovery rate is 80-100%; and the relative standard deviation is less than 15%.

Description

technical field [0001] The invention belongs to the technical field of food safety detection, and in particular relates to a method for detecting multi-residue pesticides in vegetable samples by liquid chromatography high-resolution mass spectrometry. Background technique [0002] In the past 20 years, pesticides have been widely used in crop planting and production. Its role in reducing the occurrence of diseases and insect pests, promoting growth, increasing yield and improving product quality is very significant, and has become an indispensable material basis for modern agriculture. However, the use of pesticides will undoubtedly lead to the retention or accumulation of drugs in crops, and enter the human body and ecosystem in the form of residues. The phenomenon of abuse or illegal use of pesticides still exists, and its harm to humans and the environment is mainly chronic, long-term and cumulative. Pesticide residues in agricultural products have become a recognized agr...

Claims

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Application Information

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IPC IPC(8): G01N30/72
Inventor 牟仁祥陈铭学曹赵云朱智伟
Owner CHINA NAT RICE RES INST
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