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Method for quickly extracting purified benzoylurea pesticide residues from fruits and vegetables

A technology of benzoylureas and pesticide residues, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of polluting chromatographic columns and ion sources, interfering with chromatographic analysis, etc. The effect of large surface area

Active Publication Date: 2019-01-29
GUANGXI ZHUANG AUTONOMOUS REGION ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These co-extractants may interfere with chromatographic analysis and contaminate the column and ion source

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A method for quickly extracting and purifying benzoylurea pesticide residues from fruits and vegetables, comprising the following steps:

[0023] S1. Extraction: Weigh 10 g of homogeneous fruit and vegetable samples into a centrifuge tube, add 20 mL of acetonitrile, and vortex extract for 0.5-2 minutes, then add 3 g of sodium chloride and 2 g of magnesium sulfate, and continue vortexing for 0.5-2 min. Centrifuge at 4000r / min for 2-10min to obtain supernatant.

[0024] S2. Purification: transfer the 2ml supernatant to a centrifuge tube containing 50mg C18 and 50mg tungsten disulfide nanomaterials, shake for 1-5min, centrifuge at 4000r / min for 2-10min, and then pass through a 0.22μm organic microporous filter The membrane was purified.

[0025] S3. Determination: Determination of the concentration of benzoylurea pesticides in the purified liquid by ultra-high performance liquid chromatography.

Embodiment 2

[0027] A method for quickly extracting and purifying benzoylurea pesticide residues from fruits and vegetables, comprising the following steps:

[0028] S1. Extraction: chop the fruit and vegetable samples, and then use a high-pressure homogenizer or a high-pressure homogenizer for homogenization, so that the particle size is below 50 μm. Weigh 10g of homogeneous fruit and vegetable samples into a centrifuge tube, add 15mL of acetonitrile, vortex extract for 0.5-2min, then add 4g of sodium chloride and 3g of magnesium sulfate, continue vortex for 0.5-2min, centrifuge at 4000r / min 2 to 10 minutes to obtain the supernatant.

[0029] S2. Purification: transfer the 2ml supernatant to a centrifuge tube containing 40mg C18 and 60mg tungsten disulfide nanomaterials, shake for 1-5min, centrifuge at 4000r / min for 2-10min, and then pass through a 0.22μm organic microporous filter The membrane was purified.

[0030] S3. Determination: Determination of the concentration of benzoylurea p...

experiment example

[0036] (1) Preparation of standard solution: use chromatographic grade methanol to prepare a concentration of 100mg L -1 The standard solution of siflumuron was then stored at 5 °C until use. Prepare working solutions by diluting stock solutions with methanol.

[0037] (2) Dilute the standard solution with methanol to form working solutions of different concentrations (5 μg kg -1 ~2000μg kg -1 ) were measured respectively: each concentration was measured in parallel 3 times, and the linear equation and correlation coefficient of siflumuron were obtained.

[0038] (3) The method for quickly extracting and purifying benzoylurea pesticide residues of Example 1, Example 2, Comparative Example 1 and Comparative Example 2 is used respectively to extract, purify and measure, and calculate the average recovery rate and RSD, see Table 1 .

[0039] Table 1 Analysis of results

[0040] test methods

[0041] Can find out from embodiment 1-2, comparative example 1-2, experim...

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Abstract

The invention provides a method for quickly extracting purified benzoylurea pesticide residues from fruits and vegetables, and relates to the technical field of food detection. The detection method comprises the following steps of 1 extracting, wherein a homogeneous fruit and vegetable sample is weighed and put into a centrifuge tube, extraction is conducted by adding acetonitrile, then sodium chloride and magnesium sulfate are added, and supernatant liquid is obtained; 2 purifying, wherein the supernatant liquid is taken to be transferred into a centrifuge tube containing C18 and a tungsten disulfide nanometer material to be purified and then filtered with a 0.22-micrometer organic micropore filtering membrane to obtain purified liquid; and 3 measuring. According to the detection method,extraction is conducted by adopting the organic solvent acetonitrile, dewatering is conducted by adopting sodium chloride and magnesium sulfate, purifying is conducted by adopting C18 and the tungstendisulfide nanometer material, a large number of pigments in the fruits and vegetables or proteins in the plant source sample can be effectively removed, and then the purposes of reducing chromatographic analysis interference and improving the measuring accuracy are achieved.

Description

technical field [0001] The invention relates to the technical field of food detection, in particular to a method for rapidly extracting and purifying benzoylurea pesticide residues from fruits and vegetables. Background technique [0002] Benzoylurea insecticides, the main ingredient is benzoylurea compounds (BU), which are insect growth regulators (IGRs) that can inhibit the synthesis of chitin in target pests and cause their death or sterility. Known as the third-generation insecticide or new insect control agent. Due to its unique mechanism of action, high environmental safety, broad-spectrum and high-efficiency insecticidal activity and other attractive characteristics, at present, benzoyl urea compounds have become The creation of new pesticides is an active field, which has attracted people's attention and been widely used. [0003] Even though powerful techniques have been applied to pesticide detection in modern times, direct analysis of pesticides is difficult due ...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/14
CPCG01N30/06G01N30/14G01N2030/146
Inventor 覃国新劳水兵莫仁甫周其峰杨玉霞何洁王海军韦宇宁罗丽红陈泳锨
Owner GUANGXI ZHUANG AUTONOMOUS REGION ACAD OF AGRI SCI
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