Method for determining residual quantity of prochloraz and metabolite thereof in cereal grains and application

A technology of prochloraz and metabolites, which is applied in the field of determination of prochloraz and its metabolites residues in grains, can solve the problem of ineffective removal of fat, etc., and achieve the effect of eliminating matrix effect, strong matrix effect and low cost

Pending Publication Date: 2022-04-12
江苏省理化测试中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, for the detection of residues of prochloraz and its metabolites in food, the interference of fat, protein and other substances cannot be effectively removed

Method used

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  • Method for determining residual quantity of prochloraz and metabolite thereof in cereal grains and application
  • Method for determining residual quantity of prochloraz and metabolite thereof in cereal grains and application
  • Method for determining residual quantity of prochloraz and metabolite thereof in cereal grains and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Embodiment 1: Determination of prochloraz and its metabolite residues in rice

[0055] (1) Extraction of samples: Weigh 5g (accurate to 0.01g) of rice powder that has been crushed and mixed through a 425μm standard mesh sieve into a 50mL stoppered centrifuge tube, add 10mL of experimental water, vortex and mix well, and then soak After 30 min, add 10 mL of 1% acetic acid acetonitrile, 1 g of sodium acetate, and 3 g of sodium chloride, cover the bottle cap, vibrate vigorously for 1 min, and sonicate for 10 min, then centrifuge at 4000 r / m for 3 min, and let it stand for purification;

[0056] (2) Purification of the sample: Take 5 mL of the above centrifuged supernatant in a 10 mL test tube, add 200 mg PSA and 150 mg C18, vortex for 1 minute, centrifuge, take 3 mL of the supernatant and purify it in a 10 mL test tube containing 1000 mg EMR purifier , vortex, and centrifuge to take the supernatant through a 0.22 μm organic filter membrane and bottle it for testing;

[00...

Embodiment 2

[0064] Example 2: Determination of prochloraz and its metabolite residues in corn

[0065] (1) Sample extraction: Weigh 5g (accurate to 0.01g) of corn flour that has been pulverized and mixed through a 425μm standard mesh sieve into a 50mL stoppered centrifuge tube, add 10mL of water, vortex and mix well, soak for 30min, add 10 mL of 1% acetic acid acetonitrile, 1 g of sodium acetate, and 3 g of sodium chloride were placed on the bottle, shaken vigorously for 1 min, ultrasonically 10 min, and centrifuged at 4500 r / m for 5 min.

[0066] (2) Purification of the sample: Take 3 mL of the above centrifuged supernatant in a 10 mL test tube, add 200 mg PSA and 150 mg C18, vortex for 1 minute, centrifuge, take 2 mL of the supernatant in a 10 mL test tube containing 1000 mg EMR purification agent Purify, vortex, and centrifuge to take the supernatant and pass it through a 0.22 μm organic filter membrane before bottling;

[0067] (3) The preparation of matrix mixed standard series workin...

Embodiment 3

[0074] The comparative experiment of embodiment 3 different extraction solvents

[0075] Purchase oat, wheat, rice, corn, and brown rice samples from the market, use acetone, acetonitrile, ethyl acetate, n-hexane, and 1% acetic acid acetonitrile as extraction solvents to extract the above samples, and then test, the processing and testing of the above samples All were carried out according to the operation steps in Example 1, except that the extraction solvent was replaced during the operation. The recoveries of 2,4,6-trichlorophenol and prochloraz in each sample under different extraction solvents are shown in Table 3.

[0076] The recoveries of samples under different extraction solvents in table 3

[0077]

[0078] It can be concluded from the data in the above table that in the embodiment of the present invention, the recovery efficiency of prochloraz and metabolites using 1% acetic acid acetonitrile as the extraction solvent is the highest, and the recovery result is ...

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Abstract

The invention provides a method for detecting the residual quantity of prochloraz and metabolites thereof in cereal grains, which utilizes a gas chromatography-triple quadrupole mass spectrometer for testing and specifically comprises the following steps: preparing a matrix mixed standard series working solution, extracting a sample, purifying a sample solution and detecting the sample on a machine. According to the method, the influence of factors such as the type of an extraction solvent, the type and dosage selection of a dispersive solid-phase extraction agent and the like on the extraction efficiency is investigated, and gas chromatography conditions and a triple quadrupole mass spectrometer are subjected to condition optimization. The method is simple, convenient and efficient to operate, low in reagent consumption, capable of rapidly meeting the requirement for high-flux sample treatment, capable of meeting the pesticide residue detection requirements on precision, accuracy and sensitivity and suitable for detecting the residual quantity of the prochloraz and the metabolite thereof in the oil-containing cereal grains.

Description

technical field [0001] The invention belongs to the field of analysis and testing, and in particular relates to a method and application for measuring the residual amount of prochloraz and its metabolites in grains. Background technique [0002] Prochloraz is a broad-spectrum fungicide, which can be used to prevent and control many diseases on the stems, leaves and ears of cereal crops, such as rice blast, powdery mildew, leaf spot and so on. Prochloraz will first degrade into N-propyl-N-[2-(2,4,6-trichlorophenoxy)ethyl]urea and N-formyl-N[2-(2, 4,6,-trichlorophenoxy)ethyl]urea, finally degraded into 2,4,6-trichlorophenol, see Figure 1. Prochloraz is a low-toxicity fungicide, but its final metabolites may have long-term adverse effects on the environment and humans. Therefore, it is very necessary to detect 2,4,6-trichlorophenol when detecting prochloraz. The prochloraz degradation process is as follows: [0003] [0004] Currently, gas chromatography (GC-ECD), liquid ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/16G01N30/60G01N30/30G01N30/32G01N30/34G01N30/72
Inventor 徐慧庄件兵高宏贾涛
Owner 江苏省理化测试中心
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