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GC-EI-MS method for determining ametoctradin residues in fruits and vegetables

A technology of GC-EI-MS and fenflux, which is applied in the field of determination of pesticide residues, can solve the problems of high price, long system, few methods for the determination of fenflux residues, etc., and achieves easy operation. , good repeatability, and the effect of ensuring people's food safety

Inactive Publication Date: 2016-06-29
郭庆龙
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At this stage, there are few studies on the determination of oxamethazone residues. The detection methods reported are mainly the detection methods of oxamethazone residues in vegetables and fruits. These detection methods are all based on liquid chromatography tandem mass spectrometry (LC- MS / MS) is a detection method for the determination of oxamethazone residues in vegetables and fruits. The use of LC-MS / MS to determine pesticide residues in food and agricultural products has the advantages of rapidity, simplicity, and high sensitivity. However, due to its high price, many detection methods Institutions, enterprises or scientific research institutes are not equipped with this instrument or have a small number of units. Since different compounds are detected by LC-MS / MS, different mobile phases or chromatographic columns need to be used, which requires constant replacement of chromatographic columns, mobile phases and It takes a long time to balance the system, which restricts the application of LC-MS / MS to a certain extent
Gas chromatography-mass spectrometry (GC-EI-MS) equipped with electron bombardment ionization source has great advantages in analyzing pesticide residues in food and agricultural products. Since electron bombardment ionization source mass spectrometry is a universal detector, it can realize multi-residue analysis of hundreds of pesticides. It can be qualitative and quantitative at the same time, and the price is moderate. Therefore, various testing institutions and enterprises are equipped with gas chromatography-electron bombardment ion source-mass spectrometer (GC-EI-MS) to detect pesticide residues in food and agricultural products, but so far no See the report on the GC-EI-MS method for the detection of oxaflustrobin residues in food and agricultural products, and the establishment of gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) for qualitative and quantitative analysis of grains and animal-derived foods It is of great significance to detect the residual amount of pyraclostrobin in

Method used

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  • GC-EI-MS method for determining ametoctradin residues in fruits and vegetables
  • GC-EI-MS method for determining ametoctradin residues in fruits and vegetables
  • GC-EI-MS method for determining ametoctradin residues in fruits and vegetables

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Example 1: Detection of oxamethoxam residues in apples

[0034] (1) Sample pretreatment

[0035] Weigh 10.0 g of well-mixed apples into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile, homogeneously extract for 1 min, add 3 g of anhydrous magnesium sulfate and 2 g of sodium chloride, vortex for 1 min, and centrifuge at 7000 r / min for 5 min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mgC 18 and 150mgPSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take 4 mL of the supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix evenly, pass through the membrane, and transfer it to the sample bottle for GC- EI-MS determination.

[0036] (2) Preparation of standard working solution

[0037] Accurately weigh 25±0.1mg of the standard produc...

Embodiment 2

[0063] Example 2: Detection of oxamethazone residues in cucumber

[0064] (1) Sample pretreatment

[0065] Weigh 10.0 g of well-mixed cucumber into a 50 mL centrifuge tube, accurately add 20 mL of acetonitrile solution containing 1% acetic acid, extract homogeneously for 1 min, add 3 g of anhydrous magnesium sulfate, 2 g of sodium acetate and 2 mL of water, vortex for 1 min, Centrifuge at 7000r / min for 5min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mgC 18 and 150mgPSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take 4mL of the supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix well, then transfer it to an injection bottle for GC-EI - MS determination.

[0066] (2) Preparation of standard working solution

[0067] Dilute the 1000 μg / mL s...

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Abstract

The invention discloses a GC‑EI‑MS method for determining the residues of oxamethanil in fruits and vegetables. Acetonitrile or an acetonitrile solution containing 1% acetic acid is used to homogeneously extract the residual oxamethanil in the sample, and the extract is passed through ethyl alcohol. Diamine-N-propylsilane (PSA) and octadecylsilane bonded phase (C 18 ) After the matrix is ​​dispersed and purified, it is detected by gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS), and the calibration standard working curve is established by using a blank matrix solution without the pesticide to be tested, and quantified by the external standard method. The average recovery rate of this method is 88.4%-91.6%, the average relative standard deviation (RSD) is 4.6%-7.9%, and the detection limit is lower than 6.10 μg / kg. The advantages of quantitative accuracy. It can meet the technical requirements of the United States, the European Union, Japan and other countries for corresponding product safety testing, and provide strong technical support for ensuring the food safety of our people and the healthy development of foreign export trade.

Description

technical field [0001] The present invention relates to a kind of GC-EI-MS method for measuring the residue of oxamethoxam in fruits and vegetables, more specifically, adopt gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) to qualitatively and quantitatively measure vegetables and fruits The invention relates to a method for the content of oxamethoxam residues in pesticides, which belongs to the technical field of determination of pesticide residues. Background technique [0002] Ametoctradin (Ametoctradin) is a new type of fungicide developed by BASF. a] pyrimidine-7-amine, the chemical formula is C15H25N5, and the structural formula is: [0003] [0004] Ametoctradin belongs to the class of s-triazolopyrimidines. It functions as a mitochondrial respiration inhibitor and can prevent and control oomycete fungal diseases, such as downy mildew and various diseases. Ametoctradin was first approved or approved in the European Union and South A...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 郭庆龙
Owner 郭庆龙
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