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Method for measuring fluoride ether bacteria amide residues in fruit and vegetable by GC-EI-MS

A technique of GC-EI-MS and Fluoribactin, which is applied in the field of determination of pesticide residues, achieves the effect of simple operation, high sensitivity and avoiding matrix interference

Inactive Publication Date: 2015-06-03
BEIJING TIMES HAODING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] So far, there have been no domestic and foreign reports on the detection method of fluoxetin residues in food and agricultural products. Gas chromatography-mass spectrometry (GC-EI-MS) equipped with an electron bombardment ionization source has great advantages in the analysis of 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, 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 spectrometry (GC-EI-MS) is used to detect pesticide residues in food and agricultural products. Therefore, gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) is established for qualitative and quantitative analysis of fluoxetin in vegetables and fruits. The detection method of residue is of great significance

Method used

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  • Method for measuring fluoride ether bacteria amide residues in fruit and vegetable by GC-EI-MS
  • Method for measuring fluoride ether bacteria amide residues in fruit and vegetable by GC-EI-MS
  • Method for measuring fluoride ether bacteria amide residues in fruit and vegetable by GC-EI-MS

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Example 1: Detection of fluoxetin 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, 300mg C 18 and 150mg PSA in a centrifuge tube, vortex for 1min, and centrifuge at 5000r / min for 5min. Take 4mL of supernatant in a nitrogen blowpipe, dry it with nitrogen at 40°C, add 1mL of acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue, vortex and mix evenly to pass through the membrane, then transfer it to an injection bottle for GC - EI-MS determination.

[0036] (2) Preparation of standard working solution

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

Embodiment 2

[0062] Example 2: Detection of fluoxetin residues in dehydrated green peppers

[0063] (1) Sample pretreatment

[0064] Weigh 2.0 g of fully mixed dehydrated green peppers into a 50 mL centrifuge tube, add 5 mL of water for resuscitation for 30 min, 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 2mL of water, vortexed for 1min, centrifuged at 7000r / min for 5min. After centrifugation, take 6mL of acetonitrile extract and transfer to a solution containing 900mg anhydrous magnesium sulfate, 300mg C 18 and 150mg PSA 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.

[0065...

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Abstract

The invention discloses a method for measuring fluoroether bacterial amide residues in fruit and vegetable by the GC-EI-MS (Gas Chromatography-Electron Bombardment Ion Source-Mass Spectrum). The method comprises the following steps: using acetonitrile or an acetonitrile solution containing 1% acetic acid to perform homogenization extraction on residual fluoroether bacterial amide in a sample, dispersing and purifying the extracting solution with the ethanediamine-N-propyl silane (PSA) and octadecyl silane bonded phase (C18) substrate, performing GC-EI-MS detection, and adopting a blank substrate solution without the pesticide to be measured to build a corrected standard curve, and using an external standard method to determine the quantity. According to the method, the average recovery rate is 93.5-99.0%, the average relative standard deviation (RSD) is 3.7-5.5%, and the detection limit is lower than 2.53 microgram / kg; the method has the advantages of being simple, convenient and quick to operate, high in sensitivity, good in repeatability, and accurate in qualitative and quantitative performance; the method can meet the technical requirement of uniform limit that the residual limit is 0.01 mg / kg, and provides a powerful technical support for food safety and export trade sound development in China.

Description

technical field [0001] The invention relates to a GC-EI-MS method for determining the residues of fluoxybactam in fruits and vegetables, more specifically, it uses gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) to qualitatively and quantitatively determine the residues in vegetables and fruits. The invention discloses a method for the content of residual fluoxybactam, which belongs to the technical field of determination of pesticide residues. Background technique [0002] Fluorobactylamide (LH-2010A) is a new type of fluorine-containing benzamide fungicide innovatively synthesized by Shandong United Pesticide Industry Co., Ltd. in 2010. The chemical name is: N-(3-chloro-5-(tri Fluoromethyl)pyridine-2-methyl)-2,3,5,6-tetrafluoro-4-methoxybenzamide, the structural formula is: [0003] [0004] The structural formula of fluoxetin contains 7 fluorine atoms. The C-F bond energy formed by fluorine atoms is much greater than the C-H bond, whic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 范昆郭庆龙
Owner BEIJING TIMES HAODING TECH
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