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Method for determining residual amount of fluoride ether bacterium amide in vegetables and fruits

A technique for the determination of Fluorbactyramide and its determination method, which is applied in the field of determination of Fluorbactyl amide residues, to achieve the effects of ensuring people's food safety, avoiding matrix interference, and good repeatability

Active Publication Date: 2015-05-27
广东南派食品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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-NCI-MS) equipped with a negative chemical ionization source has great advantages in the analysis of pesticide residues in food and agricultural products. Negative chemical ion source (NCI source) is called the "soft ionization source" of mass spectrometry. It has high selectivity and high sensitivity for analytes containing electronegative groups. Due to its strong characteristics, matrix interference Rarely, the qualitative and quantitative analysis of the target can be carried out very accurately

Method used

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  • Method for determining residual amount of fluoride ether bacterium amide in vegetables and fruits
  • Method for determining residual amount of fluoride ether bacterium amide in vegetables and fruits
  • Method for determining residual amount of fluoride ether bacterium amide in vegetables and fruits

Examples

Experimental program
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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, extract homogeneously 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 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- NCI-MS assay.

[0036] (2) Preparation of standard working solution

[0037]Accurately weigh 25±0.1mg of the standard product in a...

Embodiment 2

[0063] Example 2: Detection of fluoxetin residues in dehydrated green peppers

[0064] (1) Sample pretreatment

[0065] 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 the sample bottle to wait for GC-NCI - MS determination. ...

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Abstract

The invention discloses a method for determining residual amount of fluoride ether bacterium amide in vegetables and fruits. The method comprises the following steps: homogenizing and extracting residual fluoride ether bacterium amide in a sample with acetonitrile or an acetonitrile solution containing 1% of acetic acid, performing dispersion and purification on an extraction solution with a matrix of ethylenediamine-N-propylsilane (PSA) and octadecylsilane bonded phase (C18), then performing gas chromatography-negative chemical ionization-mass spectrometry (GC-NCI-MS) detection, establishing a standard curve for correction by adopting a blank matrix solution without a pesticide to be detected, and quantifying by an external standard method. According to the method, the average recovery rate is 93.0%-97.1%, the average relative standard deviation (RSD) is 4.1%-6.2%, the detection limit is lower than 2.13mu g / kg, and the method has the advantages of simplicity and convenience in operation, high speed, high sensitivity, good repeatability and accurate qualitative and quantitative properties. According to the method, the technical requirement of 'being standard without exceptions' of the residual limit of 0.01mg / kg can be met, and a powerful technical support is provided for ensuring food safety of people in China and health development of export trades.

Description

technical field [0001] The present invention relates to a method for determining the residual amount of fluoxetin in vegetables and fruits, more specifically, it adopts gas chromatography-negative chemical ion source-mass spectrometry (GC-NCI-MS) to qualitatively and quantitatively measure the residual amount of fluoxetin in vegetables and fruits. The invention discloses a method for the content of fluoxetin, belonging 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,...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 崔淑华
Owner 广东南派食品有限公司
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