GC-EI-MS measurement method for fluoride ether bacteria amide residues

A technology of GC-EI-MS and fluoxybactam, which is applied in the field of GC-EI-MS determination of fluoxibactil residues, achieves the effects of avoiding matrix interference, ensuring people's food safety, and easy operation

Active Publication Date: 2015-06-03
郭庆龙
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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-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 enterp

Method used

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  • GC-EI-MS measurement method for fluoride ether bacteria amide residues
  • GC-EI-MS measurement method for fluoride ether bacteria amide residues
  • GC-EI-MS measurement method for fluoride ether bacteria amide residues

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Detection of Fluorapyramide Residues in Pork

[0034] (1) Sample pretreatment

[0035] extract

[0036] Weigh 5g of fully mixed pork sample into a 50mL centrifuge tube, add 5mL of water to mix, let stand for 30min, accurately add 20mL of acetonitrile, extract homogeneously for 2min, add 3g of anhydrous magnesium sulfate and 2g of sodium chloride, and vortex for 1min , 7000r / min centrifugal 5min. After centrifugation, take 8 mL of the acetonitrile extract at 40°C for rotary steaming or nitrogen blowing to about 1 mL for purification.

[0037] purify

[0038] Pre-wash C with 5 mL of acetonitrile 18 / PSA solid phase extraction column, when the liquid level reaches the top of the adsorbent, transfer the above extraction solution into the column, wash the test tube with 2mL acetonitrile, and transfer the washing liquid into the SPE column, when the solution reaches the top of the adsorbent, add Add 4mL of acetonitrile to the column for elution, all the eluate...

Embodiment 2

[0064] Example 2: Detection of Fluorapyramide Residues in Rice

[0065] (1) Sample pretreatment

[0066] extract

[0067] Weigh 5g of rice sample (ground into flour) that has been thoroughly mixed into a 50mL centrifuge tube, add 20mL of water to resuscitate for 30min, then accurately add 20mL of acetonitrile solution containing 1% acetic acid, shake and extract for 20min, ultrasonically extract for 5min, add 3g of anhydrous Magnesium sulfate and 2g sodium acetate, after vortexing for 1min, centrifuge at 7000r / min for 5min. After centrifugation, take 8mL of the extract solution at 40°C by rotary steaming or blowing with nitrogen until it is nearly dry, add 1mL of acetonitrile and vortex, and wait for purification.

[0068] purify

[0069] Pre-wash C with 5 mL of acetonitrile 18 / PSA solid phase extraction column, when the liquid level reaches the top of the adsorbent, transfer the above extraction solution into the column, wash the test tube with 2mL acetonitrile, and tran...

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Abstract

The invention discloses a GC-EI-MS measurement method for fluoride ether bacteria amide residues. The method is mainly used for measuring the content of fluoride ether bacteria amide remaining in a complex matrix food and agricultural products such as cereal grains and animal derived food. The method comprises the following steps: extracting fluoride ether bacteria amide remaining in a sample in a homogenization manner by virtue of acetonitrile or an acetonitrile solution containing 1 percent of acetic acid, performing purification and concentration by virtue of a C18/PSA solid-phase extraction column, performing GC-EI-MS detection, establishing a corrected standard curve by adopting a vehicle solution free of a pesticide to be measured, and measuring the fluoride ether bacteria amide residues according to an external standard method. According to the method, the average recovery rate is 82.5 to 87.4 percent, the average relative standard deviation (RSD) is 4.4 to 6.4 percent, the detection limit is lower than 0.56[mu]g/kg, the method has the advantages of convenience and high speed in operation, good impurity removal effects, high sensitivity, high repeatability and accurate qualification and quantification, the technical requirement of uniform limit of 0.01mg/kg maximum residue limit can be met, and powerful technical support can be provided for ensuring the food safety of Chinese people and the healthy development of foreign export trade.

Description

technical field [0001] The present invention relates to a kind of GC-EI-MS determination method of fluoxetin residue, more specifically adopts gas chromatography-electron bombardment ion source-mass spectrometry (GC-EI-MS) to qualitatively and quantitatively measure grain, pork, The invention relates to a method for the content of fluoxetin residues in animal and plant-derived foods with complex matrices such as beef, mutton, chicken and other animal muscles and products, and 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 ...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 王杰郭庆龙
Owner 郭庆龙
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