GC-MS/MS (gas chromatography-mass spectrometry/mass spectrometry) determination method of residual amount of fluoride ether bacterium amide

The technology of a fluoxetamide and a determination method is applied in the field of GC-MS/MS determination of the residual amount of fluoxamid, which can solve complex problems and achieve the effects of simple operation, high sensitivity, and avoiding matrix interference.

Active Publication Date: 2015-05-27
崔淑华
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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. The use of gas chromatography-tandem mass spectrometry (GC-MS / MS) to analyze pesticide residues in food and agricultural products is fast, simple, sensitive, and selective. It can achieve multi-residue analysis of hundreds of pesticides. Since the matrix of food and agricultural products such as grains and animal-derived foods is relatively complex, it is necessary to establish a sample pretreatment method with good purification effect to meet the detection requirements. Therefore, the establishment of gas phase Chromatography-mass spectrometry (GC-MS / MS) is of great significance for the qualitative and quantitative analysis of fluoxetin residues in grains and animal-derived foods

Method used

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  • GC-MS/MS (gas chromatography-mass spectrometry/mass spectrometry) determination method of residual amount of fluoride ether bacterium amide
  • GC-MS/MS (gas chromatography-mass spectrometry/mass spectrometry) determination method of residual amount of fluoride ether bacterium amide
  • GC-MS/MS (gas chromatography-mass spectrometry/mass spectrometry) determination method of residual amount of fluoride ether bacterium amide

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. Take 8 mL of acetonitrile extract at 40°C for rotary steaming or nitrogen blowing to about 1 mL, and wait 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, receive all the eluent into th...

Embodiment 2

[0068] Example 2: Detection of Fluorapyramide Residues in Rice

[0069] (1) Sample pretreatment

[0070] extract

[0071] 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.

[0072] purify

[0073] 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-MS/MS (gas chromatography-mass spectrometry/mass spectrometry) determination method of residual amount of fluoride ether bacterium amide. The method is mainly used for determining the residual amount of fluoride ether bacterium amide in cereal grains, animal-derived foods and other complex matrix food agricultural products. 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 purification and concentration by a C18/PSA solid-phase extraction column, performing GC-MS/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 87.1%-93.8%, the average relative standard deviation (RSD) is 4.1%-5.2%, the detection limit is lower than 0.51mu g/kg, and the method has the advantages of simplicity and convenience in operation, high speed, good impurity removal effect, 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 invention relates to a GC-MS / MS method for determining the residual amount of fluoxetin, more specifically, it is a method for qualitatively and quantitatively measuring grain, pork, beef, mutton and chicken by using gas chromatography tandem mass spectrometry (GC-MS / MS). The invention relates to a method for the content of fluoxyroxybactamide residues in animal and plant-derived foods with complex matrices such as 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 en...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 崔淑华
Owner 崔淑华
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