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ECD determination method for residual quantity of N-(3-chloro-5-(trichloromethyl)pyridyl-2-methyl)-2,3,5,6-tetrafluoro-4-methoxybenzamide in vegetables and fruits

A technology of fluoxyrhidramide and fluneroxobyramide, which is applied in the field of ECD determination of fluoxyroxybactamide residues, to avoid matrix interference, ensure people's food safety, and easy to operate

Inactive Publication Date: 2015-06-03
河北德诺商品检测技术服务有限公司
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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 fluoxyrhebstramide residues in food and agricultural products. Fluoxyroxybactam molecules contain 7 fluorine and 1 chlorine atom, which are electronegative compounds, and can be captured by gas chromatography. The detector has good anti-interference ability, good selectivity and high sensitivity to analyze its residues. Therefore, a gas chromatography-electron capture detector (GC-ECD) was established to analyze the residues of fluoxetin in vegetables and fruits. The detection method is of great significance

Method used

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  • ECD determination method for residual quantity of N-(3-chloro-5-(trichloromethyl)pyridyl-2-methyl)-2,3,5,6-tetrafluoro-4-methoxybenzamide in vegetables and fruits
  • ECD determination method for residual quantity of N-(3-chloro-5-(trichloromethyl)pyridyl-2-methyl)-2,3,5,6-tetrafluoro-4-methoxybenzamide in vegetables and fruits
  • ECD determination method for residual quantity of N-(3-chloro-5-(trichloromethyl)pyridyl-2-methyl)-2,3,5,6-tetrafluoro-4-methoxybenzamide in vegetables and fruits

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1: Detection of fluoxetin residues in apples

[0032] (1) Sample pretreatment

[0033] 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 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- ECD assay.

[0034] (2) Preparation of standard working solution

[0035] Accurately weigh 25±0.1mg of the standard product in a 2...

Embodiment 2

[0054] Example 2: Detection of fluoxetin residues in dehydrated green peppers

[0055] (1) Sample pretreatment

[0056] 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 and dry it with nitrogen at 40°C. Add acetone / n-hexane mixed solvent with a volume ratio of 1 / 1 to dissolve the residue. Determination.

[0057] (2) Preparation of standard working solution

[0058] Dilute the 10ng / ...

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Abstract

The invention discloses an ECD determination method for residual quantity of N-(3-chloro-5-(trichloromethyl)pyridyl-2-methyl)-2,3,5,6-tetrafluoro-4-methoxybenzamide in vegetables and fruits. The ECD determination method comprises the following steps: homogenizing by using acetonitrile or an acetonitrile solution containing 1% acetic acid to extract residual desflurane bacteria amide in a sample; after dispersing and purifying an extract by using ethidene diamine-N-propylsilane (PSA) and octadecylsilane bonded phase (C18) matrix, determining by using a gas chromatography-electron capture detector (GC-ECD); quantifying by an external standard method. By the ECD determination method, the average recycling rate is 93.3-98.3%, the average relative standard deviation (RSD) is 4.1-6.5%, and the determination limit is lower than 3.16 [mu]g / kg; the ECD determination method has the advantages of simple, convenient and rapid operation, high sensitivity, good repeatability and accurate quantification; by the ECD determination method, a technical requirement on a uniform residue limit of 0.01mg / kg can be met; a powerful technical support is provided for guaranteeing food safety of people in China and healthy development of export trade.

Description

technical field [0001] The invention relates to an ECD method for determining the residual amount of fluotesoblast in vegetables and fruits, more specifically, a gas chromatography-electron capture detector (GC-ECD) is used to measure the content of fluotesoblast in vegetables and fruits The method 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, which significantly increases the stability and physiological activity of organic fluorine compounds. Fluorine-co...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14
Inventor 李瑞娟郭庆龙
Owner 河北德诺商品检测技术服务有限公司
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