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A kind of LC-MS/MS determination method of Fluorethyroxystamide residues in fruits and vegetables

A kind of fluoxetine and LC-MS technology, which is applied in the field of LC-MS/MS determination of fluoxamid residues to achieve the effect of ensuring people's food safety, avoiding matrix interference, and having good repeatability

Active Publication Date: 2016-07-06
湖北景田农业科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] So far, there are no domestic and foreign reports on the detection method of fluoxetin residues in food and agricultural products. The use of LC-MS / MS to determine pesticide residues in food and agricultural products has the advantages of rapidity, simplicity, and high sensitivity. Therefore, it is simple, fast, and The LC-MS / MS detection method that is accurate, durable, and capable of accurate qualitative and quantitative analysis of fluoxystrobin residues in vegetables and fruits is of great significance

Method used

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  • A kind of LC-MS/MS determination method of Fluorethyroxystamide residues in fruits and vegetables
  • A kind of LC-MS/MS determination method of Fluorethyroxystamide residues in fruits and vegetables
  • A kind of LC-MS/MS determination method of Fluorethyroxystamide residues in fruits and vegetables

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1: Detection of fluoxetin residues in apples

[0039] (1) Sample pretreatment

[0040] 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 2mL of acetonitrile extract and transfer to a solution containing 300mg anhydrous magnesium sulfate, 100mgC 18 and 50mgPSA in a centrifuge tube, vortex for 1min, and centrifuge at 7000r / min for 5min. Take the supernatant and pass it through a 0.22 μm filter membrane, and wait for determination.

[0041] (2) Preparation of standard working solution

[0042] Accurately weigh an appropriate amount of standard product in a volumetric flask, dissolve it with acetonitrile, and dilute to obtain a 1000.0 μg / mL standard stock solution; pipette 1.0 mL of the standard stock solution into a 100 mL volume...

Embodiment 2

[0075] Example 2: Detection of fluoxetin residues in dehydrated green peppers

[0076] (1) Sample pretreatment

[0077] 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 2mL of acetonitrile extract and transfer to a solution containing 300mg anhydrous magnesium sulfate, 100mgC 18 and 50mgPSA in a centrifuge tube, vortex for 1min, and centrifuge at 7000r / min for 5min. After the supernatant was passed through a 0.22 μm filter membrane, it was determined by LC-MS / MS.

[0078] The preparation of the standard working solution, liquid chromatography-tandem mass spectrometry (LC-MS / MS) determination and qualitative identification procedures...

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Abstract

The invention discloses an LC-MS / MS (liquid chromatography-mass spectrometry / mass spectrometry) determination method of residues of fluoride ether bacterium amide in fruits and vegetables. 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 LC-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 92.0%-96.2%, the average relative standard deviation (RSD) is 4.0%-5.5%, the detection limit is lower than 0.16mu 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 invention relates to a LC-MS / MS method for determining the residues of fluoxetin in fruits and vegetables, more specifically, it uses liquid chromatography tandem mass spectrometry (LC-MS / MS) to qualitatively and quantitatively measure the residues in vegetables and fruits. The invention discloses a method for the content of bacteramide, which belongs to the technical field of measuring 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 崔淑华马惠刘润珠
Owner 湖北景田农业科技发展有限公司