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A method for detecting fipronil and its metabolites in poultry eggs

A technology for medium fipronil and metabolites, which is applied in the field of detecting fipronil and its metabolites in eggs, can solve problems such as poor results and no fipronil metabolites, and achieves the effect of eliminating errors

Active Publication Date: 2020-07-24
ZHOUSHAN INST FOR FOOD & DRUG CONTROL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the detection of samples, according to the existing method, the effect is not good, and this method is only for fipronil, and does not include fipronil metabolites (such as flupronil, fipronil sulfide, fipronil sulfone) , therefore, a more complete detection method is needed

Method used

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  • A method for detecting fipronil and its metabolites in poultry eggs
  • A method for detecting fipronil and its metabolites in poultry eggs
  • A method for detecting fipronil and its metabolites in poultry eggs

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1: the establishment of extraction method

[0050]1) Sample preparation

[0051] Crack the eggshells, and put the contents into a multifunctional wall-breaking cooking machine to crush them to make samples to be tested. Put it into an aliquot container and store it at -18°C for later use.

[0052] 2) Sample pretreatment

[0053] Determination of fipronil and its metabolites in poultry eggs according to the method in SN / T 1982-2007: Weigh 10.00g sample into a 100mL plastic centrifuge tube with stopper, add 10mL water, add 40mL acetonitrile accurately, and cover Shake vigorously for 10 minutes, then add 5 g of sodium chloride, shake vigorously for 10 minutes, and centrifuge at 3000 r / min for 10 minutes. Take 20 mL of the upper extract and transfer it to a 50 mL centrifuge tube with a stopper, add 10 mL of n-hexane, shake for 3 minutes, keep the layers, discard the upper n-hexane phase, and collect the lower acetonitrile phase into a 100 mL heart-shaped bottl...

Embodiment 2

[0074] Embodiment 2: inspection sample detection

[0075] The method established in Example 1 was used to measure the content of fipronil in 15 eggs and duck eggs, and it was found that the content of fipronil sulfone was detected in one of the egg samples. Blend in a food processor until thoroughly homogenized until liquid. Weigh 2.00g of the sample into a 50mL stoppered plastic centrifuge tube, add 10mL of extraction buffer, cover and vortex for 2 minutes. Add 30mL of absolute ethanol, shake vigorously for 5 minutes after capping, centrifuge at 4000r / min for 5min, and pour the supernatant into a 100mL chicken heart bottle. The sample liquid in the chicken heart bottle was evaporated under reduced pressure in a 51°C water bath to remove ethanol. After spinning, transfer the aqueous solution to another 50mL centrifuge tube, add 5mL acetonitrile to rinse the original chicken heart bottle, combine the washing liquid into the 50mL centrifuge tube, and repeat the operation once....

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Abstract

The invention provides a method for detecting fipronil and metabolite thereof in a poultry egg. An extracting buffering solution is subjected to optimization selection; after the fipronil and the metabolite thereof in an egg sample are extracted by the extracting buffering solution, the sample is purified by using ethyl alcohol. A sample liquid is refined and purified by a QuEchERS method after being concentrated and subjected to ethyl alcohol removal; the refined and purified sample liquid is determined by a Gas Chromatography-Triple Auadrupole Mass Spectrometry (GC-MS / MS) method. According to the method provided by the invention, a poultry egg sample can be detected effectively, and whether the poultry egg sample is polluted by a pesticide, namely, the fipronil, can be authenticated. Thedetecting method provided by the invention can meet requirements on determination of the fipronil and the metabolite thereof in the poultry egg. According to the research, a standard sample is addedinto a blank egg, and the treating process of the standard sample is consistent with that of a sample to be detected, so that errors caused by a matrix effect are eliminated.

Description

technical field [0001] The invention belongs to the technical field of food detection, and in particular relates to a method for detecting fipronil and its metabolites in poultry eggs. Background technique [0002] In July 2017, eggs exported from the Netherlands were first found to contain fipronil. The "poisonous eggs" incident broke out, fermented, and quickly spread to many European countries. A large number of eggs contaminated with the pesticide fipronil were removed from shelves. The problem hens were slaughtered, and the economic loss was heavy. Hong Kong, China also detected fipronil in two egg samples imported from the Netherlands. Since my country has not clearly stipulated the limit of fipronil in eggs, and has not stipulated the detection method of fipronil in eggs, the relevant government departments are of course unable to effectively evaluate the quality and safety of eggs in my country. It directly affects the real-time and in-depth understanding, control a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/12G01N30/14
CPCG01N30/02G01N30/06G01N30/12G01N30/14G01N2030/047G01N2030/062G01N2030/126
Inventor 祝世军吴益春郭海波李栋芳罗海军周勇鲁华王萍亚
Owner ZHOUSHAN INST FOR FOOD & DRUG CONTROL