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Method for detecting residual quantity of fipronil in livestock and poultry hair

A fipronil and residue technology is applied in the field of detecting the residue of fipronil in the hair of livestock and poultry, and achieves the thorough and sufficient effects of less sampling, high accuracy, and favorable cleaning.

Active Publication Date: 2019-09-20
INST OF AGRI PROD QUALITY SAFETY & STANDARD JIANGXI ACAD OF AGRI SCI
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Problems solved by technology

Therefore, research on the detection method of fipronil in livestock and poultry hair is of great significance to effectively supervise the illegal use of this type of drug, ensure the quality and safety of livestock and poultry products, and the health of consumers. Method for the detection of fipronil residues in livestock and poultry hair

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  • Method for detecting residual quantity of fipronil in livestock and poultry hair
  • Method for detecting residual quantity of fipronil in livestock and poultry hair
  • Method for detecting residual quantity of fipronil in livestock and poultry hair

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Embodiment 1

[0044]Instruments and equipment: 1290-6495 ultra-high performance liquid chromatography-electrospray tandem mass spectrometer (Agilent Corporation, USA); Milli-Q ultrapure water device (Millipore Corporation); N-EVAP112 nitrogen blowing instrument (Organomation Corporation, USA); MS205DU electronic analysis Balance (Mettler Toledo, Switzerland); GL-88B Vortex Mixer (Qilin Bell Instrument Manufacturing Company, Haimen City).

[0045] Reagent: fipronil standard: purity>98%, methanol: chromatographically pure; other reagents are analytically pure.

[0046] 1. Preparation of standard solution

[0047] Standard stock solution: Accurately weigh an appropriate amount of fipronil standard substance into a 10mL volumetric flask, dilute to volume with acetonitrile, prepare a 1.0mg / mL standard stock solution, and store at -20°C in the dark.

[0048] Standard intermediate solution: Take 1 mL of the above standard stock solution in a 10 mL volumetric flask, dilute with acetonitrile to obt...

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Abstract

The invention discloses a method for detecting the residual quantity of fipronil in livestock and poultry hair, which detects the residual quantity of fipronil in livestock and poultry hair by adopting ultra-high performance liquid chromatography-electrospray tandem mass spectrometry. The method concretely comprises the steps of: extracting residual fipronil in hair by using an acetonitrile solution containing 2% formic acid and water, performing vortex, ultrasonic treatment and centrifugation, then performing dispersion purification on an extracted solution by using a matrix of ethylenediamine-N-propylsilane and octadecylsilane, an performing detecting by adopting ultra-high performance liquid chromatography tandem mass spectrometry, wherein, the mobile phase A is an aqueous solution containing 5 mmol / L ammonium acetate, the mobile phase B is a methanol solution containing 5 mmol / L ammonium acetate, the flow rate is 0.3 mL / min, and the chromatographic column adopts a C18 column with the diameter of 1.8 [mu]m and the size of 2.1 mm*100 mm. The method overcomes the defects of difficult sampling, living body slaughtering requirement and the like, has high specificity, high sensitivity, short time consumption and low requirement on sample purification, and provides reliable technical support for quality safety supervision of livestock and poultry products.

Description

technical field [0001] The invention relates to a method for detecting fipronil residues in livestock and poultry hair, and specifically belongs to the technical field of pesticide residue detection. Background technique [0002] Fipronil is a broad-spectrum phenylpyrazole insecticide. It is mainly stomach-toxic to pests. Its mechanism of action is to hinder the chloride metabolism controlled by insect γ-aminobutyric acid, so it has a high insecticidal activity. Animal experiments have shown that eating animal foods containing high concentrations of fipronil residues (such as meat, eggs, milk, vegetables, etc.) can cause damage to the nervous system, liver, thyroid, and kidneys, and has carcinogenic, teratogenic, and mutagenic effects. role. EU law stipulates that fipronil shall not be used in the livestock and poultry breeding process of the human food industry chain. Announcement No. 1157 of the Ministry of Agriculture of my country stipulates that the sale and use of p...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 徐俊闵佳玲周瑶敏胡丽芳谢敏肖勇陈庆隆
Owner INST OF AGRI PROD QUALITY SAFETY & STANDARD JIANGXI ACAD OF AGRI SCI
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