Method for detecting veterinary drug residues in fish meat

A detection method and technology for veterinary drug residues are applied in the field of detection of veterinary drug residues in fish meat, and can solve problems such as inability to detect hormones and the like

Pending Publication Date: 2021-09-14
成都市食品药品检验研究院 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Patents CN107167539B and CN 107817306 B disclose methods for simultaneous determination of multiple veterinary drug residues in fish and aquatic products respectively,

Method used

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  • Method for detecting veterinary drug residues in fish meat
  • Method for detecting veterinary drug residues in fish meat
  • Method for detecting veterinary drug residues in fish meat

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Qualitative detection of veterinary drug residues in embodiment 1 fish

[0044] 1) Sample solution preparation:

[0045] Accurately weigh 2.00g (accurate to 0.01g) of homogenized fish sample, transfer it to a 50mL polypropylene (PP) centrifuge tube, slowly add 10mL of 80% volume fraction acetonitrile aqueous solution containing 0.2% formic acid, let it stand for 10min, and then add two Homogenize the ceramic particles, shake vigorously and vortex for 30min (2000r / min) to fully disperse the sample, centrifuge at 9500r / min for 5min, take 5mL of the supernatant, and pass through 6cc of 200mg at 1 drop / s PRiME HLB solid-phase extraction column, collect 4mL of the second half of the effluent and accurately measure 2mL, N 2 Blow dry under the hood, dilute 1mL of the initial mobile phase, pass through a 0.22μm polytetrafluoroethylene filter membrane to obtain the sample solution;

[0046] 2) Preparation of the reference substance solution: Accurately weigh 2 mg of each refe...

Embodiment 2

[0052] Example 2 Qualitative detection of veterinary drug residues in fish meat

[0053] 1) Sample solution preparation:

[0054] Accurately weigh 2.00g (accurate to 0.01g) of homogenized fish sample, transfer it to a 50mL polypropylene (PP) centrifuge tube, slowly add 10mL of 80% volume fraction acetonitrile aqueous solution containing 0.2% formic acid, let it stand for 10min, and then add two Homogenize the ceramic particles, shake vigorously and vortex for 30min (2000r / min) to fully disperse the sample, centrifuge at 9500r / min for 5min, take 5mL of the supernatant, and pass through 6cc of 200mg at 1 drop / s PRiME HLB solid-phase extraction column, collect 4mL of the second half of the effluent and accurately measure 2mL, N 2 Blow dry under the hood, dilute 1mL of the initial mobile phase, pass through a 0.22μm polytetrafluoroethylene filter membrane to obtain the sample solution;

[0055] 2) Preparation of the reference substance solution: Accurately weigh 2 mg of each re...

Embodiment 3

[0060] Quantitative detection of veterinary drug residues in embodiment 3 fish

[0061] a. Preparation of matrix solution: Accurately weigh 2.00g (accurate to 0.01g) homogenized fish sample without veterinary drugs, transfer it to a 50mL polypropylene (PP) centrifuge tube, slowly add 80% volume fraction containing 0.2% formic acid Acetonitrile aqueous solution 10mL, after standing for 10min, add two ceramic homogenizers, shake vigorously and vortex for 30min (2000r / min) to fully disperse the sample, centrifuge at 9500r / min for 5min, take 5mL supernatant, and Drops / s over 6cc 200mg PRiME HLB solid-phase extraction column, collect 4mL of the second half of the effluent and accurately measure 2mL, N 2 Blow dry under the hood, dilute 1mL of initial mobile phase, and pass through a 0.22μm polytetrafluoroethylene filter membrane to obtain matrix solution;

[0062] b. Preparation of reference substance solution: Accurately weigh 2 mg of each reference substance, dilute it with ace...

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Abstract

The invention discloses a method for detecting veterinary drug residues in fish meat, which comprises the following steps: (1) preparing a sample solution: taking and homogenizing fish meat, adding an acetonitrile aqueous solution containing formic acid, standing for 5-25 minutes, adding homogeneous protons, performing vortex oscillation for 20-40 minutes, centrifuging for 3-7 minutes, taking supernate, enabling the supernate to pass through a reversed-phase solid-phase extraction column, collecting effluent, blow-drying the effluent by N2 gas, adding an initial mobile phase, dissolving and filtering to obtain a test solution; and (2) detecting by adopting an ultra-high performance liquid chromatography-mass spectrometer. According to the method, through a specific sample pretreatment method and an instrument analysis method, veterinary drug residues cover mainstream veterinary drug types such as hormone and macrolide antibiotics and zeranol compounds, and the detection sample range is increased to bulk consumer fish species with complex matrixes such as turbots, mandarin fishes, snakeheaded fishes and grass carps; and the method is simple and rapid, low in cost, high in accuracy and good in stability.

Description

technical field [0001] The invention specifically relates to a method for detecting veterinary drug residues in fish meat. Background technique [0002] The main source of nutrients such as high-quality protein, fat and essential amino acids for human beings is one of the main food raw materials in people's three meals a day. With the continuous improvement of the living standards of Chinese residents, people's demand for fish consumption is also increasing. However, in the process of fish farming, production, transportation and sales, in order to prevent and control fish diseases, promote the rapid growth of fish and increase industrial income, there are phenomena of misuse or abuse of veterinary drugs. The excessive use of veterinary drugs not only directly affects food safety, but also indirectly affects the ecological environment and fishery trade. The safety of veterinary drugs in food has been highly valued by the government and the people. solved problem. [0003] T...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N27/622
CPCG01N30/02G01N30/06G01N30/72G01N27/622G01N2030/065
Inventor 郭添荣吴文林张崟万渝平叶梅张龙翼杜蕾马坚任昕李桃王勇
Owner 成都市食品药品检验研究院
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