Method for measuring residual quantities of four fluoroquinolone medicaments in animal food

A fluoroquinolone, animal food technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of long time, complicated operation steps, inability to automate, etc., and achieves a high degree of automation, high sensitivity, and simple processing. Effect

Inactive Publication Date: 2011-06-01
BEIJING JITIAN INSTR CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The operation steps are complicated, the

Method used

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  • Method for measuring residual quantities of four fluoroquinolone medicaments in animal food
  • Method for measuring residual quantities of four fluoroquinolone medicaments in animal food
  • Method for measuring residual quantities of four fluoroquinolone medicaments in animal food

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Embodiment 1

[0023] Eight whitefish samples were assayed, minced and stored at -18°C.

[0024] Sample pretreatment: Accurately weigh 1.0g of the thawed sample, place it in a mortar together with 1.5g of diatomaceous earth, grind until the sample has no obvious agglomeration, and place the sample in an 11mL extraction pool with a layer of fiber filter paper at the bottom , the extraction conditions are: use 8% by volume of ammonia acetonitrile as the extraction reagent, temperature 80°C, pressure 10MPa, heating for 5 minutes, static extraction for 5 minutes, cycle 1 time, rinsing volume of 60% of the extraction pool volume, rapid extraction with acetonitrile Rinse the sample and collect all the extracts by purging with nitrogen. Add 3ml of n-hexane and 1ml of diethyl ether to the obtained extract to remove lipid impurities, oscillate and statically separate the layers, discard the n-hexane-diethyl ether layer, repeat the operation twice, transfer the lower layer solution into a concentratio...

Embodiment 2

[0033] Ten beef samples were assayed, ground and stored at -18°C.

[0034] Sample pretreatment: Accurately weigh 1.0g of the thawed sample, place it in a mortar together with 1.5g of diatomaceous earth, grind until the sample has no obvious agglomeration, and place the sample in an 11mL extraction pool with a layer of fiber filter paper at the bottom , the extraction conditions are: use 8% by volume of ammonia acetonitrile as the extraction reagent, temperature 80°C, pressure 10MPa, heating for 5 minutes, static extraction for 5 minutes, cycle 1 time, rinsing volume of 60% of the extraction pool volume, rapid extraction with acetonitrile Rinse the sample and collect all the extracts by purging with nitrogen. Add 3ml of n-hexane and 1ml of diethyl ether to the obtained extract to remove lipid impurities, oscillate and statically separate the layers, discard the n-hexane-diethyl ether layer, repeat the operation twice, transfer the lower layer solution into a concentration bottl...

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Abstract

The invention discloses a method for measuring residual quantities of four fluoroquinolone medicaments in animal food, and relates to a liquid chromatography method for measuring the residual quantities of medicaments in animal food. The invention aims to provide a measuring method which is simple and quick in operation, high in automation degree, high in extraction efficiency, high in recovery rate and good in repeatability. The method for measuring the residual quantities of the four fluoroquinolone medicaments in the animal food comprises the following steps: sample preparation; sample pretreatment: accurately weighing a sample, mixing the sample and kieselguhr uniformly, transferring the mixture to an extraction tank, placing the extraction tank on a quick solvent extraction instrument to perform extraction, adding n-hexane and diethyl ether into the obtained extract to remove lipid impurities, performing violent oscillation, standing for demixing, removing the n-hexane-diethyl ether layer, repeatedly operating for two times, transferring the solution at the lower layer to a concentration bottle, rotationally steaming the solution in a rotary evaporator till the solution is dried, dissolving the dregs by using a mobile phase, and filtering the solution through a filter membrane for high performance liquid chromatography (HPLC) analysis; preparation of a standard solution; and efficient liquid chromatography measurement.

Description

technical field [0001] The invention relates to a method for determining veterinary drug residues in animal food, in particular to a method for simultaneously determining four fluorides of norfloxacin, ciprofloxacin, enrofloxacin and sarafloxacin in animal food. Method for the determination of quinolone residues. Background technique [0002] Fluoroquinolones are artificially synthesized antibacterial drugs, widely used in the prevention and treatment of bacterial diseases in aquatic animals, and also commonly used in the disinfection of ponds and water bodies, and sometimes as feed additives to promote animal growth, increase growth rate and output. However, the extensive and large-scale use of this drug in veterinary clinics will inevitably lead to its residue in animal food. If it is not controlled, it will seriously endanger human health; it will affect the export of animal food in my country and cause huge economic losses. Both my country and the European Union have es...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 赵萍于辉
Owner BEIJING JITIAN INSTR CO LTD
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