A method for rapid determination of sulfonamide antibiotic residues in animal muscle tissue based on magnetic separation

A technology for rapid determination of animal muscle, applied in the field of sulfonamide antibiotic residues, can solve the problems of complex sample preparation methods, and achieve the effects of low cost, high sensitivity, and simple pretreatment

Active Publication Date: 2018-09-25
CHINESE ACAD OF FISHERY SCI
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although there are detection methods such as high performance liquid chromatography (HPLC) and high performance liquid chromatography triple quadrupole tandem mass spectrometry (HPLC-MS/MS) for the analysis of sulfonamide antibiotics in animals, due to the interference of fat and pro

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  • A method for rapid determination of sulfonamide antibiotic residues in animal muscle tissue based on magnetic separation
  • A method for rapid determination of sulfonamide antibiotic residues in animal muscle tissue based on magnetic separation

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[0018] Example 1: 1. Preparation of fish body samples: carp tissues were homogenized and stored in a refrigerator at -20°C;

[0019] 2. Extraction: Melt the surimi at room temperature, weigh 2g sample into a 50mL centrifuge tube with a lid, add 5mL mixed solution to fully infiltrate, vortex and mix; add Fe 3 O 4 Magnetic material mixture (consisting of 2g anhydrous magnesium sulfate, 0.5g sodium chloride and 100mg Fe 3 O 4 Magnetic particle composition), vortex and mix immediately to prevent anhydrous magnesium sulfate from agglomerating, and quickly separate under the action of an external magnet;

[0020] 3. Purification: Pipette 1mL of the sample extract supernatant into a 5mL centrifuge tube, concentrate by nitrogen blowing, add 1mL 1‰ formic acid solution to dissolve the residue, transfer the solution to a 5mL centrifuge tube containing 1mL n-hexane, vortex and shake After centrifugation, the upper n-hexane phase was discarded, the lower clear liquid was sucked and filtered thr...

Example Embodiment

[0022] Example 2: Add standard samples of sulfonamide antibiotics at three levels of 0.1, 0.25, and 0.5 mg / kg to blank fish samples, extract and purify the samples, calculate the recovery rate, and repeat 5 times.

[0023] The recovery rate of standard addition for carp muscle is as follows:

[0024]

[0025]

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Abstract

Relating to the technical field of physicochemical detection of drug residue in animals, the invention discloses a magnetic separation based method for rapidly determining residual amount of sulfonamide antibiotics in animal muscle tissue. The method includes extraction of an animal muscle sample with acidified acetonitrile, rapid phase separation of Fe3O4 magnetic particles, removal of fat from supernatant with n-hexane, and determination of sulfonamide compound content by HPLC-MS/MS analysis. The specific steps include: preparation: conducting animal dissection, homogenizing, and cryopreservation in a refrigerator at -20DEG C; extraction; purification: absorbing the subnatant and performing filtering with a 0.22micrometer organic phase filter membrane, then conducting HPLC-MS/MS analysis. The method provided by the invention overcomes the disadvantages of multiple steps and long time in the pretreatment process in the prior art. The method provided by the invention achieves mixed solution extraction, rapid phase separation of magnetic separation, and n-hexane purification, and has the advantages of simple pretreatment, high efficiency, solvent saving, high sensitivity and low cost.

Description

Technical field: [0001] The invention relates to the technical field of physical and chemical detection of drug residues in animals, in particular to a method based on magnetic separation to quickly determine the amount of sulfonamide antibiotic residues in animal muscle tissues. Background technique: [0002] With the continuous improvement of people's living standards, the consumption of animal-derived foods is increasing. In order to meet the ever-increasing consumer demand and increase the output of animal breeding, people add a lot of forbidden and restricted drugs in their breeding process to ensure their survival rate. The drugs involved in the breeding process will accumulate and concentrate in the organism through the food chain and eventually be transmitted to the human body, which brings potential harm to human food safety. Sulfonamide antibiotics have been widely used in the breeding of various animals such as aquatic products due to their broad-spectrum, high-effici...

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Application Information

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IPC IPC(8): G01N30/14
Inventor 李晋成
Owner CHINESE ACAD OF FISHERY SCI
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