Detection method for antibiotic residue in milk

A detection method and antibiotic technology, applied in the detection field, can solve the problems of large consumption of consumables, aggravating the difficulty of milk antibiotic detection, and inability to realize automatic online connection, etc., and achieve the effect of improving accuracy

Inactive Publication Date: 2017-05-10
WUXI X RES PROD DESIGN & RES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, solid-phase extraction technology is the most widely used, but in the pretreatment of antibiotic residue detection in milk, solid-phase extraction technology generally has complex sample processing process, more exposure to toxic reagents, large consumption of consumables, and the need for additional nitrogen blowing. , poor reproducibility and the inability to realize fully automatic online connection
Especially drugs such as tetracyclines, because they combine with proteins or minerals to form a bound state, so it is more difficult to detect residual antibiotics in milk

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] A detection method for antibiotic residues in milk, (1) Measure 2-4mL of milk into a centrifuge tube, add 0.3g of demulsifier, after ultrasonic oscillation for 20 minutes, add 10mL of ethyl acetate, after the dispersion is uniform, add 10mL phosphate buffer solution, ultrasonic extraction for 10 minutes, after centrifugation, pipette 5mL supernatant, add 5mL phosphate buffer solution to mix, dissolve in sodium hydroxide or potassium hydroxide solution, then extract with toluene, take the upper layer solution as the standard solution; (2) Transfer the standard solution in step (1) to a solid-phase extraction column, rinse with 5mL water and 5mL methanol aqueous solution in sequence, discard the effluent, and dry it under reduced pressure, then use 5mL methanol Elution, collect the eluate. In a water bath at 50°C, blown to nearly dry with nitrogen gas, add 5mL of acetonitrile aqueous solution, mix on a vortex mixer, and pass through a microporous membrane to test the filt...

Embodiment 2

[0016] A detection method for antibiotic residues in milk, (1) Measure 4mL of milk into a centrifuge tube, add 0.5g of demulsifier, after ultrasonic oscillation for 30 minutes, add 20mL of ethyl acetate, after the dispersion is uniform, add 30mL of phosphoric acid Salt buffer solution, ultrasonic extraction for 20 minutes, after centrifugation, pipette 5mL supernatant, add 5mL phosphate buffer solution and mix well, dissolve in sodium hydroxide or potassium hydroxide solution, then extract with toluene, take the upper layer solution as Standard solution; (2) Transfer the standard solution in step (1) to a solid-phase extraction column, rinse with 5mL water and 5mL methanol aqueous solution in sequence, discard the effluent, dry it under reduced pressure, and elute with 5mL methanol , and collect the eluate. In a water bath at 50°C, blown to nearly dry with nitrogen gas, add 5mL of acetonitrile aqueous solution, mix on a vortex mixer, and pass through a microporous membrane to ...

Embodiment 3

[0018] A detection method for antibiotic residues in milk, (1) Measure 3mL of milk into a centrifuge tube, add 0.4g of demulsifier, after ultrasonic oscillation for 20 minutes, add 15mL of ethyl acetate, after the dispersion is even, add 20mL of phosphoric acid Salt buffer solution, ultrasonic extraction for 15 minutes, after centrifugation, pipette 5mL supernatant, add 5mL phosphate buffer solution to mix, dissolve in sodium hydroxide or potassium hydroxide solution, then extract with toluene, take the upper layer solution as Standard solution; (2) Transfer the standard solution in step (1) to a solid-phase extraction column, rinse with 5mL water and 5mL methanol aqueous solution in sequence, discard the effluent, dry it under reduced pressure, and elute with 5mL methanol , and collect the eluate. In a water bath at 50°C, blown to nearly dry with nitrogen gas, add 5mL of acetonitrile aqueous solution, mix on a vortex mixer, and pass through a microporous membrane to test the ...

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PUM

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Abstract

The invention discloses a detection method for antibiotic residue in milk. The detection method comprises the steps of (1) taking and adding 2 to 4mL of milk into a centrifuge tube, adding 0.3 to 0.5g of demulsifying agent, ultrasonically oscillating for 15 to 30min, then adding 10 to 20mL of ethyl acetate, uniformly dispersing, adding 10 to 30mL of phosphate buffered solution, ultrasonically extracting for 10 to 20min, centrifuging, then transferring 5mL of liquid supernatant, adding 5mL of phosphate buffered solution, uniformly mixing, then dissolving in a sodium hydroxide solution or a potassium hydroxide solution, adding methylbenzene for extraction and taking an upper solution as a standard solution; (2) transferring the standard solution in the step (1) to a solid phase extraction column, leaching by using 5mL of water and 5mL of methanol aqueous solution in sequence, discarding effluent, decompressing and pumping, then eluting with 5mL of methanol and collecting eluant. Blowing to nearly dry with nitrogen at 50 DEG C water bath, adding 5mL of acetonitrile water solution, mixing by a turbine mixer, and obtaining filter liquor through a microfiltration membrane for being detected; (3) adding the filter liquor into a gas chromatograph for detection. The detection method provided by the invention can effectively improve detection result accuracy and provides guarantee for food safety.

Description

technical field [0001] The invention relates to a detection method, in particular to a detection method for antibiotic residues in milk. Background technique [0002] Milk is rich in all nutrients needed by the human body except dietary fiber, and its high nutrition is irreplaceable by other foods. Fresh milk and dairy products have become an important part of people's (especially the elderly and children's) life food. In recent years, with the rapid development of my country's animal husbandry industry, milk production has increased significantly. In order to prevent the occurrence of diseases and treat diseases such as mastitis, farmers will add feed additives containing a certain proportion of antibiotics to cattle feed and drinking water. However, this will inevitably result in antibiotic residues in milk. If you drink milk containing antibiotics for a long time, the antibiotics in the milk can enter the human body through the food chain, which is undoubtedly equivalent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/60
CPCG01N30/06G01N30/6052
Inventor 蒋韦艳刘金杰吴敏芳徐静赵春城胡勇朱倩倩
Owner WUXI X RES PROD DESIGN & RES
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