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Method for measuring antibiotic in animal excretion

A technology of antibiotics, feces, applied in the field of analysis of trace pollutants in the environment

Inactive Publication Date: 2010-04-07
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Capillary electrophoresis and radioimmunoassay are also used for the determination of antibiotics in environmental samples, but this method is semi-quantitative and further confirmation is required by liquid chromatography tandem mass spectrometry

Method used

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  • Method for measuring antibiotic in animal excretion
  • Method for measuring antibiotic in animal excretion
  • Method for measuring antibiotic in animal excretion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The chicken manure of two intensive farming areas A and B in Tianjin was selected as the analysis object. The analysis method and effect are as follows:

[0041]Extraction process: Weigh 0.5g of freeze-dried chicken feces samples into a polytetrafluoroethylene extraction tank, add 15ml of 0.1M EDTA-McIlvaine buffer solution, microwave-assisted extraction at 40°C for 15min, and extract the suspension The solution was transferred to a centrifuge tube, and then the buffer solution was added to extract again, and the suspension extracted twice was transferred to the same centrifuge tube and refrigerated for 30 minutes;

[0042] Concentration and purification process: 15ml of distilled water, 10ml of methanol and 15ml of distilled water are sequentially passed through the solid phase extraction column. After centrifugation, the supernatant of chicken manure passed through the pretreated solid-phase extraction column, and then eluted the solid-phase extraction column with 10m...

Embodiment 2

[0047] The pig feces of two intensive breeding areas C and D in Tianjin were selected as the analysis objects. The analysis methods and results are as follows:

[0048] Extraction process: Weigh 0.5 g of freeze-dried pig feces samples into a polytetrafluoroethylene extraction tank, add 15 ml of formic acid-acidified acetonitrile (pH=4), and microwave-assisted extraction at 40 ° C for 15 min, and extract the obtained Transfer the suspension to a centrifuge tube, then re-add the buffer and extract again, and transfer the suspension extracted twice to the same centrifuge tube for refrigerated centrifugation for 30 minutes;

[0049] Concentration and purification process: 15ml of distilled water, 10ml of methanol and 15ml of distilled water are sequentially passed through the solid phase extraction column. When the centrifuged pig feces supernatant is blown to about 5ml by nitrogen, add 200ml of distilled water to dilute, then pass through the solid phase extraction column, and fi...

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Abstract

The invention belongs to the analysis field of trace pollutant in environment, in particular relates to a method for measuring antibiotic in animal excretion. In the method, EDTA-McIlvaine buffering solution and acetonitrile acidulated by formic acid are taken as extracting solution which is extracted by a microwave assisted extractor, and then the steps such as solid phase extraction cartridge, purification and concentration are carried out, finally, liquid chromatogram-mass spectra / mass spectra (LC-MS / MS) is utilized for analytic determination, thereby accurately and rapidly analyzing the antibiotic in animal excretion. The concrete analytic determination method is as follows: taking a given amount of frozen and dried excretion, putting the excretion into a polytetrafluoroethylene extracting tank, adding the EDTA-McIlvaine buffering solution and acetonitrile acidulated by formic acid into the extracting tank, utilizing the debugged microwave assisted extractor for extraction, and then carrying out solid phase extraction cartridge, concentration and purification after optimization, drying by nitrogen, fixing volume, and at last, utilizing regulated HPLC-MS / MS for accurate measurement. The measuring method of the invention is simple and rapid, and has the characteristics of high recovery rate, low detection limit, high sensitivity, matrix interference resistance and the like.

Description

【Technical field】 [0001] The invention belongs to the field of analysis of trace pollutants in the environment, in particular to a method for accurately and quickly determining antibiotics in livestock manure. 【Background technique】 [0002] In the animal husbandry industry, antibiotics have been used for the treatment and prevention of animal diseases for a long time, and the situation of weak supervision and blind abuse is very serious. Antibiotics are discharged into the environment in the form of feces and urine in the form of prototypes or their degradation products. Studies have shown that the concentration of oxytetracycline in feces is as high as 29mg / kg, that of aureomycin is 26mg / kg, and that of sulfamethazine is as high as 100mg / L. Incalculable impact on the environment. [0003] Antibiotics in feces can be extracted using inorganic solvents or organic solvents, wherein the inorganic solvent EDTA-McIlvaine buffer is widely used in the determination of antibiotics...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 胡献刚周启星罗义
Owner NANKAI UNIV
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