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Detection method for metabolite residues of carbadox and olaquindox in animal tissues

A technology of animal tissue and detection method, applied in measurement devices, instruments, scientific instruments, etc., can solve problems such as unsatisfactory sensitivity and accuracy, inability to meet residue limit requirements, etc., and achieve satisfactory sensitivity, accuracy, and low operating costs. Effect

Inactive Publication Date: 2017-05-10
SHIJIAZHUANG UNIVERSITY
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  • Abstract
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  • Claims
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Problems solved by technology

[0003] At present, there are reports and standards on the detection of carbadox and olaquindox metabolite residues in animal tissues, but their sensitivity and accuracy are not ideal, and they cannot meet the increasingly stringent residue limit requirements

Method used

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  • Detection method for metabolite residues of carbadox and olaquindox in animal tissues
  • Detection method for metabolite residues of carbadox and olaquindox in animal tissues
  • Detection method for metabolite residues of carbadox and olaquindox in animal tissues

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Embodiment Construction

[0033] The technical solution of the present invention will be described in detail below with specific examples.

[0034] 1. Sample preparation

[0035] Rabbit liver and chicken samples were purchased from the market and pulverized into uniform samples with a micro pulverizer for detection.

[0036] 2. Determination steps

[0037] Accurately weigh 5 g (accurate to 0.01 g) of animal tissue samples in a 50 mL centrifuge tube, add 100 µL internal standard working solution, add 15 mL metaphosphoric acid-methanol solution, homogenize for 2 min, and centrifuge for 10 min (10000 r / min ), transfer the supernatant to another 50 mL polypropylene centrifuge tube; add 10.0 mL metaphosphoric acid-methanol solution to the residue, repeat the above operation, combine the supernatant, add 15 mL ethyl acetate, and vortex to mix Homogenize for 2 minutes, centrifuge for 5 minutes (6000 r / min), take the upper ethyl acetate layer into a chicken heart bottle, add 15 mL of ethyl acetate, repeat th...

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Abstract

The invention discloses a detection method for metabolite residues of carbadox and olaquindox in animal tissues. The detection method comprises the following steps: adding internal standard working fluid in a sample, extracting the sample by using a metaphosphoric acid-methanol solution, adding ethyl acetate in an extracting solution to be extracted, separating upper-layer ethyl acetate layer, carrying out rotary evaporation until being dried, carrying out constant-volume dissolution on the residues by using a methanol-formic acid solution, filtering through a 0.22<mu>m filter membrane, and performing qualitative and / or quantitative detection by using a liquid chromatograph-tandem mass spectrometer. The detection method for the metabolite residues of carbadox and olaquindox in the animal tissues disclosed by the invention is simple in sample treatment method and low in operation cost, the determination low limit of quinoxaline-2-carboxylic acid and 3-dimethyl quinoxaline-2-carboxylic acid is 1 mu g / kg, quinoxaline-2-carboxylic acid and 3-dimethyl quinoxaline-2-carboxylic acid are in line with a linear relationship in the range of 2 ng / mL to 200 ng / mL, the linear correlation coefficient r is more than 0.99 and the average recovery rate is ranged from 82.71% to 121.09%, and RSD is ranged from 4.07% to 9.51% (n is equal to 6), thereby indicating that the accuracy and sensitivity of the method meet detecting demands.

Description

technical field [0001] The invention relates to the field of detection of drug residues, in particular to a detection method for residues of carbadox and olaquindox metabolites in animal tissues. Background technique [0002] Carbadox and olaquindox belong to quinoxaline compounds, which have antibacterial effect, and adding them to feed can improve the digestion and immunity of poultry and livestock, and promote their growth and development. However, both of them have potential mutagenic and carcinogenic effects, and their metabolites may also bring health risks. Therefore, many countries have listed carbadox and olaquindox as banned or restricted drugs for food animals. Because the original drugs of the two Metabolized rapidly in animal tissues, while the corresponding metabolites quinoxaline-2-carboxylic acid (QCA) and 3-methyl-quinoxaline-2-carboxylic acid (MQCA) are relatively stable, so these two Metabolites are targeted for residue analysis and monitoring. [0003] ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 王惠李中秋陈丁龙次立杰
Owner SHIJIAZHUANG UNIVERSITY
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