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Method for detecting veterinary drug residues such as sulfonamides and quinolones in animal-derived foods

A technology for detecting quinolones and animals, which can be used in measuring devices, instruments, scientific instruments, etc., and can solve problems such as easy plugging of fillers and low recovery rates

Inactive Publication Date: 2017-07-28
NANJING UNIV OF FINANCE & ECONOMICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solid-phase extraction is often used to purify trace or trace substances. For complex matrices, there are disadvantages such as low recovery rate and easy plugging of packing materials.

Method used

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  • Method for detecting veterinary drug residues such as sulfonamides and quinolones in animal-derived foods
  • Method for detecting veterinary drug residues such as sulfonamides and quinolones in animal-derived foods
  • Method for detecting veterinary drug residues such as sulfonamides and quinolones in animal-derived foods

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take 0.5g pork in a 15ml centrifuge tube, add 2 and 10μg / kg two levels of 33 veterinary drug mixed standard solutions, add 2.00ml 1% formic acid acetonitrile, shake vigorously for 5min, and centrifuge at 4500rmp for 10min at room temperature; Add 2.00ml of n-hexane to the supernatant and shake for 2 minutes, let it stand for stratification, remove the upper n-hexane layer, and repeat degreasing once. The supernatant was diluted twice with water, then passed through a 0.22 μm filter membrane, and the spiked samples of each level were measured in parallel 3 times for liquid mass analysis.

Embodiment 2

[0020] Embodiment 2 typical curve and limit of detection

[0021] Take 0.5g of pork in a 15ml centrifuge tube, add 2.00ml of 1% formic acid acetonitrile, shake vigorously for 5min, and centrifuge at 4500rmp for 10min at room temperature; take the supernatant, add 2.00ml of n-hexane and shake for 2min, let stand for stratification, remove The upper n-hexane layer was degreased repeatedly. After concentrating to dryness, add 1.00ml of mixed standard solution to redissolve, vortex to mix, pass through 0.22μm filter membrane, prepare 3 levels of matrix-matched mixed standard solutions, and take the peak area (Y) of the quantifying ion of the target compound as the ordinate , The mass concentration (X, μg / L) is drawn as abscissa, and the correlation coefficient r is 0.99004~0.99995, and the linear relationship is good. The limit of detection (LOD) of the sample was determined by the quantitative ion signal-to-noise ratio S / N=3, and the lower limit of quantitation (LOQ) was defined...

Embodiment 3

[0025] Embodiment 3 recovery rate experiment

[0026] According to the method of Example 1, 33 kinds of veterinary drug mixed standard solutions were added to the blank pork sample, and the spiked samples were 2 and 10 μg / kg respectively, and the recovery test was carried out according to the above-mentioned pretreatment method and measurement conditions. Do 3 parallel measurements. The average recovery of each compound was 69.53%-120.80%, and the relative standard deviation (RSD) was 1.09%-9.98%, which met the requirements of multi-residue analysis.

[0027] Table 2 Pork sample spiked recovery and precision

[0028]

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PUM

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Abstract

The invention discloses a method for detecting veterinary drug residues such as sulfonamides and quinolones in animal-derived foods. The method is suitable for rapid detection of veterinary drug residues in animal-derived foods by high-resolution mass spectrometry and comprises (1) preparation of a standard solution, 2) sample pretreatment, and (3) liquid chromatography / mass spectrometry separation and detection. The method utilizes 1% formic acid solution of acetonitrile to extract and n-hexane to remove fat and is combined with high-resolution mass spectrometry for synchronously detecting 33 veterinary drug residues in the animal-derived foods. Compared with the prior art, the method is easy to operate, realizes accurate quantification and has a great significance for high-resolution mass spectrometry-based quantitative analysis of conventional drugs.

Description

technical field [0001] The invention relates to a method for detecting sulfonamide and quinolone veterinary drug residues in pork, belonging to the technical field of instrument detection. Background technique [0002] In the process of modern agricultural production, fish, chicken, pork and other animal-source foods are often used in the feeding process with a large amount of antibiotics in the feed to assist in the prevention and treatment of diseases. However, the abuse or inappropriate use of these drugs may cause potential harm to the human body. Therefore, the problem of veterinary drug residues has gradually become the social focus of people's general attention. [0003] The current veterinary drug pretreatment technologies mainly include: liquid-liquid extraction, solid-phase extraction and QuEChERS, etc. The liquid-liquid extraction method takes a long time to operate and uses more organic solvents that are harmful to the human body and the environment. Solid-pha...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 李彭王杰裴斐方勇胡秋辉刘琴
Owner NANJING UNIV OF FINANCE & ECONOMICS
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