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A method for analyzing residual antibiotics in beef

A technology for antibiotics and beef, which is applied in the analysis of materials, material separation, instruments, etc., can solve the problems of prolonging the detection cycle, high detection limit and quantification limit, time-consuming and labor-intensive, etc., to avoid interference of detection results and detection limit and the effect of lower limit of quantitation and improved detection sensitivity

Active Publication Date: 2019-12-20
XINJIANG ACADEMY OF ANIMAL SCI QUALITY STANDARDS INST OF ANIMAL HUSBANDRY XINJIANG UYGUR AUTONOMOUS REGION SHEEP & WOOL CASHMERE QUALITY SAFETY SUPERVISION & INSPECTION CENT
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The current veterinary drug detection methods in my country are mainly based on the classification of veterinary drugs. These methods have exposed several defects: for example, the screening ability for non-testing items of veterinary drug residues is insufficient, and for different types of veterinary drug residues, its detection method There are differences, so that the detection of veterinary drug residues can only measure the specified types of veterinary drugs, but lacks the ability to screen for other types of non-detected veterinary drug residues in the sample, which makes food safety monitoring hidden dangers
Secondly, different pretreatment and detection methods are required for different veterinary drug residue detection items of the same sample, which not only prolongs the detection cycle, increases detection cost and difficulty, but also reduces work efficiency
Furthermore, the extraction and purification process of traditional veterinary drug detection methods is cumbersome, costly, and time-consuming, which is difficult to meet the purpose of large-scale sample determination
Moreover, when detecting the content of residual veterinary drugs in meat, due to the relatively strong interaction between some veterinary drugs and the meat matrix, the detection process has a greater impact on the detection of some veterinary drugs, resulting in deviations in the detection limit and quantitative limit of these drugs. High, for example, less mycin in beef, due to its special structure, is easily affected by beef matrix and solvents during the detection process, the detected result is lower than the actual content, and may affect the quality of other veterinary drugs Test Results

Method used

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  • A method for analyzing residual antibiotics in beef
  • A method for analyzing residual antibiotics in beef
  • A method for analyzing residual antibiotics in beef

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Embodiment 1 provides a method for analyzing residual antibiotics in beef, comprising the steps of:

[0067] (1) take a certain amount of beef samples for mincing and homogenization;

[0068] (2) Weigh 5.00g of the processed beef sample and place it in a 100ml centrifuge tube with a stopper, add 25ml of n-hexane, shake and homogenize for 30 minutes, then add 25ml of acetonitrile and 2g of surfactant, vortex for 3 minutes, centrifuge, remove Take the separated solution, add 25ml of acetonitrile and 2g of surfactant to the filter residue, vortex for 3 minutes, centrifuge, combine the acetonitrile extracts, concentrate and dilute to 50ml;

[0069] (3) Take 20ml of the extract obtained in step (2), add a demulsifier, shake and mix, and separate the liquid. The obtained clear liquid is transferred to a solid-phase extraction column, rinsed with 5ml of water and 5ml of methanol aqueous solution successively, and discarded. The effluent was dried under reduced pressure, elute...

Embodiment 2

[0086] Example 2 provides a method for analyzing residual antibiotics in beef, which is different from Example 1 in that the antibiotic is josamycin.

[0087] Performance Testing

[0088] 1. Linear correlation test: Quantitative calculation of the sample is performed according to the external standard matrix matching standard curve of the target compound.

[0089] The linear correlation coefficient of the standard josamycin obtained from the test is: 0.9180.

[0090] 2. Detection limit and quantification limit test: The detection limit of the method is calculated with the signal-to-noise ratio as 3, and the quantification limit of the method is determined with the signal-to-noise ratio greater than or equal to 10.

[0091] The detection limit of the standard josamycin obtained from the test was 4.9 μg / kg; the limit of quantification was 28 μg / kg.

[0092] 3. Determination of recovery rate: standard addition recovery test was performed at four concentration levels of 5, 10, 2...

Embodiment 3

[0095] Example 3 provides a method for analyzing residual antibiotics in beef, and the difference from Example 1 is that the antibiotics are erythromycin, roxithromycin, tylosin, guitarmycin, and rotamycin. , Spiramycin.

[0096] Performance Testing

[0097] 1. Linear correlation test: Quantitative calculation of the sample is performed according to the external standard matrix matching standard curve of the target compound.

[0098] The linear correlation coefficients of erythromycin, roxithromycin, tylosin, guitarmycin, roxithromycin, and spiramycin standard products obtained from the test are: 0.9672, 0.9505, 0.9699, 0.9990, 0.9988, and 0.9996, respectively.

[0099] 2. Detection limit and quantification limit test: The detection limit of the method is calculated with the signal-to-noise ratio as 3, and the quantification limit of the method is determined with the signal-to-noise ratio greater than or equal to 10.

[0100]The detection limits of erythromycin, roxithromyci...

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Abstract

The invention relates to the technical field of veterinary drug residue detection, in particular to a method for analyzing residual antibiotics in beef. The method at least comprises the steps that beef samples are subjected to pretreatment, extraction, purification and monitoring analysis, wherein the monitoring analysis is conducted by means of a chromatogram-mass spectrometry combined technology. In the extraction process, a surfactant is adopted for increasing a dissolution rate of the target antibiotics; in the purification process, a demulsifier is adopted for reducing an emulsificationrate of a system, matrices and other impurities are precipitated and removed, and the precision and sensitivity of the detection process are further improved.

Description

technical field [0001] The invention relates to the technical field of veterinary drug residue detection, in particular to a method for analyzing residual antibiotics in beef. Background technique [0002] Veterinary drug residues refer to drug prototypes, metabolites and drug impurities accumulated or stored in cells, tissues or organs after administration of drugs to animals. In recent years, veterinary drugs, including pharmaceutical additives, have been widely used in animal husbandry. They play a very significant role in reducing morbidity, mortality, promoting growth, improving feed utilization, and improving the quality of animal products. It has become a modern animal husbandry. An indispensable material basis, it is no longer realistic to reduce or even cancel the use of drug additives. However, the use of veterinary drugs will lead to the retention or accumulation of drugs in animals. Long-term consumption of animal food with veterinary drug residues is equivalent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 胡波高维明宫平魏佩玲邢巍婷吕雪峰
Owner XINJIANG ACADEMY OF ANIMAL SCI QUALITY STANDARDS INST OF ANIMAL HUSBANDRY XINJIANG UYGUR AUTONOMOUS REGION SHEEP & WOOL CASHMERE QUALITY SAFETY SUPERVISION & INSPECTION CENT
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