Method for analyzing residual antibiotics in beef

A technology of antibiotics and beef, which is applied in the direction of analyzing materials, material separation, measuring devices, etc., can solve the problems of prolonging the detection cycle, high detection limit and quantification limit, time-consuming and labor-intensive, etc., so as to avoid interference of detection results and detect The effect of lower limit and limit of quantitation and improved detection sensitivity

Active Publication Date: 2018-05-11
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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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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  • Method for analyzing residual antibiotics in beef
  • Method for analyzing residual antibiotics in beef
  • Method for analyzing residual antibiotics in beef

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Embodiment 1 provides a kind of method for analyzing residual antibiotic in beef, comprises the steps:

[0067] (1) Get a certain amount of beef samples to grind and homogenize;

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

[0069] (3) Take 20ml of the extract obtained in step (2) and add a demulsifier, shake and mix, separate the liquid, transfer the obtained clear liquid to a solid phase extraction column, rinse with 5ml of water and 5ml of methanol aqueous solution in turn, discard The effluent was dried under reduced pressure, eluted with 8ml ...

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 standard curve matched with the external standard matrix of the target compound.

[0089] The linear correlation coefficient obtained by the test for the josamycin standard substance is: 0.9180.

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

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

[0092] 3. Determination of recovery rate: Do standard recovery test at four concentration levels of 5, 10, 20 and 50 μg / kg.

[0093] The ave...

Embodiment 3

[0095] Embodiment 3 provides a kind of method for analyzing residual antibiotic in beef, and difference with embodiment 1 is that described antibiotic is erythromycin, roxithromycin, tylosin, kitasamycin, rotamycin , Spiramycin.

[0096] Performance Testing

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

[0098] The linear correlation coefficients of standard products of erythromycin, roxithromycin, tylosin, kitasamycin, rotamycin and spiramycin were 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 a signal-to-noise ratio of 3, and the quantification limit of the method is determined with a signal-to-noise ratio greater than or equal to 10.

[0100]The detection limits of erythromycin, roxithromycin, tylosin, ki...

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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 detection of veterinary drug residues, 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 that accumulate or store in cells, tissues or organs after administration of drugs to animals. In recent years, veterinary drugs, including drug 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 animal product quality. It has become a modern animal husbandry industry. Indispensable material basis, it is unrealistic to reduce or even cancel the use of pharmaceutical additives. However, the use of veterinary drugs will lead to the retention or accumulation of drugs in animals. Long-term consumption of animal foods with veterinary drug residues is equivalent t...

Claims

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Application Information

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Patent Type & Authority Applications(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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