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Method for detecting antibiotic residues in milk, and application thereof

A detection method and antibiotic technology, applied in the field of food safety and food safety detection, to achieve the effects of avoiding loss of analytes, strong selectivity, and improving detection efficiency and throughput

Inactive Publication Date: 2015-10-21
ANIMAL AND PLANT & FOOD DETECTION CENTER JIANGSU ENTRY EXIT INSPECTION AND QUARANTINE BUREAU
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a simple and rapid detection method for the current detection of antibiotic residues in milk, so that sulfonamides, quinolones, β-lactams, tetracyclines, and chloramphenicols in milk can be detected simultaneously A total of 33 veterinary drug residues in five categories

Method used

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  • Method for detecting antibiotic residues in milk, and application thereof
  • Method for detecting antibiotic residues in milk, and application thereof
  • Method for detecting antibiotic residues in milk, and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1. Detection of multiple antibiotic residues in pasteurized milk

[0024] ⑴Sample preparation

[0025] Accurately weigh 1.00g (±0.01g) of milk sample into a centrifuge tube, add 0.5ml of zinc acetate solution with a concentration of 1mol / L, vortex and mix well, then add 1ml of 1mol / L phosphate buffer solution to control the pH of the solution The value is 4.5. After centrifugal filtration, pass through a 0.45 μm filter membrane into a sampling bottle for determination by an online solid phase extraction-high resolution liquid chromatography-mass spectrometer.

[0026] (2) The gradient elution conditions of the online solid phase extraction column are shown in Table 1, and the required solid phase extraction column is a C18 or HLB column.

[0027] Table 1 Gradient conditions of online solid phase extraction

[0028]

[0029] (3) The chromatographic separation conditions of the high-performance liquid chromatography-high resolution mass spectrometer are shown...

Embodiment 2

[0037] On the basis of Example 1, further in this example, prepare standard working solutions with mass concentrations of 10, 50, 75, 100.0, and 200.0 ng / mL, and take the ratio of the peak area of ​​the standard solution to the area of ​​the internal standard as the ordinate , the solution concentration (ng / ml) is the abscissa, and the standard working curve is drawn. All compounds had a good linear relationship in the range of 10-200ng / mL, and the correlation coefficient (r) was greater than 0.99. Samples were quantified using a standard working curve. The response value of the drug in the sample solution should be within the linear range of the instrument.

[0038]To determine whether there is a certain antibiotic in the sample, the following conditions must be met: the retention time of the chromatographic peak that appears in the sample is no more than ±2.5% from the retention time of the standard; the deviation of the accurate mass number between the sample and the stand...

Embodiment 3

[0041] Example 3. Detection of multiple antibiotic residues in organic milk

[0042] Using pasteurized milk as a negative control, the antibiotic residues in pasteurized milk and organic milk were detected respectively.

[0043] Treat pasteurized milk and organic milk separately as follows.

[0044] Accurately weigh 1.00g (±0.01g) of milk sample into a centrifuge tube, add 0.5mL zinc acetate solution with a concentration of 1mol / L, vortex and mix well, then add 1mL of 1mol / L phosphate buffer solution to control the pH of the solution The value is 4.5. After centrifugal filtration, pass through a 0.45 μm filter membrane into a sampling bottle for determination by an online solid phase extraction-high resolution liquid chromatography-mass spectrometer. The online solid phase extraction and analysis chromatographic conditions are shown in Table 2 and Table 3. The recoveries for pasteurized milk and organic milk for negative samples analyzed are shown in Table 4.

[0045] Table...

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Abstract

The invention relates to a method for detecting antibiotic residues in milk, and an application thereof, and belongs to the field of food safety. The invention discloses an online solid phase extraction-high performance liquid chromatography-mass spectrometry detection method in order to solve the detection problem of antibiotic residues in milk. The method allows five types of 33 veterinary drug residues comprising sulfanilamides, quinolones, beta-lactams, tetracyclines and chloramphenicols in the milk to be simultaneously detected. Influences of various factors on the reservation and selectivity of various antibiotics are optimized, so the method has the characteristics of high sensitivity, high recovery rate, high stability and high precision. The detected antibiotics can be qualitatively and quantitatively determined according to the reservation time and accurate mass numbers. The amounts of samples and reagents required and used in the method are small, the detection speed is fast, all operation processes are completed within 15.5min, and cost reduction and operating risk mitigation of dairy product processing enterprises are guaranteed.

Description

technical field [0001] The invention relates to a method for monitoring antibiotic residues in milk and an application thereof, belonging to the field of food safety, in particular to the field of food safety detection. Background technique [0002] Milk is rich in all nutrients needed by the human body except dietary fiber, and its high nutrition is irreplaceable by other foods. Fresh milk and dairy products have become an important part of people's (especially the elderly and children's) life food. In recent years, with the rapid development of my country's animal husbandry industry, milk production has increased significantly. In order to prevent the occurrence of diseases and treat diseases such as mastitis, farmers will add feed additives containing a certain proportion of antibiotics to cattle feed and drinking water. However, this will inevitably result in antibiotic residues in milk. If you drink milk containing antibiotics for a long time, the antibiotics in the mi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 吴斌刘芸丁涛唐茂芝吴海文王茂华张睿沈崇钰陈国强
Owner ANIMAL AND PLANT & FOOD DETECTION CENTER JIANGSU ENTRY EXIT INSPECTION AND QUARANTINE BUREAU
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