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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  • Summary
  • 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 sulfo

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

Example Embodiment

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

[0024] ⑴ Preparation of samples

[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 a 0.45μm filter membrane into the sample bottle for online solid phase extraction-high resolution liquid chromatography-mass spectrometer determination.

[0026] ⑵The gradient elution conditions of the online solid phase extraction column are shown in Table 1. The required solid phase extraction column is C18 or HLB column.

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

[0028]

[0029] ⑶ The chromatographic separation conditions of the high performance liquid chromatography-high resolution mass spectrometer are shown in Table 2. The analytical column...

Example Embodiment

[0036] Example 2

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

[0038] To determine whether there is a certain antibiotic in a sample, the following conditions must be met: the retention time of the chromatographic peak of the sample and the retention time of the standard product does not exceed ±2.5%; the deviation of the accurate mas...

Example Embodiment

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

[0042] The pasteurized milk was used as a negative control substance to detect antibiotic residues in pasteurized milk and organic milk.

[0043] Follow the methods below to treat pasteurized milk and organic milk separately.

[0044] Accurately weigh 1.00g (±0.01g) 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 1mol / L phosphate buffer solution to control the pH of the solution The value is 4.5. After centrifugal filtration, pass a 0.45μm filter membrane into the sample bottle for online solid phase extraction-high resolution liquid chromatography-mass spectrometer determination. On-line solid phase extraction and analytical chromatographic conditions are shown in Table 2 and Table 3. The recovery rates of the analyzed negative samples of pasteurized milk and organic milk are shown in Table 4.

[0045] Table 4 Standard a...

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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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