Method for rapidly screening out cephalosporins drug residues from animal muscle tissue

A cephalosporin, animal muscle technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of inability to achieve the purpose of high-throughput screening of cephalosporins, inability to detect oil content, false positive test results, etc. Simple operation, high resolution and reproducible results

Active Publication Date: 2017-03-15
CHINESE ACAD OF INSPECTION & QUARANTINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Our research group has established LC-MS / MS detection technology for 22 cephalosporin residues in pork, but this method cannot detect beef and mutton samples with high fat content
In addition, although LC-MS / MS detection technology has improved the sensitivity and selectivity of the method, it still has the disadvantages of low resolution and prone to false positive detection results. The purpose of high-throughput screening of cephalosporins has brought certain hidden dangers to human health

Method used

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  • Method for rapidly screening out cephalosporins drug residues from animal muscle tissue
  • Method for rapidly screening out cephalosporins drug residues from animal muscle tissue
  • Method for rapidly screening out cephalosporins drug residues from animal muscle tissue

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The method for rapid screening of cephalosporin residues in animal muscle tissue provided by the present embodiment comprises the following steps:

[0037] Sample processing and detection analysis

[0038] (1) Extraction, crush the sample to be tested and place it in a centrifuge tube, add an extraction solvent, vortex and mix, extract by ultrasonic, and take the supernatant after centrifugation;

[0039] (2) purification, the centrifuged supernatant passes through the solid-phase extraction column, collects the effluent, and adds the eluent to the solid-phase extraction column for elution after the flow is exhausted, collects the eluent that flows out, and merges the collected effluent and The eluate was concentrated by nitrogen blowing, added acetonitrile to constant volume, and filtered the membrane, and the filtered liquid was injected into the ultra-high performance liquid chromatography-quadrupole-orbitrap mass spectrometry system for detection and analysis;

[0...

Embodiment 2

[0051] In order to improve the detection comprehensiveness and accuracy of the screening method provided in this example, this example carried out a comparative analysis of different sample processing methods, and compared the ultra-high performance liquid chromatography-quadrupole-orbitrap mass spectrometry The different experimental conditions of the system were compared and analyzed, and the screening method provided in this example was optimized, so that a comprehensive screening method for the above-mentioned cephalosporin compounds could be established.

[0052] In order to obtain the best separation effect, in this embodiment, the separation effects of five chromatographic columns and five mobile phases for cephalosporin compounds were comparatively studied, and the specific process is as follows.

[0053] The five chromatographic columns are Waters ACQUITY UPLC BEH Shield RP18 (1.7μm, 2.1×100mm), Waters ACQUITY UPLC BEH HILIC (1.7μm, 2.1×100mm), phenomenonex Kinetex F...

Embodiment 3

[0080] Based on the optimized conditions provided in Example 2, this example provides a preferred implementation of the rapid screening method for cephalosporin residues in animal muscle tissue, taking pork samples as an example to verify the reliability of the detection method provided in this example .

[0081] The optimized sample pretreatment process is as follows: Weigh 5.0±0.05g sample into a 50mL centrifuge tube, take 10mL acetonitrile-water (4:1; v / v) solution as the extraction solution, and extract the target substance from the crushed sample After centrifugation, take 2 mL of the supernatant and pass it through the PRiMEHLB solid-phase extraction column. After the flow is exhausted, collect the effluent, and add 2 mL of acetonitrile-water containing 0.1% formic acid (5:1; v / v) to the PRiMEHLB solid-phase extraction column. solution, and then collect the effluent, blow nitrogen to less than 1mL, take acetonitrile to 1mL, pass through a 0.2μm microporous filter membran...

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Abstract

The invention relates to a method for rapidly screening out cephalosporins drug residues from animal muscle tissue. The method comprises the following steps of performing sample processing and detection analysis, manufacturing a standard curve, and utilizing inspection data obtained in the sample processing and detection analysis process for calculating the concentration of a cephalosporins compound in a to-be-tested sample through the standard curve. According to the method, by means of an ultra-high performance liquid chromatography-quadrupole-track trap mass spectrum combination system, the technology for screening out cephalosporins drug residues from animal derived food is successfully built, and 44 cephalosporins drug residues can be screened out from the animal muscle tissue; in addition, the detection method is easy to implement, good in repeatability, high in analysis speed and high in resolution ratio, the resolution ratio is within 0.17-1.23 ppm, the recovery rate of all the 44 target objects is stable, the recovery rate is within 69.20-129.00%, and the method can be effectively used for screening out cephalosporins drug residues from the animal source food.

Description

technical field [0001] The invention relates to the technical field of drug residue detection, in particular to a rapid screening method for cephalosporin drug residues in animal muscle tissue. Background technique [0002] Cephalosporins have been a class of frequently used antibiotics since the discovery of cephalosporin C in the 1950s. In recent years, there are more than 40 kinds of cephalosporin antibiotics commonly used in daily life. This type of drug has the characteristics of a broad antibacterial spectrum and is often used in the treatment of bacterial infections. Cephalosporins are also commonly used in the treatment and prevention of animal infectious diseases in the process of food-borne animal breeding, but the allergic reactions and kidney toxicity that may be caused by the use of cephalosporins cannot be ignored. At present, there have been many reports on allergic reactions and kidney toxicity caused by taking such drugs. Since the 1980s, there have been ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 张峰许秀丽聂雪梅洪云鹤
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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