Method for simultaneously detecting bacitracin A and bacitracin B residues in eggs

A technology of bacitracin and residual amount, applied in the field of analysis and detection, can solve the problems of inability to detect the effective components of bacitracin B, difficulty in separation, inability to separate bacitracin, etc., and achieve good chromatographic peak shape, good separation effect, and easy observation Effect

Pending Publication Date: 2022-06-03
QILU PHARMA INNER MONGOLIA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The HPLC detection method provided by the present invention is simple and accurate, and is used to quickly and accurately detect the output of bacitracin A. This method also only realizes the detection of a single active ingredient bacitracin A, and cannot detect the active ingredient of bacitracin B. limitations
[0012] Due to the large number of bacitracin components, it is difficult to separate them. The existing methods cannot effectively separate bacitracin A and bacitracin B. Therefore, a method for simultaneously detecting bacitracin A and bacitracin B residues in eggs method, which is of great significance for effectively monitoring the use of this drug and ensuring the safety of animal-derived food in my country.

Method used

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  • Method for simultaneously detecting bacitracin A and bacitracin B residues in eggs
  • Method for simultaneously detecting bacitracin A and bacitracin B residues in eggs
  • Method for simultaneously detecting bacitracin A and bacitracin B residues in eggs

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Embodiment 1

[0075] A method for simultaneously detecting bacitracin A and bacitracin B residues in eggs, comprising the following steps:

[0076] 1) Extraction of egg blank sample: Take 2 g of egg blank sample (accurate to 0.01 g), put it in a 50 mL centrifuge tube, add 4 mL of 10% trichloroacetic acid acetonitrile solution, vortex for 1 min, and then add 10 mL of 0.5% trifluoroacetic acid aqueous solution, Shake and extract for 10 min, centrifuge at 10 000 rpm for 8 min, transfer to another centrifuge tube, repeat the above operation, repeat the extraction once, combine the supernatant of the two extractions, mix well, blow the supernatant nitrogen to 20 mL, add 10 mL of n-hexane hexane, shake for 5 min, centrifuge at 10,000 rpm for 5 min, discard the upper n-hexane layer, and transfer the lower supernatant to another centrifuge tube to prepare a blank sample solution;

[0077] 2) Purify the blank sample solution; activate and equilibrate the HLB solid-phase extraction column with 5 mL o...

experiment example

[0088] Experimental example: detection condition selection

[0089] 1. The effect of different solvent treatment methods on leaching

[0090]a. Due to the high content of impurities in the egg extract, egg samples are rich in protein and fat. Extraction with 4%, 10%, and 30% trichloroacetic acid acetonitrile solution, respectively, showed that the drug recovery rate was lower when 30% trichloroacetic acid acetonitrile solution was used. However, the 4% and 10% trichloroacetic acid acetonitrile solution has no significant difference in the protein removal effect. The 10% trichloroacetic acid acetonitrile solution has less influence on the peak shape change, less matrix interference and the recovery rate meets the requirements. Therefore, 10% was selected. % trichloroacetic acid in acetonitrile as the extraction solvent.

[0091] b. Polypeptide drugs contain multiple amino groups and carboxyl groups, which are polar compounds. Strongly acidic solutions are often used to extrac...

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Abstract

The invention relates to a method for simultaneously detecting the residual quantity of bacitracin A and bacitracin B in an egg. The method comprises the following steps: extracting an egg blank sample, purifying a blank sample solution, and drawing an egg matrix matching standard curve; a sample to be detected is extracted and purified, and the purified liquid of the sample to be detected is subjected to liquid chromatography-tandem mass spectrometry determination; according to the method, the bacitracin A and the bacitracin B are simultaneously determined at one time through the liquid chromatography-tandem mass spectrometry, the method is simple, convenient and rapid, the separation effect is good, the determination precision is high, the result reproducibility is good, observation is easy, the specificity is high, the chromatographic peak shape is good, time and reagents are saved, and accurate and rapid determination can be carried out. The method has the characteristics of strong anti-interference capability, low detection limit and high sensitivity.

Description

Technical field: [0001] The invention relates to a method for simultaneously detecting the residual amounts of bacitracin A and bacitracin B in eggs, belonging to the field of analysis and detection. Background technique: [0002] Bacitracin (Bacitracin) is a bacterial strain that produces antibacterial substances, Bacillus licheniformis, isolated by Johnson et al. of Columbia University in the United States when dealing with tibial trauma cases, and the finished product is obtained by fermentation. Because it is a polypeptide produced by Bacillus, it is called Bacitracin in Chinese. The antibacterial spectrum of bacitracin is similar to that of penicillin, and it has a strong antibacterial effect on gram-positive bacteria, and is also effective on some gram-negative bacteria (such as meningococcus, influenza bacillus), actinomycetes, and spirochetes. Bacitracin can promote animal growth, improve feed conversion rate, prevent and treat various animal intestinal diseases, an...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14G01N30/34G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/14G01N30/34G01N30/7266G01N30/8675G01N2030/062
Inventor 陈富荣贾曼陈刚
Owner QILU PHARMA INNER MONGOLIA
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