Method for measuring residual quantity of chloramphenicol in propolis by using high performance liquid chromatography tandem mass spectrum

Abstract

The invention relates to a method for measuring the residual quantity of chloramphenicol in propolis by using a high performance liquid chromatography tandem mass spectrum. At present, a measuring method with low detection cost and detection limit reaching 0.1mu g / kg is not found. The method comprises work procedures of standard solution preparation, standard curve preparation, propolis sample solution preparation and chloramphenicol residual quantity detection, wherein the work procedure of propolis sample solution preparation comprises the following steps of: adding 1mol / L NaOH solution to dissolve a propolis sample; diluting with water to dilute a target object in the propolis sample; acidizing with HCLO4 so as to precipitate propolis components in the propolis sample; adjusting the pH value of filtrate of the propolis sample solution to be 10.5 with the 1mol / L NaOH solution; and finally measuring the residual quantity of chloramphenicol in the propolis sample solution through a high performance liquid chromatography and a trebling quadrupole rod tandem mass spectrum. The invention has low detection cost and high detection efficiency, the detection limit energy reaches 0.1mu g / kg, the quantitation limit is 0.3mu g / kg and the linear correlation coefficient is 0.9999.

Description

technical field [0001] The present invention relates to a method for determining the residual amount of chloramphenicol in propolis, in particular to a method for determining the residual amount of chloramphenicol in propolis by high performance liquid chromatography tandem mass spectrometry, which is mainly used for determining the residual amount of chloramphenicol in propolis It is also suitable for checking the residual amount of chloramphenicol in royal jelly and honey. Background technique [0002] Chloramphenicol is an antibiotic produced by Streptomyces venezuela, and it is a broad-spectrum antibacterial agent. Due to its high toxicity to the blood system, it is banned from being used in food of animal origin by the European Union, Japan, the United States and other countries. [0003] Chloramphenicol detection methods mainly include LC / MS / MS method, GC / MS method, GC method, ELISA method, HPLC method and CHARM II method, etc. The detection method of the amount of c...

AI Technical Summary

Problems solved by technology

However, due to the different components of different types of samples, the degree of sample purification is also different. When using liquid chromatography-tandem mass spectrometry, not all samples can reach the detection limit of 0.1μg / kg. When the liquid chromatography-tandem mass spectrometry method for determining the residual amount of chloramphenicol is used to determine the residual amount of chloramphenicol in propolis, the detection limit is far less than 0.1 μg / kg. This is because there are nearly a thousand components in propolis, and there are still There is no ideal method as a standard for the detection of chloramphenicol residues in propolis, and there is no relevant literature on the detection of chloramphenicol residues in propolis in China

[0005] To sum up, there is no simple and accurate method, low detection cost, high detection efficiency, and a detection limit of 0.1 μg / kg for the determination of chloramphenicol residues in propolis, which is difficult to detect in propolis. Meet foreign requirements for chloramphenicol residue limit in propolis

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