Method for determining nitroimidazole drug in bee pollen powder through combination of rapid solvent extraction-gel chromatography purification-LC/MS/MS

Abstract

The present invention relates to a detection method for a nitroimidazole drug in bee pollen powder, particularly to a method for determining a nitroimidazole drug in bee pollen powder through combination of rapid solvent extraction-gel chromatography purification-LC / MS / MS. According to the method, ethyl acetate is adopted as an extraction solvent, extraction with an accelerated solvent extractor (ASE) and gel chromatography purification (GPC) are performed, a liquid chromatography-mass spectrometry multiple reaction positive ion monitoring mode is used to determine, a matrix-matched standard curve isotope internal standard method is used to quantitate, and the results comprise the nitroimidazole compound detection limit is 1.5 [mu]g.kg<-1>, and the quantification limit is 5.0 [mu]g.kg<-1>. According to the present invention, the method recovery rate is 93.5-114.2%, and the relative standard deviation is 0.3-5.2%; and the conclusion is that the method has advantages of high automation degree, high sensitivity, accurate qualitative and quantitative result, and the like.

Description

technical field [0001] The invention relates to a method for detecting nitroimidazoles in bee pollen. Background technique [0002] Nitroimidazole drugs are a class of antibacterial and antiprotozoal drugs, mainly used in the field of livestock and poultry breeding. Such drugs mainly include metronidazole, dimernidazole, ronidazole, tinidazole, pronidazole, hydroxylated metronidazole, etc. Studies have shown that this type of drug has potential cell mutagenesis and carcinogenicity. Therefore, the United States, the European Union, Japan and my country will include this type of drug in the list of prohibited compounds. At present, the determination of such drugs reported in the literature is mainly concentrated in honey, milk, aquatic products, cosmetics, feed and other matrices. The pretreatment mainly uses organic reagents such as ethyl acetate for manual extraction, and the operation steps are cumbersome and time-consuming. [0003] Rapid solvent extraction is a newly de...

AI Technical Summary

Problems solved by technology

At present, the determination of such drugs reported in the literature is mainly concentrated in honey, milk, aquatic products, cosmetics, feed and other matrices. The pretreatment mainly uses organic reagents such as ethyl acetate for manual extraction. The operation steps are cumbersome and time-consuming.

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