液质联用法检测禽肉及禽蛋中硝基咪唑类残留量方法研究

Determination of nitroimidazole residues in poultry meat and eggs by liquid chromatography-mass spectrometry

目的 利用超高效液相色谱-串联质谱仪建立一种快速、准确检测禽肉和禽蛋中硝基咪唑类药物(替硝唑、奥硝唑、络硝哒唑、甲硝唑和二甲硝唑)残留的新方法。方法 样品经三氯乙酸提取,提取液浓缩后酸性溶液溶解,采用MCX混合阳离子固相萃取柱净化,采用超高效液相色谱-串联质谱测定,基质匹配内标法定量。结果 本方法硝基咪唑类药物检出限为:1.0μg/kg,定量限为:3.0μg/kg。目标检测物在5.0~50μg/L浓度范围内线性关系良好,且3个添加浓度加标回收率大于70%,相对偏差小于20%。结论 该方法高效简便、准确可靠,可应用于禽肉及禽蛋中硝基咪唑类药物残留的检测。

Objective To establish a new method for rapid and accurate determination of nitroimidazoles(including tinidazole,ornidazole,ronidazole,metronidazole,and dimethylmetronidazole)residues in poultry meat and eggs by using ultra-high performance liquid chromatography tandem mass spectrometry.Methods The samples were extracted with trichloroacetic acid,and then the extraction solution was concentrated and dissolved in acid solution.Before use of ultra-high performance liquid chromatography tandem mass spectrometry for the analysis,the extraction solution was purified by a mixed-mode cation exchange(MCX)solid-phase extraction column,and quantification of the detection data was performed by internal standard method.Results In this method,the detection and quantitation limits of nitroimidazoles were 1.0μg/kg and 3.0μg/kg respectively.A good linear relationship was obtained with the concentrations ranged from 5.0μg/L to 50μg/L,the spiked recoveries were above 70%and the relative deviation was less than 20%with three different spiked concentrations.Conclusion The method is efficient,simple,accurate and reliable,which can be used for the determination of nitroimidazole residues in poultry meat and eggs.