超高效液相色谱-串联质谱法测定禽蛋中去呋喃头孢噻呋残留

目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定禽蛋中去呋喃头孢噻呋残留量的分析方法。方法样品用0.4%二硫赤藓醇溶液及14%碘乙酰胺溶液在室温条件下衍生化,用水饱和的正己烷除脂,经PRiME HLB固相萃取小柱净化浓缩,UPLC-MS/MS测定,采用电喷雾电离源正离子扫描,多反应监测(multiple reaction monitoring,MRM)模式检测,内标法进行定量分析。结果在2～100μg/L的质量浓度范围内,去呋喃头孢噻呋呈良好线性关系,相关系数(r²)为0.9988。样品中去呋喃头孢噻呋的检出限为1μg/kg,定量限为2μg/kg,在2、4、20μg/kg的添加浓度下的平均回收率为92.0%～99.9%,相对标准偏差(relative standard deviations,RSDs)均小于10%。结论本方法专属性强、灵敏度高,适用于禽蛋中的去呋喃头孢噻呋药物残留的检测。

Determination of desfuroyl ceftiofur residues in poultry eggs by ultra performance liquid chromatography-tandem mass spectrometry

Objective To establish a method for the determination of desfuroyl ceftiofur residues in poultry eggs by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The samples were derivatized with 0.4%dithiocarbitol solution and 14%iodine acetate solution at room temperature,saturated with hexane,then purified by PRiME HLB solid phase extraction column.UPLC-MS/MS was determined by electrospray ionization source positive ion scanning,multiple reaction monitoring(MRM)mode detection,and internal standard method was used for quantitative analysis.Results In a standard solution of 2 to 100μg/L,the desfuroyl ceftiofur showed good linear relationship.The correlation coefficient(r2)was 0.9988.The limits of detection of desfuroyl ceftiofur in the samples were 1μg/kg and the limits of quantitative were 2μg/kg.The average recoveries were 92.0%-99.9%at the range of 2,4,20μg/kg and the relative standard deviations(RSDs)were less than 10%.Conclusion This method has strong specificity and high sensitivity,and is suitable for the determination of desfuroyl ceftiofur drug residues in poultry eggs.