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

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

中文关键词:  禽蛋  去呋喃头孢噻呋  兽药残留  超高效液相色谱-串联质谱法

英文关键词:poultry eggs  desfuroyl ceftiofur  veterinary drug residues  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      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2~100 μg/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1 μg/kg, 定量限为2 μg/kg, 在2、4、20 μg/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。

英文摘要:

      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 100 μg/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 1 μg/kg and the limits of quantitative were 2 μg/kg. The average recoveries were 92.0%?99.9% at the range of 2, 4, 20 μg/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.