超高效液相色谱–串联质谱法测定鸡蛋中7种喹诺酮类药物残留量的研究

Determination of Seven Quinolones Residues in Eggs by UPLC-MS/MS

建立了鸡蛋中7种喹诺酮类药物残留检测的超高效液相色谱–串联质谱方法 (UPLC–MS/MS)。样品经EDTA-Mcllvaine缓冲溶液提取,正己烷除脂,HLB固相萃取柱净化后,进行UPLC–MS/MS分析。7种喹诺酮类药物在2.5~100.0 ng/mL的浓度范围内,呈良好的线性关系,相关系数均>0.990;该方法检测限为0.05~1.2μg/kg,定量限为0.2~5.0μg/kg;在0.2~25.0μg/kg的样品添加中,方法的平均回收率在91.5%~108.0%,批内、批间RSD均<15%。该方法定性、定量准确,结果重复性好,灵敏度高,适用于鸡蛋中7种喹诺酮类药物残留量的定性和定量分析。

An UPLC-MS/MS method was established for the determination of seven Quinolones in eggs. The samples were extracted by EDTA-Mcllvaine buffer solution, degreased by Hexane, purified by HLB solid phase extraction column and determined by UPLC-MS/MS. The good linearity was obtained within the mass concentration range of 2.5 -100.0 ng/mL（r0.99）; the LOD was 0.05 -1.2 μg/kg and LOQ was 0.2 -25.0 μg/kg. The average recovery was 91.5% -108%, when0.2-25.0 μg/kg quinolones were added into the eggs,and the RSD was less than 15%. The method is accurate, simple and highly sensitive, which is satisfied to qualitative and quantitative determination of the seven quinolones residues in eggs.