HPLC-MS/MS同位素内标法测定鸡蛋中14种喹诺酮类药物残留量

Determination of 14 quinolones residues in eggs by HPLCMS/MS with isotopic internal standard

本研究建立了同时测定鸡蛋中14种喹诺酮类药物残留的高效液相色谱-串联质谱方法。样品经EDTA-Mcllvaine缓冲液提取,正己烷脱脂,HLB固相萃取柱净化,反相C 18色谱柱分离,采用多反应监测正离子模式测定,使用同位素内标法定量。在优化条件下,14种喹诺酮类药物均能达到检测限0.5μg/kg,定量限2μg/kg。在2~100 ng/mL的质量浓度范围内线性良好,相关系数r均大于0.99。在空白鸡蛋中添加2,5,10μg/kg水平的药物回收试验中,平均回收率在83.9%~110.7%之间,批内变异系数在1.5%~13.7%之间(n=6),批间变异系数在4.5%~13.1%之间(n=18)。结果表明,该方法灵敏、准确、重复性好,适用于鸡蛋中喹诺酮类药物残留的定性定量检测。

A high performance liquid chromatography-tandem mass spectrometry method was developed for the simultaneous determination of 14 quinolones residues in eggs. The samples were extracted with EDTA-Mcllvaine buffer,followed by defatted with n-hexane,and purified by HLB solid phase extraction column,separated by reversedphase C 18 column,determined by multiple reaction monitoring positive ion mode,and quantified by isotope internal standard method. Under the optimized conditions,the detection limit and quantification limit of 14 quinolones were0.5 μg/kg and 2 μg/kg,respectively. The linearity was fine in the range of 2~100 ng/mL,and the correlation coefficients r was greater than 0.99. Adding 2,5,and 10 μg/kg to blank eggs sample,the average recoveries were83.9%~110.7%,the intra-assay coefficient of variation were between 1.5% and 13.7%(n=6),and the inter-assay coefficient of variation were from 4.5% to 13.1%(n=18). The results showed that the method was sensitive,accurate,and reproducible,and was suitable for the qualitative and quantitative detection of quinolones residues in eggs.