超高效液相色谱-串联质谱内标法快速测定水产品中9种氟喹诺酮类药物残留量

Rapid determination of 9 fluoroquinolones residues in aquatic products by UPLC/MS/MS with internal standard method

建立了超高压液相色谱-串联质谱方法快速检测水产品中9种氟喹诺酮类药物残留量的方法。试样中残留的氟喹诺酮类药物采用酸化乙腈进行提取,以正己烷两次净化,再经过滤除杂后,采用LC/MS/MS多反应监测（MRM）正离子模式测定,内标法定量。9种氟喹诺酮类药物在1~20μg.L-1范围内线性关系良好,相关系数均大于0.99。在3.5min内,9种氟喹诺酮类药物可依次检出。在2.5、5.0、10.0μg.kg-13个加标浓度下平均回收率75%~110%,相对标准偏差（RSD）范围为2.4%～11.8%（n=6）。本方法对水产品中9种氟喹诺酮类药物的检出限（S/N〉3）为0.1~0.5μg.kg-1,定量限（S/N〉10）为0.5~1.0μg·kg-1。

A method for fast determination of 9 FQs residues in aquatic products was developed by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）.The sample was extracted with acidified acetonitrile,cleaned up with hexane for twice times,and dislodged with filters.The mass spectrometer was operated in positive ion mode using multiple reaction monitoring（MRM）for quantitative by internal standard method.The correlation coefficients of linear calibration curves were over 0.99 within the FQs concentration range 1～20μg.L-1.9 FQs were detected one by one in 3.5 minute.The average recoveries for 9 FQs were between 75% and 110% at the concentration level of 2.5,5.0 and 10.0μg.kg-1.The RSD between 2.4 and 11.8（n=6）.The detection limits for 9 FQs were 0.1～0.5ng.g-1（S/N=3）,and the quantitative limits were 0.5～1.0ng.g-1.