超高效液相色谱-串联质谱法测定鳗鱼肌肉组织中6种喹诺酮类药物残留  

Determination of Quinolone Residues in Eel Muscle by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：刘正才[1] 余孔捷[1] 杨方[1] 张琼[1] 刘素珍[1] 

机构地区：[1]福建出入境检验检疫局,福建省检验检疫技术研究重点实验室,福建福州350001

出　　处：《分析科学学报》2014年第6期863-867,共5页Journal of Analytical Science

基　　金：福建省检验检疫局科技计划(No.FK2010-23);质检公益项目(No.201310143-02);福建省科技重点项目(No.2012Y6001)

摘　　要：建立了快速测定鳗鱼肌肉中氧氟沙星、诺氟沙星、恩诺沙星、环丙沙星、氟甲喹和恶喹酸6种喹诺酮类（QNs）药物残留的超高效液相色谱-串联质谱（UPLC-MS/MS）方法。样品经0.2mol/L磷酸盐缓冲液（PBS,pH=7.0）匀浆后,采用酸性乙腈（含0.2%甲酸）提取,正己烷脱脂,用ACQUITY UPLC BHE C18柱（100×2.1 mm,1.7μm）,以乙腈-5mmol/L乙酸铵溶液（含0.2%甲酸）为流动相,用多反应监测（MRM）正离子扫描方式进行质谱检测,内标法定量。结果表明,该方法对以上6种喹诺酮类药物的线性范围为0.1-50μg/kg,相关系数（r）均大于0.9976;检出限为0.03-0.25μg/kg,定量限为0.1-0.8μg/kg,在1.0、2.0、10μg/kg 3个添加水平的回收率为84.8%-97.8%,相对标准偏差为4.5%-11.3%。该法简单、灵敏、特异性强,适用于鳗鱼肌肉中喹诺酮类药物多残留的检测。A ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）method for the determination of six quinolone（QN）residues in eel muscle has been developed.The sample was extracted with acetonitrile（containing 0.2% formic acid）after homogenized by phosphate solution（0.2mol/L,pH=7.0）,and then cleaned-up with hexane.The LC separation was performed on a column of ACQUITY UPLC BHE C18（100×2.1 mm,1.7μm）with acetonitrile and 5 mmol/L ammonium acetate solution（containing 0.2%formic acid）as the mobile phase.The analyte was detected by positive electrospray ionization（ESI）mode and multiple reaction monitoring（MRM）mode.The calibration curve showed good linearity within the concentrations of 0.1-50 μg/kg.The limits of detection were 0.03-0.25 μg/kg,and the limits of quantification were 0.1-0.8μg/kg.Average recoveries of six QNs（spiked at the levels of 1.0,2.0and 10.0μg/kg）ranged from 84.8% to 97.8%,with relative standard deviations between 4.5% and 11.3%.The results demonstrate that the method is simple,accurate and suitable for the simultaneous determination of multi-residues of quinolones in eel muscle.

关 键 词：超高效液相色谱-串联质谱法 喹诺酮类 残留检测 鳗鱼 

分 类 号：O657.63[理学—分析化学]