QuEChERS-超高效液相色谱-串联质谱法测定牧草中氟喹诺酮类药物残留

Simultaneous determination of quinolones in forage grass by QuEChERS-ultra-high performance liquid chromatography-tandem mass spectrometry

建立了QuEchERS-超高效液相色谱-串联质谱(UPLC-MS/MS)检测牧草中7种氟喹诺酮类药物残留的方法。样品采用0.1 mol/L Na2EDTA-Mcllvaine缓冲液和1%乙酸-乙腈提取,经QuEchERS净化后Ag-ilent ZORBAX Eclipse Plus C_(18)色谱柱分离,正离子模式扫描,多反应监测模式,内标法定量。7种氟喹诺酮类药物在0.5~50μg/L范围内线性相关系数(R^(2))均大于0.9955,方法检出限为0.05~0.2μg/kg,定量限为0.1~0.5μg/kg。平均添加回收率为79.0%~115.4%,相对标准偏差为0.20%~8.5%。该方法适用于牧草中氟喹诺酮类药物检测分析,可为牧草中氟喹诺酮类药物残留风险评估、质量安全监管、牧草品质评价等提供技术支撑。

A QuEChERS-ultra-high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous determination of 7 kinds of fluorchinolones in forage grass was developed.Forage grass sample was extracted with 0.1 mol/L Na2EDTA-Mcllvaine buffer and 1%formic acid acetonitrile solution,and purified by QuEChERS.Then the target compounds were separated by Agilent ZORBAX Eclipse Plus C_(18) column,analyzed by electrospray ionization in positive ion scanning under multiple reaction monitoring mode,and quantified with internal standard method.The 7 kinds of fluorchinolones displayed good linearity within the concentration ranges of 0.5-50μg/L,and the correlation coefficients(R ^(2))were above 0.9955.The limits of detection were 0.05-0.2μg/kg,and the limits of quantification were 0.1-0.5μg/kg.The recoveries were 79.0%-115.4%,and the relative standard deviations(RSDs)were between 0.2%and 8.5%.The method is suitable for the simultaneous analysis of 7 kinds of fluorchinolones in forage grass,which can provide a scientific basis for fluorchinolones residues risk assessment,and quality and safety supervision of forage grass.