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

作　　者：谢敏 徐俊[1,2] 费丹 侯玉洁 刘昌林 俞莉 周瑶敏[1] 于翔 王梦芝[4] XIE Min;XU Jun;FEI Dan;HOU Yujie;LIU Changlin;YU Li;ZHOU Yaomin;YU Xiang;WANG Mengzhi(Institute of Quality Safety and Standards of Agricultural Products,Jiangxi Academy of Agricultural Sciences,Key Laboratory of Agro-product Quality and Safety of Jiangxi Province,Nanchang 330200,China;Animal Husbandry and Veterinary Science of Jiangxi Academy of Agricultural Sciences,Nanchang 330200,China;Institute of Nanchang Agricultural Sciences Academy of Agricultural Sciences,Nanchang 330200,China;Yangzhou University College of Animal Science and Technology,Yangzhou 225009,China)

机构地区：[1]江西省农业科学院农产品质量安全与标准研究所,江西省农产品质量安全重点实验室,南昌330200 [2]江西省农业科学院畜牧兽医研究所,南昌330200 [3]南昌市农业科学院,南昌330200 [4]扬州大学动物科学与技术学院,扬州225009

出　　处：《分析试验室》2024年第4期547-552,共6页Chinese Journal of Analysis Laboratory

基　　金：江西省重点研发计划(20201BBF61008);江西省肉牛创新联盟项目(JXXTCX201702)资助。

摘　　要：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.

关 键 词：牧草 QUECHERS 超高效液相色谱串联质谱 氟喹诺酮 残留 

分 类 号：S859.84[农业科学—临床兽医学] O657.6[农业科学—兽医学]