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高效液相色谱-串联质谱内标法同时测定水产品中15种喹酮类药物残留量
引用本文:王志杰,冷凯良,孙伟红,宁劲松,翟毓秀,谭志军,郭萌萌.高效液相色谱-串联质谱内标法同时测定水产品中15种喹酮类药物残留量[J].分析科学学报,2010,26(4).
作者姓名:王志杰  冷凯良  孙伟红  宁劲松  翟毓秀  谭志军  郭萌萌
作者单位:中国水产科学研究院黄海水产研究所,山东青岛,266071
基金项目:国家863计划,农业部行业专项,基本科研业务费 
摘    要:建立了水产品中15种喹诺酮类药物(QNs)残留量的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。以氘代试剂为内标,样品经酸性乙腈萃取后,用正己烷脱脂,旋转蒸发浓缩,采用HPLC-MS/MS选择反应监测(SRM)正离子模式测定,内标法定量。可同时对水产品中的15种QNs进行定性和定量测定。15种QNs的检出限(S/N=3)为1.0μg/kg,定量限(S/N=10)为2.0μg/kg;在10.0~200.0ng/mL时峰强度与质量浓度的线性关系良好(r0.99)。方法的平均回收率范围为66%~121%。该法简便快捷,分析成本低,在一定程度上实现了药物残留的快速检测。

关 键 词:高效液相色谱-串联质谱  内标法  水产品  喹诺酮类药物  多残留同时测定

Simultaneous Determination of 15 Quinolone Residues in Aquatic Products by HPLC-MS/MS with Internal Standard Method
WANG Zhi-jie,LENG Kai-liang,SUN Wei-hong,NING Jin-song,ZHAI Yu-xiu,TAN Zhi-jun,GUO Meng-meng.Simultaneous Determination of 15 Quinolone Residues in Aquatic Products by HPLC-MS/MS with Internal Standard Method[J].Journal of Analytical Science,2010,26(4).
Authors:WANG Zhi-jie  LENG Kai-liang  SUN Wei-hong  NING Jin-song  ZHAI Yu-xiu  TAN Zhi-jun  GUO Meng-meng
Institution:WANG Zhi-jie,LENG Kai-liang,SUN Wei-hong,NING Jin-song,ZHAI Yu-xiu,TAN Zhi-jun,GUO Meng-meng(Yellow Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Qingdao 266071)
Abstract:A method for simultaneous determination of 15 QNs residues in aquatic products was developed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Deuterium substituted reagents were added to the sample before extraction as internal standard. The sample was extracted with acidified acetonitril,cleaned-up with hexane,and concentrated with a rotary evaporator.The mass spectrometer was operated in positive ion mode using select reaction monitoring for qualitative and quantitative ana...
Keywords:High performance liquid chromatography-tandem mass spectrometry  Internal standard method  Aquatic products  Quinolone  Multi-residue  Simultaneous determination  
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