摘要
同时以左氧氟沙星和环丙沙星为模板分子,α-甲基丙烯酸(MAA)为功能单体,三羟甲基丙烷三甲基丙烯酸酯(TRIM)为交联剂,合成了复合模板分子印迹聚合物,建立了以此聚合物为分子印迹固相萃取(MISPE)富集净化样品,结合高效液相色谱-离子阱质谱(HPLC-ITMS)同时测定鱼肉中10种氟喹诺酮类药物残留量的方法。采用2%醋酸乙腈提取样品,提取液经正己烷脱脂后,过自制的复合模板分子印迹固相萃取柱净化,以0.05%甲酸溶液和乙腈为流动相,梯度洗脱程序进行色谱分离,离子阱质谱进行定性和定量分析。方法的回收率为80.6%～104.6%,相对标准偏差小于8.6%(n=3);检出限(LOD)为0.11～0.25μg/kg;定量限(LOQ)为0.35～0.84μg/kg,可以满足水产品中氟喹诺酮类药物的确证和多残留分析的要求。
The molecularly imprinted polymer（MIP） has been prepared using levofloxacin and ciprofloxacin as the mixed-templates,α-methacrylic acid（MAA） as functional monomers and trimethylolpropane trimethylacrylate（TRIM） as crosslinker.A method has been established for simultaneous determination of residues of ten fluoroquinolones in grass carp by high performance liquid chromatography-ion trap mass spectrometry（HPLC-ITMS） combining with molecularly imprinted polymer solid phase extraction（MISPE）.The samples were extracted with 2% acetic acid in acetonitrile and defatted with n-hexane,then purified by the self-made molecularly imprinted cartridge.The preparation of samples and the separation conditions had been optimized,HPLC was performed with a gradient elution program while acetonitrile and water（containing 0.05% formic acid） were used as mobile phase.The identification and quantification were done with ion trap mass spectrometry.The recove-ries ranged from 80.6% to 104.6% with a relative standard deviations of 8.6%.The limits of detection（LOD） were 0.11-0.25 μg/kg and the limits of quantification（LOQ） were 0.35-0.84 μg/kg.This method is suitable for validation and multi-residue analysis of fluoroquolones in aquatic products.
出处
《分析化学》
SCIE
CAS
CSCD
北大核心
2012年第5期693-698,共6页
Chinese Journal of Analytical Chemistry
基金
河北省自然科学基金(No.B2005000105)
河北省科技支撑计划(No.12220402D)资助项目
关键词
高效液相色谱-离子阱质谱
复合模板印迹聚合物
氟喹诺酮
High performance liquid chromatography-ion trap mass spectrometry
Mixed-templates imprinted polymer
Fluoroquinolones
