分散固相萃取-同位素内标-液相色谱串联三重四极杆质谱法测定禽蛋中氟吡禾灵、氟吡禾灵酯及共轭物残留量

Determination of haloxyfop,haloxyfop-esters and conjufates residue in eggs by liquid chromatography tandem triple quadrupole mass spectrometry combined with dispersive solid phase extraction-isotope internal standard

通过优化禽蛋前处理方法,建立一种分散固相萃取-同位素内标-液相色谱串联三重四极杆质谱法测定水产品中氟吡禾灵、氟吡禾灵酯及共轭物残留量方法.称取5.0 g试样,用10 mL乙腈萃取,加氧化钠溶液水解氟吡禾灵酯成氟吡禾灵,经100 mgGCB和100 mgC18净化,取上清液,采用三重四极杆串联质谱正离子模式下的多反应监测检测,内标法定量.研究结果表明,本方法中氟吡禾灵在0.001—0.500μg·L^(−1)范围内具有良好的线性关系,相关系数0.9996,加标回收率93.7%—97.1%,检出限0.003 mg·kg^(−1),定量限0.010 mg·kg^(−1).本方法具有前处理简单、灵敏度高等特点,适用于禽蛋中氟吡禾灵、氟吡禾灵酯及共轭物残留量的检测.

An analytical method was developed for the determination of haloxyfop,haloxyfop-esters and conjufates residue in eggs using LC-MS/MS combined with dispersive solid phase extractionisotope internal standard.After 5.0 g aquatic product samples were extracted with 10 mL acetonitrile,the sodium hydroxide solution hydrolyzed haloxyfop-esters into haloxyfop.After purification by 100 mg GCB and 100 mg C18,the supernatant was detected by MRM under the positive ion mode of liquid chromatography-tandem mass spectrometry and quantified by internal standard method.The method displayed good linearity in the concentration of haloxyfop ranged from 0.001μg·L^(−1)to 0.500μg·L^(−1)with the correlation coefficient of 0.9996,the average recoveries ranged from 93.7%to 97.1%,the limit of detection of 0.003 mg·kg^(−1)and the limit of quantification of 0.01 mg·kg^(−1).This method is fast,ensitivity and suitable for determination of haloxyfop,haloxyfop-esters and conjufates residue in eggs.