色谱Issue(11)：1199-1204,6.DOI:10.3724/SP.J.1123.2015.06016
QuEChERS-超高效液相色谱-高分辨串联质谱技术检测鸡肉中6种抗球虫药物
Determination of six anticoccidials in chicken using QuEChERS combined with ultra high liquid chromatography-high resolution mass spectrometry
摘要
Abstract
An ultra high liquid chromatography-Q Exactive orbitrap mass spectrometry multi-residue method has been developed for the determination of six anticoccidials residues (dinitlmide,nicarbazin,diclazuril,toltrazuril,monensin and salinomycin)in chicken tissue. Sample preparation was based on QuEChERS method,using 1%( v/v)trichloroacetic acid/acetonitrile aqueous solution(3:7,v/v)as the extraction solvent and salting-out with sodium chloride followed by clean-up with 50 mg/mL primary secondary amine( PSA)+50 mg/mL neu-tral alumina( Alumina-N ) dispersive solid phase extraction ( DSPE ). The separation of the compounds in liquid chromatography was carried out using a Waters Acquity UPLC ® BEH C8 column( 100 mm × 2. 1 mm,1. 7 μm ) with mobile phases consisting of methanol-5 mmol/L ammonium acetate aqueous solution in gradient elution. The Q Exactive orbitrap mass spectrometric detection was carried out with positive and negative electrospray ionization simul-taneously. The results showed the linear ranges of the six target compounds were as follows:dinitolmide,1. 0-30. 0 μg/L;nicarbazin,0. 2-6. 0 μg/L;diclazuril and toltrazuril,2. 0-60. 0μg/L;monensin and salinomycin,4. 0-120. 0 μg/L. The external standard method was used for quantification. The spiked recoveries at three levels for the six anticoccidials ranged from 67. 7% to 126. 8%. The relative standard deviations( RSDs)were ≤10. 4%. The limits of quanti-fication( LOQs)were as follows:dinitolmide,2. 50 μg/kg;nicarbazin,0. 50 μg/kg;diclazuril and toltrazuril,5. 00 μg/kg;monensin and salinomycin,20. 00 μg/kg. The developed method is easy of operation and of high sensitivity. It can meet the requirements of daily inspection.关键词
QuEChERS/超高效液相色谱-高分辨串联质谱/抗球虫药/鸡肉Key words
QuEChERS/ultra high liquid chromatography-high resolution mass spectrometry/anticoccidials/chicken分类
化学化工引用本文复制引用
木合他拜尔,严华,徐姗,冯楠,郝杰,朱尘琪,郭爽,张朝晖,韩南银..QuEChERS-超高效液相色谱-高分辨串联质谱技术检测鸡肉中6种抗球虫药物[J].色谱,2015,(11):1199-1204,6.基金项目
北京市科委重大项目（ D151100003815002）． （）
