title: [Determination of six anticoccidials in chicken using QuEChERS combined with ultra high liquid chromatography-high resolution mass spectrometry].
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 neutral 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 x 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 simultaneously. 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, 2.0-60.0 [μg/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 quantification (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.
authors.forename: Muhteber
authors.initials: M
authors.lastname: Muharem
authors.forename: Hua
authors.initials: H
authors.lastname: Yan
authors.forename: Shan
authors.initials: S
authors.lastname: Xu
authors.forename: Nan
authors.initials: N
authors.lastname: Feng
authors.forename: Jie
authors.initials: J
authors.lastname: Hao
authors.forename: Chenqi
authors.initials: C
authors.lastname: Zhu
authors.forename: Shuang
authors.initials: S
authors.lastname: Guo
authors.forename: Zhaohui
authors.initials: Z
authors.lastname: Zhang
authors.forename: Nanyin
authors.initials: N
authors.lastname: Han
mesh_terms: D000818:Animals; D002645:Chickens; D002851:Chromatography, High Pressure Liquid; D003049:Coccidiostats / Q000032:analysis*; D005506:Food Contamination / Q000032:analysis*; D013058:Mass Spectrometry; D008460:Meat / Q000032:analysis*
chemical_list: D003049:Coccidiostats