Citation: MUHAREM Muhteber, YAN Hua, XU Shan, FENG Nan, HAO Jie, ZHU Chenqi, GUO Shuang, ZHANG Zhaohui, HAN Nanyin. Determination of six anticoccidials in chicken using QuEChERS combined with ultra high liquid chromatography-high resolution mass spectrometry[J]. Chinese Journal of Chromatography, ;2015, 33(11): 1199-1204. doi: 10.3724/SP.J.1123.2015.06016 shu

Determination of six anticoccidials in chicken using QuEChERS combined with ultra high liquid chromatography-high resolution mass spectrometry

MUHAREM Muhteber ¹ ,
YAN Hua ² ,
XU Shan ² ,
FENG Nan ³ ,
HAO Jie ³ ,
ZHU Chenqi ¹ ,
GUO Shuang ¹ ,
ZHANG Zhaohui ² ,
HAN Nanyin ^1,,

1.
1. School of Pharmaceutical Science, Peking University, Beijing 100191, China;

Corresponding author: HAN Nanyin,
Received Date: 10 June 2015

Fund Project: 北京市科委重大项目(D151100003815002). (D151100003815002)

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×2.1 mm, 1.7 μ m) 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 μ g/L; nicarbazin, 0.2-6.0 μ g/L; diclazuril and toltrazuril, 2.0-60.0 μ g/L; monensin and salinomycin, 4.0-120.0 μ g/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 μ g/kg; nicarbazin, 0.50 μ g/kg; diclazuril and toltrazuril, 5.00 μ g/kg; monensin and salinomycin, 20.00 μ g/kg. The developed method is easy of operation and of high sensitivity. It can meet the requirements of daily inspection.
- QuEChERS,
- ultra high liquid chromatography-high resolution mass spectrometry,
- anticoccidials,
- chicken
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