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Determination of Residues of the Novel Veterinary Drug Fluralaner in Chicken Tissues and Eggs by High Performance Liquid Chromatography-Tandem Mass Spectrometry |
LING Yihan, WANG Xiaomeng, WU Shouxun, ZHOU Ting, LI Xingjie, ZHOU Heting, ZHANG Shuwen, YIN Wenya, WANG Jianping, WANG Yi |
1. West China School of Public Health/West China Fourth Hospital, Sichuan University, Chengdu 610041, China; 2. Animal Nutrition Institute, Sichuan Agricultural University, Chengdu 611130, China; 3. Sichuan Institute of Food Inspection, Chengdu 611731, China |
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Abstract This study established a method for the determination of fluralaner residues in chicken tissues (meat, liver, skin and kidney) and eggs by high performance liquid chromatography-tandem mass spectrometry. Positive animal samples were obtained from white-feathered laying hens orally administered of low (0.10 mg/kg), medium (0.25 mg/kg) and high (0.50 mg/kg) doses of fluralaner (in two fractions, 7 d apart). Samples were extracted with acetonitrile and purified by solid phase extraction on a PRiME HLB column. The target analyte was separated on an Eclipse Plus C18 column with gradient elution using a mobile phase consisting of methanol and 5 mmol/L ammonium formate solution and analyzed using electrospray ionization in the negative ion mode with multiple reaction monitoring (MRM). A matrix-matched calibration curve was prepared and the external standard method was used for quantification under the optimal conditions. The calibration curve showed good linearity in the concentration range of 0–200 ng/mL with correlation coefficient (r2) greater than 0.99. The limit of detection (LOD) and the limit of quantification (LOQ) were 2.0 and 5.0 μg/kg, respectively. The recoveries of added fluralaner from chicken meat, eggs, liver, skin and kidney were 81.2%–99.1% with relative standard deviations (RSDs) of 1.29%–7.86% at spiked levels of 5, 15 and 50 μg/kg (n = 6). The method is simple, rapid, sensitive, and has been successfully applied for the determination of fluralaner residues in medicated chicken samples.
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