Simultaneous Analysis of Nicarbazin, Diclazuril, Toltrazuril, and Its Two Metabolites in Chicken Muscle and Eggs by In-Syringe Dispersive Solid-Phase Filter Clean-Up Followed by Liquid Chromatography–Tandem Mass Spectrometry

Author:

An Yuxin1,Pan Xiaodong1,Cai Zengxuan1,Xu Meijia1,Jiang Dingguo2,Xu Xiaomin1

Affiliation:

1. Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China

2. NHC Key Laboratory of Food Safety Risk Assessment, China National Center for Food Safety Risk Assessment, Beijing 100026, China

Abstract

Nicarbazin (NICA) and triazine anticoccidial drugs (diclazuril (DIZ) and toltrazuril (TOZ)) are the primary strategy for preventing and treating coccidiosis. To prevent the development of drug resistance and mitigate the potential chronic toxicity to humans resulting from prolonged exposure, a liquid chromatography–tandem mass spectrometry method with high reliability and sensitivity was developed to determine NICA, DIZ, TOZ, and its two metabolites in chicken muscle and eggs. Upon establishing the extraction conditions involving 10 mL of acetonitrile and 10 min of sonication, in-syringe dispersive solid-phase extraction with silica was performed in combination with n-hexane clean-up. The selection of isotope peaks of precursor ions and low-mass range scanning allowed the two transitions for the quantification of all compounds. The limits of detection for DIZ and NICA were both 0.1 μg/kg, and for TOZ and metabolites, they were 0.3 μg/kg; the limits of quantitation were 0.3 and 1 μg/kg, respectively. The linear range was 0.25–50 ng/mL with a correlation coefficient r > 0.999. The average recoveries at three spiking levels in muscle and eggs were 90.1–105.2% and 94.0–103.7% with the relative standard deviations of 3.0–8.1% and 3.1–14.4%, respectively. The precision, accuracy, and stability were evaluated by three quality control samples.

Publisher

MDPI AG

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