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Development and Validation of a HPLC-HESI-MS/MS Method for Simultaneous Determination of Robenidine Hydrochloride and Its Metabolites in Fish and Exploration of Their Kinetic Regularities in Grass Carp

  • Yongtao LiuEmail author
  • Yi Song
  • Bo Cheng
  • Jing Dong
  • Ning Xu
  • Shun Zhou
  • Qiuhong Yang
  • Xiaohui AiEmail author
Article

Abstract

An original method for the simultaneous determination of robenidine hydrochloride (ROBH) and its main metabolites 4-chlorohippuric acid (PCHA) and 4-chlorobenzoic acid (PCBA) in fish plasma and muscle was established by high-performance liquid chromatography coupled with heat electrospray ionization tandem mass spectrometry (HPLC-HESI-MS/MS) using predefined time segments in the alternating positive/negative mode. Fish muscle samples were prepared using a modified QuEChERS procedure, and plasma samples were prepared by a liquid–liquid extraction (LLE) procedure. The entire procedure was validated according to the guidelines defined by the US Food and Drug Administration. Matrix-matched calibration curves for plasma and muscle of fish showed good linearity with correlation coefficients (R2) ≥ 0.9985. The accuracy exhibited a relative error (RE) ranging from −14.2–8.2%, and intra- and inter-day precisions of analytes expressed as relative standard deviation (RSD) were within 12.4%. Limits of detection (LODs) and limits of quantitation (LOQs) were lower than 2.5 μg L−1 and 5 μg L−1 for target compounds in plasma and not more than 2.5 μg kg−1 and 5 μg kg−1 for analytes in muscle, respectively. The present method was successfully applied to explore the kinetic profiles of ROBH and its metabolites in grass carp (Ctenopharyngodon idella), and it demonstrated that PCBA is the major metabolite of ROBH in grass carp plasma and muscle. The elimination half-lives (t1/2β) of ROBH and PCBA in grass carp muscle were calculated to be 17.31 h and 138.53 h, respectively.

Keywords

Robenidine hydrochloride Metabolites Kinetic regularity Fish HPLC-HESI-MS/MS 

Notes

Funding Information

This study was supported financially by the Central Public-interest Scientific Institution Basal Research Fund, CAFS (Nos. 2019ZD0901 and 2018JBF02), the National Natural Sciences Foundation of China (No. 3150219), and China Agriculture Research System (CARS-49).

Compliance with Ethical Standards

Conflict of Interest

Yongtao Liu declares that he has no conflict of interest. Yi Song declares that he has no conflict of interest. Bo Cheng declares that he has no conflict of interest. Jing Dong declares that he has no conflict of interest. Ning Xu declares that he has no conflict of interest. Shun Zhou declares that he has no conflict of interest. Qiuhong Yang declares that he has no conflict of interest. Xiaohui Ai declares that he has no conflict of interest.

Ethical Approval

All applicable international and national/institutional guidelines for the care and use of animals were followed.

Information Consent

Not applicable.

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Copyright information

© Springer Science+Business Media, LLC, part of Springer Nature 2019

Authors and Affiliations

  1. 1.Yangtze River Fisheries Research InstituteChinese Academy of Fishery SciencesWuhanChina
  2. 2.Key Laboratory of Control of Quality and Safety for Aquatic ProductsMinistry of Agriculture and Rural AffairsBeijingChina
  3. 3.Hubei Province Engineering and Technology Research Center for Aquatic Product Quality and SafetyWuhanChina
  4. 4.Aquatic Products Quality and Standards Research CenterChinese Academy of Fishery SciencesBeijingChina

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