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Development of a Rapid Method for the Confirmatory Analysis of Flunixin Residue in Animal Tissues Using Liquid Chromatography–Tandem Mass Spectrometry

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Abstract

Flunixin is approved for use in veterinary medicine as a nonsteroidal anti-inflammatory agent. There is a need for the control of residues and development of methods to monitor its compliance with legislation. However, few methods have been reported for the analysis of flunixin in the animal liver, kidney, and fat. Therefore, the aim of this work was to develop a relatively rapid sample preparation and sensitive using liquid chromatography–tandem mass (LC-MS/MS) confirmatory method to detect flunixin residues in the liver, kidney, muscle, and fat of swine and chicken. After acid hydrolysis, the sample was extracted with ethyl acetate. The extract was finally evaporated to dryness and reconstituted in a water/methanol mixture, and determination was carried out by LC-MS/MS. Flunixin was detected using positive electrospray ionization in selected reaction monitoring (SRM). Estimated limit of quantification of the method was 0.5, 0.5, 0.25, and 0.05 μg/kg for the liver, kidney, muscle, and fat, respectively. The method was validated in animal tissues in terms of selectivity, linearity, trueness, precision, decision limit (CCα), and detection capability (CCβ). All the trueness values fell within a range between 73.6 and 84.8 %. Precision values for all levels of concentration tested showed excellent relative standard deviation (RSD < 15 %). The CCα and CCβ values have been established for each tissue. A relatively rapid and sensitive LC-MS/MS method for the quantitative determination of flunixin in different animal tissues was developed and validated. The method is suitable for monitoring the flunixin residues in animal tissues.

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Acknowledgments

The authors are grateful to the Ministry of Agriculture of the People’s Republic of China for the financial support.

Compliance with Ethics Requirements

The authors declare that the design, performance, and reporting of research funded under Ministry of Agriculture of the People’s Republic of China are free from bias resulting from investigator financial conflicts of interest. No financial relationship with other institutions or private industry has influenced the results of this study. All institutional and national guidelines for the care and use of laboratory animals were followed.

Conflict of Interest

Zhao-Ying Liu declares that he has no conflict of interest. Kun Yang declares that he has no conflict of interest. Fu-Hua Chen declares that he has no conflict of interest. Xue-Ming Long declares that he has no conflict of interest. Yun-Bo Deng declares that he has no conflict of interest. Guang-Wei Kuang declares that he has no conflict of interest. Zhi-Liang Sun declares that he has no conflict of interest.

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Liu, ZY., Yang, K., Chen, FH. et al. Development of a Rapid Method for the Confirmatory Analysis of Flunixin Residue in Animal Tissues Using Liquid Chromatography–Tandem Mass Spectrometry. Food Anal. Methods 8, 352–362 (2015). https://doi.org/10.1007/s12161-014-9901-z

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