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New matrix certified reference material for accurate measurement of ciprofloxacin residue in egg

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Abstract

Matrix certified reference materials (CRMs) are an indispensable part of method validation and have played an important role in ensuring reliable analytical results. To retain similarity to real samples, a new matrix CRM for the mass fraction of ciprofloxacin in whole liquid egg was developed by use of incurred materials with a target value corresponding to residue levels in real sample. The source materials were collected from laying hens following oral administration of ciprofloxacin. An optimized homogenization method and a strict bottling process were applied to bulk whole egg materials to prepare the CRM candidate. The mass fraction of ciprofloxacin in whole liquid egg was certified by a collaborative characterization program with eight accredited participating laboratories. Liquid chromatography coupled with isotope dilution mass spectrometry was studied as a reliable reference method for value assignment and was used by all participating laboratories. The certified value and expanded uncertainty (k = 2, at a confidence level of 95%) was 39.7 ± 5.2 μg/kg for ciprofloxacin in whole liquid egg. Homogeneity, long-term stability at -70 °C for 12 months, and short-term stability at -18 °C, 4 °C, and room temperature were assessed for 9 days. Additionally, uncertainties arising from inhomogeneity, instability, and characterization were analyzed in detail and fully estimated. This CRM would be a useful tool for validation of analytical methods and proficiency testing in ciprofloxacin residue analysis of egg.

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Acknowledgements

The authors gratefully acknowledge financial support from the National Key Research and Development Program of China (2016YFF0201105) and the Agricultural Science and Technology Innovation Program of China.

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Authors and Affiliations

  1. Key Laboratory of Agro-Product Quality and Safety, Ministry of Agriculture and Rural Affairs, Institute of Quality Standard and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing, 100081, China

    Mengrui Yang, Fang Liu, Min Wang, Jian Zhou, Liyuan Zhang, Lingbo Jian & Tongtong Wang

  2. Jiangsu Key Laboratory for Food Quality and Safety—State Key Laboratory Cultivation Base of Ministry of Science and Technology, Institute of Food Safety and Nutrition, Jiangsu Academy of Agricultural Sciences, Nanjing, 210014, Jiangsu, China

    Ruicheng Wei & Ran Wang

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  1. Mengrui Yang
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  2. Fang Liu
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  3. Min Wang
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  4. Jian Zhou
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  5. Ruicheng Wei
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  6. Ran Wang
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  7. Liyuan Zhang
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  8. Lingbo Jian
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  9. Tongtong Wang
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Correspondence to Min Wang.

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All animal experiments were approved by the Animal Care and Ethics Committee of Nanjing Agricultural University (permit number IACECNAU20111105) and followed the Guiding Principles for Biomedical Research Involving Animals.

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Yang, M., Liu, F., Wang, M. et al. New matrix certified reference material for accurate measurement of ciprofloxacin residue in egg. Anal Bioanal Chem 412, 635–645 (2020). https://doi.org/10.1007/s00216-019-02264-5

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  • DOI: https://doi.org/10.1007/s00216-019-02264-5

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