Safety Monitoring

Determination of amphenicol antibiotics and metabolite residues in eggs by UPLC-MS/MS*

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  • Ningxia Veterinary Drugs and Fodder Inspection Institute, Yinchuan 750011, China

Revised date: 2022-07-21

  Online published: 2024-06-24

Abstract

Objective: To establish an ultra-high performance liquid chromatography-mass spectrometry (UPLC-MS/MS) method for the simultaneous determination of chloramphenicol,thiamphenicol,florfenicol and florfenicol amine residues in eggs to be used for determination of amphenicols and their metabolite residues in eggs. Methods: The samples were extracted by ammoniated ethyl acetate and degreased by hexane, then separated on a Waters BEH C18(50 mm×2.1 mm, 1.7 μm) column with acetonitrile-water as the mobile phase for gradient elution. Meanwhile, the samples were quantified by internal standard with positive and negative ion multiple reaction monitoring (MRM) mode through polarity switching between time segments. Results: The results showed that the linear relationships of chloramphenicol(CAP), florfenicol(FF) and florfenicol amine (FFA) were good in the range from 0.5 ng·mL-1 to 200 ng·mL-1. The linear relationship of thiamphenicol (TAP) was in the range from 2.5 ng·mL-1 to 1 000 ng·mL-1(r>0.998). The detection limits and quantitative limits of CAP, FF and FFA were 0.05 μg·kg-1 and 0.1 μg·kg-1, respectively. The detection limit and quantitative limit of TAP were 0.15 μg·kg-1, 0.4 μg·kg-1, respectively. The average recovery of CAP, FF, FFA from 0.2 μg·kg-1 to 10 μg·kg-1 and TAP from 1 to 50 μg·kg-1 were 71.7%-114.2%. The intra and inter RSDs were 0.59%-18.8%. Twenty-two batches of random egg samples were tested and the four target drugs were not detected. Conclusion: This method is simple and rapid with high sensitivity, accuracy and precision, and it can be used as a method for the determination of amphenicol antibiotics and metabolite residues in eggs.

Cite this article

BU Ning-xia, CHEN Juan, LI Yong-qin, YANG Qi . Determination of amphenicol antibiotics and metabolite residues in eggs by UPLC-MS/MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2022 , 42(9) : 1625 -1633 . DOI: 10.16155/j.0254-1793.2022.09.16

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