<p>Preprocessing methods involving liquid–liquid extraction (LLE) and solid-phase extraction (SPE) were combined with gas chromatography‒tandem mass spectrometry (GC–MS/MS) to perform qualitative and quantitative evaluations of enrofloxacin and ofloxacin in dairy products (raw milk and milk powder) and eggs (whole egg, albumen, and yolk). Trimethylsilyl diazomethane (TMSD) was applied as the precolumn derivatization reductant. The limits of detection (LODs) and limits of quantitation (LOQs) of enrofloxacin were 0.4 ~ 1.1 and 1.0 ~ 2.0&#xa0;µg/kg, respectively. The LODs and LOQs of ofloxacin were 0.1 ~ 0.2 and 0.2 ~ 0.4&#xa0;µg/kg, respectively. The recoveries of enrofloxacin and ofloxacin ranged from 79.78 to 92.33% and 78.26 to 90.79%, respectively. The RSDs were all less than 5.60%. The method was validated to satisfy the demand of the FAO &amp; WHO (2014) standard. Moreover, successful utilization of this method is needed to satisfy the technical requirements of various laboratories.</p> Graphical Abstract <p></p>

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Analytical Method Established via Derivatization-Integrated Gas Chromatography–Tandem Mass Spectrometry for the Determination of Enrofloxacin and Ofloxacin Residues: A Focus on Eggs and Dairy Products

  • Junjie Xu,
  • Hao Ding,
  • Jingjing Cai,
  • Pengfei Gao,
  • Sihui Cheng,
  • Yang Cao,
  • Yiwei Hong,
  • Xing Xie,
  • Tao Zhang,
  • Genxi Zhang,
  • Xiaodong Guo,
  • Guojun Dai,
  • Maoda Pang,
  • Kaizhou Xie

摘要

Preprocessing methods involving liquid–liquid extraction (LLE) and solid-phase extraction (SPE) were combined with gas chromatography‒tandem mass spectrometry (GC–MS/MS) to perform qualitative and quantitative evaluations of enrofloxacin and ofloxacin in dairy products (raw milk and milk powder) and eggs (whole egg, albumen, and yolk). Trimethylsilyl diazomethane (TMSD) was applied as the precolumn derivatization reductant. The limits of detection (LODs) and limits of quantitation (LOQs) of enrofloxacin were 0.4 ~ 1.1 and 1.0 ~ 2.0 µg/kg, respectively. The LODs and LOQs of ofloxacin were 0.1 ~ 0.2 and 0.2 ~ 0.4 µg/kg, respectively. The recoveries of enrofloxacin and ofloxacin ranged from 79.78 to 92.33% and 78.26 to 90.79%, respectively. The RSDs were all less than 5.60%. The method was validated to satisfy the demand of the FAO & WHO (2014) standard. Moreover, successful utilization of this method is needed to satisfy the technical requirements of various laboratories.

Graphical Abstract