Combining GC-MS/MS with a LLE-SPE sample pretreatment step to simultaneously analyse enrofloxacin and ofloxacin
Maoda Pang1, Junjie Xu2, Yayun Tang2
1Key Laboratory of Control Technology and Standard for Agri-product Safety and Quality, Key Laboratory of Food Quality and Safety of Jiangsu Province-State Key Laboratory Breeding Base, Institute of Food Safety and Nutrition, Jiangsu, Academy of Agricultural Sciences, Nanjing 210014, PR China.
Abstract:
A widely applicable original gas chromatography-tandem mass spectrometry (GC-MS/MS) method was explored to qualitatively and quantitatively measure enrofloxacin and ofloxacin residues in chicken tissues and pork. The experimental samples were processed based on liquid-liquid extraction (LLE) and solid-phase extraction (SPE). Trimethylsilyl diazomethane (TMSD) was chosen to react derivatively with enrofloxacin and ofloxacin. In total, 78.25% ∼ 90.56% enrofloxacin and 78.43% ∼ 91.86% ofloxacin was recovered from the blank fortified samples. The limits of detection (LODs) were 0.7-1.0 μg/kg and 0.1-0.2 μg/kg, respectively. The limits of quantitation (LOQs) were 1.6-1.9 μg/kg and 0.3-0.4 μg/kg, respectively. It was verified that various experimental data met the requirements of the FAO & WHO (2014) for the detection of veterinary drug residues. Real samples obtained from local markets were analysed using the established method, and no residues of enrofloxacin or ofloxacin were detected in the samples.
