柱前衍生结合气相色谱-串联质谱法测定鸽蛋中4种氟喹诺酮类抗生素残留量OA北大核心

A pre-column derivatization-gas chromatography-tandem mass spectrometry method(GC-MS/MS)was es-tablished for the simultaneous determination of enrofloxacin,ofloxacin,sarafloxacin and danofloxacin residues in pigeon eggs.The samples were extracted twice using 10％trichloroacetic acid in acetonitrile.The supernatant was purified using an Oasis PRiME HLB solid-phase extraction column,and then concentrated under nitrogen.The residues were reconstituted in methanol and derivatized with 300 μL of trimethylsilyl diazomethane for 30 min.The derivatives were subsequently an-alyzed by GC-MS/MS for confirmatory analysis.The results showed that the matrix-matched standard curves exhibited excellent linearity within their respective concentration ranges,with correlation coefficients(R2)exceeding 0.999 3.The limits of detection and quantification were 0.2-1.0 and 0.4-2.0 μg·kg-1,respectively.The recoveries were 78.30％-92.75％.The relative standard deviation,intra-day relative standard deviation and inter-day relative standard deviation were 2.11％-4.55％,1.04％-5.84％and 3.53％-6.33％,respectively.The method has high sensitivity,accurate qualitative and quantitative characteristics,and meets the requirements of veterinary drug residues in China.It provides robust technical foundation for the detection of multi-veterinary drug residues in poultry eggs and supports the develop-ment of relevant detection standards.