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

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关键词：鸽蛋；柱前衍生-气相色谱-串联质谱法；氟喹诺酮类药物；残留量中图分类号：S859.796 文献标志码：A 文章编号：1671-4652（2025）05-0046-10

ABSTRACT： A pre-column derivatization-gas chromatography-tandem massspectrometry method （GC-MS/MS）was establishedforthesimultaneous determinationof enrofloxacin，ofloxacin，sarafloxacinand 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 300μL of trimethylsilyl diazomethane for 30min . The derivatives were subsequently analyzed by GC-MS/MSforconfirmatory analysis.The results showed thatthe 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 0.4-2.0μg⋅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 therequirements of veterinary drug residues in China.It provides robusttechnical foundation for the detection of multi-veterinary drug residues in poultry eggs and supports the development of relevant detection standards.

KEY WORDS：pigeon egg；pre-column derivatizationgaschromatography-tandemmasspectrometry;fluoroquinolones；residues

恩诺沙星（enrofloxacin，ENR）、氧氟沙星（ofloxacin，OFL）、沙拉沙星（sarafloxacin，SAR）和达氟沙星（danofloxacin，DAN）均属于第3代氟喹诺酮类抗生素，对众多革兰阴（阳）性菌有广泛的抗菌谱，其抗菌机制主要在于抑制细菌拓扑异构酶Ⅱ以及拓扑异构酶N，使细菌DNA的复制、转录和修复过程受阻[1]。（剩余16864字）