본 연구는 불법적으로 수산물에 사용될 수 있는 염료 18종에 대한 안전관리 강화를 위해 정량 및 정성 분석이 가능한 LC-MS/MS를 적용하여 검증하기 위해 수행되었다 . 확립된 시험법은 CODEX CAC/GL-71 가이드라인에 따라 직선성, 정밀성 , 정량한계 및 회수율 등을 통해 유효성을 확인하였다 . 대상시료에 1% 아세트산을 함유한 아세토니트릴로 추출 후 C18 과 PSA로 정제하였다 . 본 실험에서 정량한계는 0.002 mg/kg 수준으로 정량한계를 포함한 농도에 따라 검량선을 작성하였고 모두 0.98 이상의 직선성을 확인하였다 . 또한 정확성은 63%-112% 이고, 정밀도는 15% 이하로 재현성이 우수하였다 . 국내 유통 중인 수산물 124 건을 수거하여 개발된 분석법의 적용성 검증과 안전성을 확인하고자 잔류실태조사를 실시 하였고 그 결과 7건이 미량으로 검출 되었고 부적합은 없었다 . 확립된 시험법은 수산물 안전관리에 활용할 수 있을 것으로 사료되는 바이다 .

A reversed-phase high-performance liquid chromatography with tandem mass-spectrometric detection was developed and validated for the simultaneous analysis of 13 quinolones (orbifloxacin, sarafloxacin, marbofloxacin, ofloxacin, enrofloxacin, danofloxacin, pefloxacin, ciprofloxacin, norfloxacin, difloxacin, oxolinic acid, flumequine, nalidixic acid) in pork. The drugs were extracted from homogenized sample using acidic buffer (2% trichloracetic acid) and acetonitrile with ethyl acetate. Analysis was performed by liquid chromatograph with tandem mass spectrometry (LC-MS/MS) in positive mode for all quinolones. Mass spectral acquisition was performed in the multi reaction monitoring mode (MRM), selecting two structurally significant transitions per compound. Good linear relationship (R2=0.999) was observed at 6 concentrations of 2.5～100 ng/g. Satisfied recoveries (73.3～105.4%) of all quinolones were demonstrated in spiked pork at three levels from 5 to 20 ng/g. The limits of quantitation (LOQs) for quinolones ranged from 0.25 to 5.0 ng/g.

A simple, selective and sensitive procedure for the confirmation of 14 sulfonamide antibacterials in milk was developed. The milk samples were homogenized, extracted and deproteinized by acetonitrile and defatted by n-hexane. Analysis was performed by liquid chromatography with tandem mass spectrometry (LC-MS/MS) in positive mode for all 14 analytes. Mass spectral acquisition was performed in the multi reaction monitoring mode (MRM), selecting two structurally significant transitions per compound. The calibrations were performed in sample matrixes and the interference effect of sample matrixes on the ionization was effectively eliminated. Good linear relationship (R2=0.992～ 0.999) were observed at 6 concentrations of 2.5～100 ng/g. Satisfied recoveries (86.3～110.2%) of all sulfonamides were demonstrated in spiked milk at three levels from 5 to 20 ng/g. The limits of quantitation (LOQs) for sulfonamides ranged from 0.25～2.1 ng/g.