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 .

This study aimed to develop an analytical method for determination of 18 dyes in livestock and fishery products by liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The developed method was validated for linearity, accuracy, limit of quantifications (LOQ) and recovery based on the CODEX guideline (CAC/GL- 71). Target matrices (beef, pork, chicken, egg, milk, flatfish, eel, and shrimp) were extracted using acetonitrile (containing 1% of acetic acid) and then, purified with C18 and primary secondary amine (PSA). Calibration linearity was obtained (r 2>0.98) and LOQs were 0.002 mg/kg in animal products. The recoveries of dyes were ranged from 63 to 112% and relative standard deviations (RSDs, %) were less than 15%. The residues of 18 dyes were investigated in real samples (n=124) collected from retail markets in South Korea. As a result, a total of seven samples showed positive results for target analytes in fish samples. However, there was no violation according to the maximum residue limits set by the Korean Food Code. The proposed method will be used for routine analysis of dye residues in livestock and fishery products.

ABSTRACT
Materials and Methods
    Reagents and chemicals
    Preparation of stock and standard solutions
    Sample preparation
    LC-MS/MS analysis
    Method validation
Results and Discussion
    Optimization of LC-MS/MS conditions
    Optimization of extraction and purification
    Method validation
    Application and real sample monitoring
국문요약
References

• Hyunjin Park(Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation)
• Joohye Kim(Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation)
• Hui-Seung Kang(Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation) Correspondence to
• Byung-Hoon Cho(Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation)
• Jae-Ho Oh(Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation)