논문 상세보기
pp.94-98
HPLC-MS/MS를 이용하여 벌꿀의 동물용의약품 동시분석을 위한 분석법을 정립하고자 식품공전 중 벌꿀에 규격이 설정된 11종의 동물용의약품을 2개 그룹 Group 1 (streptomycine, dihydrostreptomycine, neomycine)과 Group 2 (oxytetracycline, enrofloxacin, ciprofloxacin, cymiazole, chloramphenicol, amitraz, coumaphos, fluvalinate)으로 나눠서 동시에 분석 할 수 있는 방법을 연구 하였다. 두 그룹모두 RT는 15분 이내였고, 검출한계는 0.0056~0.0643 μg/g, 정량한계는 0.0169~0.1948 μg/g으로 나타났으며 Group 1 (0.05~1.0 μg/g의 농도범위)과 Group 2 (0.01~1.0 μg/mL) 의 검량선을 작성한 결과 각 동물용의약품의 직선상관계수(R2)는 0.9917~0.9987, 0.9923~1.000으로 매우 양호한 상태를 보였고, 최종 농도가 0.25 μg/g, 1.0 μg/g에서의 회수율은 Group 1 65.1~80.6%, Group 2 64.2~90.3%를 나타났다, 또한 area 및 RT 에 대한 inter (n = 3), intra day (n = 6) RSD (%) 분석결과는 area는 10.92%이하, RT은 1.57% 이하로 나타나 양호한 수준을 보여 벌꿀 중 동물용의약품동시분석 방법으로 적합하다고 판단된다.
This study was conducted to establish the simultaneous analysis method for veterinary drug residues in honey by high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS). The eleven targeting veterinary drugs with honey test method in Korean Food Standards Codex were divided into Group 1 (streptomycine dihydrostreptomycine, neomycine) and Group 2 (oxytetracycline, enrofloxacin, ciprofloxacin, cymiazole, chloramphenicol, amitraz, coumaphos, fluvalinate) to be analyzed simultaneously. From the results, the retention time (RT) of the targeting drugs was within 15 min, the range of detection limits was 0.0056 to 0.0643 μg/g and the range of quantification limits was 0.0169 to 0.1948 μg/g. The coefficients of determination (R2) for Group 1 (0.05~1.0 μg/mL) and Group 2 (0.01~1.0 μg/mL) were 0.9917~0.9987 and 0.9923~1.000 respectively, and showed the good linearity. The recovery rates for Group 1 (final conc. 0.25 μg/g) and Group 2 (final conc. 1.0 μg/g) were 65.1~80.6% and 64.2~90.3% respectively. Also, the analysis results of inter day (n = 3) and intra day (n = 6) RSD (%) for area and retention time showed that the RSD (%) for area and retention time was below 10.92% and 1.57%. Therefore, the simultaneous analysis method of this study is evaluated to be a good test method for veterinary drug residues in honey.
표준품 및 시약
표준용액 조제
시료 전처리
장비 및 분석조건
Results and Discussion
시료전처리법 확립
MS/MS 조건
직선성
정밀성
회수율
검출한계 및 정량한계
국문 요약
References
