Simultaneous Analysis for Veterinary Drug Residues in Honey by HPLC/MS/MS

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 $0.0643{\mu}g/g$ and the range of quantification limits was 0.0169 to $0.1948{\mu}g/g$. The coefficients of determination ($R^2$) for Group 1 ($0.05{\sim}1.0{\mu}g/mL$) and Group 2 ($0.01{\sim}1.0{\mu}g/mL$) were 0.9917~0.9987 and 0.9923~1.000 respectively, and showed the good linearity. The recovery rates for Group 1 (final conc. $0.25{\mu}g/g$) and Group 2 (final conc. $1.0{\mu}g/g$) 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.

HPLC-MS/MS를 이용한 벌꿀 중 동물용의약품 동시분석방법 연구

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 그룹 모두 RT는 15분 이내였고, 검출한계는 $0.0056{\sim}0.0643{\mu}g/g$, 정량한계는 $0.0169{\sim}0.1948{\mu}g/g$으로 나타났으며 Group 1 ($0.05{\sim}1.0{\mu}g/g$의 농도범위)과 Group 2 ($0.01{\sim}1.0{\mu}g/mL$)의 검량선을 작성한 결과 각 동물용의약품의 직선상관계수($R^2$)는 0.9917~0.9987, 0.9923~1.000으로 매우 양호한 상태를 보였고, 최종 농도가 $0.25{\mu}g/g$, $1.0{\mu}g/g$에서의 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 동물용의약품 동시분석 방법으로 적합하다고 판단된다.