Establishment of an Analytical Method of Fluoroquinolones in Milk by HPLC

A high-performance liquid chromatography (HPLC) method was established for the determination of fluoroquinolones in milk. Protein was removed by using trichloroacetic acid in order to increase a mean recovery of milk. The extracts were using $Strata^{TM}$-X solid-phase extraction cartridge. The analytes were detected by HPLC on a $C_{18}$ column. HPLC method with fluorescence detection system (Ex: 278 nm, Em: 456 nm) provided a high degree of sensitivity in detecting fluoroquinolones. The limits of quantitation (LOQ) and mean recoveries of fluoroquinolones were 40 ${\mu}g$/kg and 73.6-95.2% (ofloxacin), 10 ${\mu}g$/kg and 77.3-91.9% (norfloxacin), 20 ${\mu}g$/kg and 91.6-94.3% (ciprofloxacin), 10 ${\mu}g$/kg and 81.0-87.8% (enrofloxacin), 10 ${\mu}g$/kg and 71.3-81.0% (sarafloxacin), 10 ${\mu}g$/kg and 89.4-90.8% (orbifloxacin), 2 ${\mu}g$/kg and 69.4-85.5% (danofloxacin).

HPLC를 이용한 우유에서의 fluoroquinolones 시험법 확립

본 연구에서는 우유에서 플루오르퀴놀론계 합성 항균제의 확인과 정량을 위하여 HPLC를 이용한 방법을 개발하였다. 우유 내 단백질을 제거하기 위하여 삼염화초산을 사용하였고 아세토니트릴로 추출하였다. 그리고 $Strata^{TM}$-X 카트리지로 정제한 후 $C_{18}$ 칼럼을 이용한 HPLC로 분석하였다. 높은 감도를 얻기 위하여 형광 검출기를 사용하였고, 최적파장 Ex: 278 nm, Em: 456 nm에서 분석한 결과 우유 내에서 정량한계와 회수율은 각각 ofloxacin 40 ${\mu}g$/kg, 73.6-95.2%, norfloxacin 10 ${\mu}g$/kg, 77.3-91.9%, ciprofloxacin 20 ${\mu}g$/kg, 91.6-94.3%, enrofloxacin 10 ${\mu}g$/kg, 81.0-87.8%, sarafloxacin 10 ${\mu}g$/kg, 71.3-81.0%, orbifloxacin 10 ${\mu}g$/kg, 89.4-90.8%, danofloxcin 2 ${\mu}g$/kg, 69.4-85.5%이었다.