• 한국수산과학회지
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• 제42권4호
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• pp.329-334
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• 2009

The residues of fluoroquinolones in Olive flounder (Paralichthys olivaceus) and Black rockfish (Sebastes schlegeli) were investigated after oral doses of 20 mg/kg for 30 days. Blood samples were taken at 5 hours, 10 hours, 1 day, 2 days, 3 days, 5 days, 7 days, 9 days, 13 days, 20 days and 30 days after treatment. The concentrations of fluoroquinolones were detected by high performance liquid chromatography using a UV detector. The recovery rates of fluoroquinolones in fish samples ranged from 92.0-99.7%, 93.4-97.5% and 93.0-97.9% for treatment of 0.1, 0.5, and $1.0{\mu}g/g$, respectively. Ciprofloxacin, enrofloxacin, norfloxacin and sarafloxacin were detected in the blood of the olive flounder at 10 hours, 10 hours, 1 day and 10 hours after treatment with $6.43{\mu}g/g$, $6.07{\mu}g/g$, $11.83{\mu}g/g$ and $11.02{\mu}g/g$ as maximum level, respectively. Ciprofloxacin, enrofloxacin, norfloxacin and sarafloxacin were detected in the blood of black rockfish 1 day, 1 day, 1 day and 10 hours after treatment with $8.26{\mu}g/g$, $8.03{\mu}g/g$, $7.29{\mu}g/g$ and $9.38{\mu}g/g$ as maximum level, respectively. However, ciprofloxacin, enrofloxacin, norfloxacin and sarafloxacin were not detected in olive flounder samples at 20, 30, 20 and 20 days after treatment in any experiments (

• 한국수산과학회지
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• 제43권6호
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• pp.623-628
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• 2010

The distribution of fluoroquinolones was investigated in the carp (Cyprinus carpio) and eel (Anguilla japonica) after an oral dose of 20 mg/kg body weight/day for 35 days. Blood samples were collected at 5 and 10 hours and 1, 2, 3, 5, 7, 9, 13, 20, 30, and 35 days after treatment. The fluoroquinolone concentrations were determined high- performance liquid chromatography with an ultraviolet detector. The recovery rates of fluoroquinolones in the fish samples ranged from 91.4-96.6, 91.2-96.5, and 90.4-98.6% for concentrations of 0.1, 0.5, and $1.0\;{\mu}g/g$, respectively. In the blood of carp, ciprofloxacin, enrofloxacin, norfloxacin, and sarafloxacin reached maximums level of 11.03, 9.37, 9.10, and $9.81\;{\mu}g/g$ 10 hours, 1 day, 10 hours, and 10 hours after treatment, respectively. In the eel blood, these reached maximum levels of 12.65, 11.18, 11.91, and $8.74\;{\mu}g/g$ all at 10 hours. Carp sample concentrations of ciprofloxacin, enrofloxacin, norfloxacin, and sarafloxacin were not measurable 20, 30, 20, and 20 days after treatment, respectively, in all experiments (

• 한국식품과학회지
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• 제42권5호
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• pp.521-526
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• 2010

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.

• 한국식품위생안전성학회지
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• 제23권4호
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• pp.324-329
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• 2008

본 논문에서는 식품 중 퀴놀론계(QNs) 합성항균제(marbofloxacin, norfloxacin, danofloxacin, ciprofloxacin, enrofloxacin, difloxacin, sarafloxacin, oxolinic acid 그리고 flumequine) 9종을 분석하기 위하여, 액-액 추출 과정을 거쳐서 형광검출기가 장착된 액체크로마토그래피를 이용하여 QNs를 효율적으로 동시 분석하는 방법을 확립하였다. 컬럼은 Zorbax Eclipse XDB-C8($150\;mm{\times}4.6\;mm,\;5{\mu}m$), 이동상 용매는 200mM ammonium acetate buffer (pH 4.5)와 ACN로 기울기 용리를 사용하였으며, 유속은 1.5 ml/min, 그리고, 주입량은 $10{\mu}l$로 설정하여 분석하였다. 확립된 분석조건으로, 표준검정 곡선은 $10-500{\mu}g/kg$의 농도범위에서 상관계수가 0.9989 이상의 양호한 직선성을 나타내었으며, 회수율은 50, 100 그리고 $500{\mu}g/kg$의 농도에서 89.6-106.5%로, 향상된 추출효율을 나타내었다. 검출한계는 $1-16{\mu}g/kg$이었고, 정량한계는 $3-47{\mu}g/kg$이었으며, 일내(intra-day)와 일간(inter-day) 정밀도(CV%)는 0.2-15.0%, 0.5-11.7%이었다. 따라서, 확립된 분석방법은 광어 및 계란 중의 QNs을 효과적으로 분석하는데 이용될 수 있을 것으로 사료된다.

• 한국동물위생학회지
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• 제42권4호
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• pp.289-296
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• 2019

A novel rapid procedure with liquid chromatography tandem mass spectrometry (LC-MS/MS) detection has been developed by changing various conditions including sample preparation such as QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) methodology. This work has been involved the optimization and validation of detection method for fluoroquinolones which are widespread used in livestock especially in the chicken. Five grams of homogenized chicken muscle were extracted with QuEChERS EN and acetonitrile containing 5% formic acid and cleaned with anhydrous magnesium sulfate and C₁₈ sorbent. The separation was performed on Acquity UPLC HSS T3 (2.1 mm×100 mm, 1.8 ㎛) column. The mobile phase A and B were composed of water containing 0.1% formic acid and acetonitrile containing 0.1% formic acid, respectively. Flow rate was 0.25 mL/min and column temperate was 40℃. LC-MS/MS with multiple reaction monitoring has been optimized for ten fluoroquinolones (ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, marbofloxacin, norfloxacin, ofloxacin, orbifloxacin, pefloxacin and sarafloxacin). The method developed in this study has been presented good linearity with correlation coefficient (R²) of 0.9971~0.9998. LOD and LOQ values ranged from 0.09 to 0.76 ppb and from 0.26 to 2.29 ppb, respectively. The average recoveries were from 77.46 to 111.83% at spiked levels of 10.0 and 20.0 ㎍/kg. Relative standard deviation (%) ranged 1.28~11.90% on intra-day and 3.10~8.38 % on inter-day, respectively. This analysis method was applicable to the livestock residue laboratories and was expected to be satisfactory for the residue surveillance system.