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KMID : 1023520190420040289
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Korean Journal of Veterinary Service
2019 Volume.42 No. 4 p.289 ~ p.296
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The development and validation of a novel liquid chromatography tandem mass spectrometry (LC-MS/MS) procedure for the determination of fluoroquinolones residues in chicken muscle using modified QuEChERS (quick, easy, cheap, effective, rugged and safe) method
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Park Sun-Jin
Kim Hyo-Bi
Choi Byung-Kook
Hong Chung-Oui
Lee Seon-Young
Jeon In-Hae
Lee Su-Young
Kwak Pil-Hee
Park Sung-Won
Kim Yong-Sang
Lee Kwang-Jick
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Abstract
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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°C. 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 μg/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.
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KEYWORD
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Fluoroquinolones, QuEChERS, Chicken, Muscle, LC-MS/MS
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