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KMID : 0380420020260040269
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Journal of Prventive Veterinary Medicine
2002 Volume.26 No. 4 p.269 ~ p.281
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Matrix Solid-Phase Dispersion (MSPD) for the Isolation and Liquid Chromatographic Determination of Fluoroquinolones in Eggs
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서계원/Seo, Kye-Won
이재일/이채용/김은선/이정치/Lee, Jae-Il/Lee, Chai-Yong/Kim, Eun-Seon/Lee, Jeong-Chi
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Abstract
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A multi-residue matrix solid-phase dispersion extraction and the liquid chromatographic determination of enrofloxacin, ciprofloxacin, norfloxacin and ofloxacin in eggs is described. Blank and fluoroquinolones fortified egg samples (0.5 g) containing oxalic acid 0.05 g and sodium sulfate (anhydrose) 0.5 g were blended with octadecylsilyl (C_(18), 40 m, 18% load, endcapped, 2 g) derived from silica. After homogenization, C_(18)/egg matrix was transferred to column made of 10 ml plastic syringe and filter paper, and compressed 4.0 4.5 ml volume. A column was washed with 8 ml of hexane followed by 8 ml of ethylacetate and dried under N2 gas. Fluoroquinolones were eluated with 8 ml of methanol under gravity. The eluate contained fluoroquinolones, was free from interferences when analyzed by high performance liquid chromatography with fluorescence detection. Correlation coefficients for the fluoroquinolones standard curves (linear regression analysis, n = 5) ranged from 0.99918 (± 0.0035) to 0.99985 (± 0.0002). Aveage recoveries of fortified samples were between 89.4 and 103.5%. The method comparared favorably with the classical method in terms of the sample size, analysis time and overalls costs.
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