以高效能液相層析螢光法同時分析畜禽水產品中11 種J諾酮類抗菌劑殘留之研究   全文下載

Simultaneous Determination of Eleven Quinolones Antibacterial Residues in Marine Products and Animal Tissues by Liquid Chromatography with Fluorescence Detection

建立簡單及有效之多重分析方法檢測雞肉、豬肉、魚及蝦中11 種?諾酮抗菌劑殘留（marbofloxacin、norfloxacin、ciprofloxacin、lomefloxcain、danofloxacin、enrofloxacin、sarafloxacin、difloxacin、oxolinic acid、nalidixic acid、flumequine）。樣品以0.3% 偏磷酸：氰甲烷（1：1, v/v）萃取，經減壓濃縮去除乙?後注入OASIS HLB 固相萃取匣淨化。高效能液相層析分析條件使用以symmetry column C-18（250 mm × 4.5 mm i.d., 5 μm）管柱分離，配合3 段式程式螢光偵檢器偵測，移動相由0.1% 甲酸水溶液及乙?組成進行梯度沖堤。空白肌肉組織添加3 種濃度（25、50 及250 ng/g；除了DAN 添加濃度為6.25, 12.5 及62.5 ng/g）建立線性、偵測極限、定量極限、精密度及精確度之確效試驗。11 種?諾酮抗菌劑之添加試驗之平均回收率為71.7 至105.3%，定量極限為5.0 至28.0 ng/g。結果顯示本方法簡單、快速、敏感且適合例行性分析工作。"

A simple and efficient multiresidue method was developed for determining 11 quinolones (QNs; marbofloxacin, norfloxacin, ciprofloxacin, lomefloxacin, danofloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid, nalidixic acid and flumequine) in chicken, pork, fish and shrimp. The analytes were extracted with 0.3% metaphosphoric acid and acetonitrile (1:1, v/v), followed by a HLB cartridge clean-up procedure. The HPLC separation was carried out on a symmetry column C-18 (250 mm × 4.5 mm i.d., 5 μm) with linear gradient elution of 0.1% formic acid and acetonitrile as mobile phase and programmable fluorescence detection. The method was validated by spiking blank animals tissues at three different levels (25, 50 and 250 ng/g; except 6.25, 12.5 and 62.5 ng/g for DAN) while the linearity, detection limit, quantification limit, precision and accuracy were checked. Mean recoveries of 11 QNs from edible animal tissues were 71.7-105.3%. The limits of quantification in different muscle tissues ranged from 5.0 to 28.0 ng/g. The results showed this method was simple, rapid, sensitive and suitable for routine tests.