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

以高效能液相層析螢光法同時分析畜禽水產品中11種喹諾酮類抗菌劑殘留之研究

張菊香(Chui-Shiang Chang) ； 王維賢(Wei-Hsien Wang) ； 蔡清恩(Chin-En Tsai)

《藥物食品分析》 16卷6期 (2008/12) Pp. 87-96

摘要

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種喹諾酮抗菌劑殘留(marbofloxacin、norfloxacin、ciprofloxacin、lomefloxcain、danofloxacin、enrofloxacin、sarafloxacin、difloxacin、oxolinic acid、nalidixicacid、flumequine)。樣品以0.3%偏磷酸∶氰甲烷(1:1, v/v)萃取，經減壓濃縮去除乙腈後注入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%甲酸水溶液及乙腈組成進行梯度沖堤。空白肌肉組織添加3種濃度（25、50及250 ng/g；除了DAN添加濃度爲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種喹諾酮抗菌劑之添加試驗之平均回收率爲71.7至105.3%，定量極限爲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。

關鍵字

喹諾酮 ； 殘留 ； 高效能液相層析

並列摘要

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.

並列關鍵字

Quinolones ； residue ； HPLC