以高效能液相層析串聯式質譜儀同時分析畜禽水產品中 18 種J諾酮類抗菌劑殘留之研究   全文下載

Simultaneous Determination of 18 Quinolone Residues in Marine and Livestock Products by Liquid Chromatography/Tandem Mass Spectrometry

建立簡單及有效之液相層析──電噴灑──串聯式質譜儀方法檢測牛奶、雞肉、豬肉、魚及蝦中18種?諾酮抗菌劑殘留，此方法能篩檢及確認包括12種兩性的?諾酮抗菌劑（marbofloxacin 、norfloxacin 、enrofloxacin 、 ciprofloxacin 、desethylene ciprofloxacin 、lomefloxacin 、danofloxacin 、 sarfloxacin 、difloxacin 、ofloxacin 、orbifloxacin 、enoxacin）及6種酸性的?諾酮抗菌劑（oxolinic acid 、nalidixic acid 、flumequine 、cinoxacin 、 piromidic acid 、pipemidic acid）。樣品之萃取液為含1%甲酸之乙?溶液，經減壓濃縮後以10%乙?定容，再以正己烷去脂。高效能液相層析分析條件為XDB C-8（150 mm × 4.6 mm, 5 μm）分離管柱，移動相由20 mM甲酸銨、0.1%甲酸水溶液及乙?組成進行梯度沖提，質譜儀使用正離子多重反應（MRM）模式。CCα及CCβ之測定乃參考歐盟2002/657/EC 指令及ISO 11843號標準，使用禁用物質之模式。本實驗條件下所測得之CCα 範圍為0.18至0.68 ng/g，CCβ 範圍為0.24至0.96 ng/g。"

A simple and efficient LC/ESI/MS/MS method was developed to determine 18 (fluoro)quinolone (QNs) residues in milk, chicken, pork, fish and shrimp. This method is capable of screening and confirming the presence of 12 amphoteric QNs (marbo-floxacin, norfloxacin, enrofloxacin, ciprofloxacin, desethylene ciprofloxacin, lomefloxacin, danofloxacin, sarfloxacin, difloxacin, ofloxacin, orbifloxacin and enoxacin) and 6 acidic QNs (oxolinic acid, nalidixic acid, flumequine, cinoxacin, piromidic acid and pipemidic acid). The drugs were extracted from matrix with acetonitrile containing 1% formic acid, diluted in 10% acetonitrile and defatted by extraction with hexane. The LC separation was conducted on an XDB C-8 (150 mm × 4.6 mm, 5 μm) column with gradient elution of 20 mM ammonium formate in 0.1% formic acid-acetonitrile as the mobile phase. Mass spectrum acquisition was completed in the positive ion mode by applying multiple reaction mode (MRM). The decision limit (CCα) and detection capability (CCβ), stated in the Decision No. 2002/657/EC and the ISO standard No.11843, have been calculated in the case of nonauthorized substance. The values of CCα ranged from 0.18 to 0.68 ng/g and CCβ ranged from 0.24 to 0.96 ng/g under specified conditions.