以液相層析串聯式質譜儀測定多重動物用藥在魚產品中分析方法之研究   全文下載

Multi-Residue Determination of Sulfonamide and Quinolone Residues in Fish Tissues by High Performance Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS)

本研究著重於以液相層析串聯式質譜儀法分析?諾酮類及磺胺類藥物，同時萃取多種藥物的方法開發，包括?諾酮類藥物四種（oxolininc acid 、enrofloxacine 、ciprofloxacine 、norfloxacine）以及磺胺類藥物四種（sulfamethoxypyridazine 、 sulfadoxine 、sulfadimidine 、sulfamerazine），方法確效根據歐盟法規所規範之確效參數；1.0 g樣品是經酸性氰甲烷溶液（0.5 mL 0.1%甲酸溶於7 mL氰甲烷）進行萃取，以LC-ESI-MS/MS分析。本研究結果發現此魚肉中，四種?諾酮類及磺胺類藥物之5.0 μg/kg的添加回收率分別為85 - 104%及75 - 94%，決策極限（CCα）分別為1.35 - 2.10 μg/kg和1.62 - 2.53 μg/kg，而偵測能力（CCβ）則分別為1.67 - 2.75 μg/kg與2.01 - 3.13 μg/kg。

A LC-MS/MS method was validated for the simultaneous quantification of 4 quinolones (oxolinic acid, enrofloxacine, ciprofloxacine, norfloxacine) and 4 sulfonamides (sulfamethoxypyridazine, sulfadoxine, sulfadimidine, sulfamerazine) on fish muscle following the Euro-pean Union’s (EU) criteria for the analysis of veterinary drug residues in foods. One gram of sample was extracted by acidic acetonitrile (0.5 mL of 0.1% formic acid in 7 mL of ACN), followed by LC-MS/MS analysis using an electrospray ionization interface. Typical recoveries of the 4 quinolones in the fish tissues ranged from 85 to 104%. While those of the sulfonamides ranged from 75 to 94% at the fortification level of 5.0 μg/kg. The decision limits (CCα) and detection capabilities (CCβ) of the quinolones were 1.35 to 2.10 μg/kg and 1.67 to 2.75 μg/kg, respectively. Meanwhile, the CCα and CCβ of the sulfonamides ranged from 1.62 μg/kg to 2.53μg/kg and 2.01μg/kg to 3.13 μg/kg, respectively.