利用液相層析串聯質譜儀進行食品中歐黴素及紅黴素殘留之同步檢測

歐黴素及紅黴素為人畜共通用藥，屬於14環巨環黴素類抗生素(Macrolides)，為中廣效性抗生素。本研究建立之歐黴素及紅黴素檢驗方法，移動相採用0.1%甲酸水溶法與乙腈(70:30, v/v)之混合液，以流速0.2mL/min 、注射量10μL，經Thermo BDS HYPERSIL C18分析管柱(2.1×50 mm, 3.0μm)層析後進入串聯質譜儀進行分析，歐黴素及紅黴素經由電灑游離正離子離子化可得母離子分別為m/z 688及734，歐黴素主要生成子離子片段為m/z 158、544，紅黴素為m/z 158、576，利用離子片段訊號之滯留時間、訊號面積及特徵子離子片段強度比，可做為歐黴素及紅黴素殘留檢測定性及定量之依據。萃取淨化之方法，經測試以0.2%偏磷酸與甲醇(6:4, v/v)之混合液，比較三種固相萃取匣（Oasis HLB, Oasis MAX及C18），結果以利用Oasis HLB固相萃取匣萃取及分析，可得到最佳之回收率及淨化效果，且具有良好之再現性。本方法在歐黴素及紅黴素檢出限量均為0.01μg/g(ppm)，平均回收率78.2%~86.4%。

關鍵字

歐黴素；紅黴素；液相層析串聯質譜儀

並列摘要

Oleandomycin and erythromycin are 14-membered ring macrolide antibiotics. A simple and reliable method using liquid chromatography-tandem mass spectrometry had been developed for determination of oleandomycin and erythromycin in beef; pork, chicken and sheep. The LC separation was performed on Thermo BDS HYPERSIL C18 column (2.1×50 mm, 3.0 μm) with 0.1% formic acid/acetonitrile (70:30, v/v) as the mobile phase at the flow rate 0.2 mL/min. The electrospray positive ionization produced the molecular related ions at m/z 688 and 734 for oleandomycin and erythromycin, respectively. Two characteristic transition reactions (m/z 688→158, 544; m/z 734→158, 576) in selected reaction monitoring were tested for detection and confirmation of oleandomycin and erythromycin, simultaneously. The analytes were extracted with 0.2% metaphosphoric acid/methanol (6:4, v/v) then cleaned up by three solid-phase extraction cartridges (Oasis HLB, Oasis MAX and Cl8), and had better results from Oasis HLB cartridges. The recoveries for oleandomycin and erythromycin analysis by developed method were 78.2%~86.4%. The limits of determination were 0.01 μg/g (ppm) for both oleandomycin and erythromycin analysis.

並列關鍵字

Oleandomycin ； Erythromycin ； Liquid Chromatography Tandem Mass Spectrometry ； LC/MS/MS

國際替代計量

利用液相層析串聯質譜儀進行食品中歐黴素及紅黴素殘留之同步檢測

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