篇名 | 動物食品組織中安保寧之液相層析串聯質譜法檢驗方法開發 |
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卷期 | 53:4 |
並列篇名 | Development of a Liquid Chromatography-tandem Mass Spectrometry Method for Quantifying Amprolium Residues in Animal Food Tissues |
作者 | 陳浩民 、 趙偉博 、 黃志能 、 於柏伸 、 廖家鼎 、 曾素香 、 高雅敏 |
頁次 | 160-170 |
關鍵字 | 超高效液相層析串聯質譜法 、 安保寧 、 七氟丁酸 、 Amprolium 、 Ultra high liquid chromatography/tandem mass spectrometry 、 Heptafluorobutyric acid 、 Scopus 、 TSCI |
出刊日期 | 201508 |
本研究建立以超高效液相層析串聯質譜儀(ultra high liquid chromatography/tandem mass spectrometer, LC/MS/ MS)之正離子電灑法,配合多重反應偵測(multiple reaction monitoring, MRM)模式分析雞蛋、雞肉、牛肉及 牛肝等動物食品中之安保寧含量。均質樣品以含1%甲酸之80%甲醇進行萃取,離心後之上清液經由primary secondary amine及C18淨化後,再以LC/MS/MS分析並運用基質匹配檢量線進行定量。層析條件方面,以 Acquity BEHC18, 1.7m,2.1 x 100 管柱搭配含20 mM七氟丁酸溶液及含0.1%甲酸之乙腈做梯度沖提,可達 到良好層析效果。確效試驗上,於空白雞蛋、雞肉、牛肉及牛肝檢體中分別添加0.02、0.05及0.1 yg/g之安保寧 對照用標準品,其同日內五重複之回收率介於79.3-102.5%,變異係數介於1.4-5.4%之間,符合本署食品化學檢 驗方法之確效規範,本方法定量極限為0.02 g/g。
This study presented a method for analyzing amprolium residues in chicken eggs, chicken meat, beef and beef livers by ultra high liquid chromatography/tandem mass spectrometer (LC/MS/MS) under a multiple reaction monitoring (MRM) mode with positive electrospray ionization. Homogenized samples were extracted with 80% methanol solution containing 1% formic acid. After centrifugation, the supernatant was cleaned up by primary secondary amine (PSA) and C18. Analysis was performed using LC/MS/MS and matrix-matched calibration was used to quantity the analyte. Acquity® BEH C18 column (1.7 μm, 2.1 × 100 mm) with gradient elution under 20 mM heptafluorobutyric acid solution and acetonitrile containing 0.1% formic acid can reach good sample separation. Validation was conducted by spiking 0.02, 0.05 and 0.1 μg/g amprolium in chicken eggs, chicken meat, beef and beef livers. The recoveries of amprolium for four tissues ranged from 79.3-102.5% and the coefficients of variation was between 1.4-5.4%. The quantitation limit of the above method is 0.02 μg/g.