篇名 | 利用液相層析軌道捕捉式高解析度質譜儀進行果汁中 殘留農藥之快速篩檢 |
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卷期 | 52:2/3 |
並列篇名 | Fast Screening of Pesticide Residues in Juice by High Performance Liquid Chromatograph/Orbitrap High Resolution Mass Spectrometer |
作者 | 於柏伸 、 沈盈如 、 楊凱智 、 曾素香 、 高雅敏 、 闕麗卿 、 施養志 |
頁次 | 075-086 |
關鍵字 | 果汁 、 農藥 、 液相層析軌道捕捉式高解析度質譜儀 、 juice 、 pesticide 、 LC/high resolution Orbitrap MS 、 Scopus 、 TSCI |
出刊日期 | 201404 |
本研究建立以液相層析高解析度軌道眺質譜儀(liquid chromatograph/high resolution orbitrap mass spectrometer) 進行果汁檢體中殘留農藥之快速篩檢方法。前處理採用快速QuEChERS前處理技術,將果汁與1%醋酸之乙 腈、醋酸鈉及無水硫酸鎂等鹽類粉劑混合振搖萃取後離心取上層萃取液,以PSA (primary secondary amine)及 C18粉劑進行淨化。筛檢方式依質量準確度(accuracy)及同位素波峰相對離子強度(relative ion intensity)等參數 篩檢出檢體中可疑波峰,進一步與建立之農藥資料庫比對滯留時間,可快速篩檢鑑別400項以上農藥。進行 市售果汁13件檢體中殘留農藥之快速篩檢,結果於四件柳橙汁中篩檢出微量之貝芬替(carbendazim)、依滅列 (imazalil)及派美尼(pyrimethanil)等三項台灣核可使用於樹橋類作物之農藥,以基質匹配檢量線(matrix matched calibration curve)進行定量,檢出濃度為0.014〜0.028ppm,遠低於樹橋類農藥殘留量標準3.0〜7.0ppm。
A fast screening method was developed for determining pesticide residues in juice using liquid chromatograph/electrospray ionization high resolution orbitrap mass spectrometer (LC/Orbitrap MS). For sample preparation, the QuEChERS technique was applied to extract pesticide residues from juice samples using 1% acetic acid in acetonitrile containing sodium acetate and anhydrous magnium sulphate. After shaking and centrifugation, an aliquot of the organic phase (upper layer) was subjected to further clean up using dispersive soild-phase extraction (d-SPE) with primary-secondary amine (PSA) and octadecyl-bonded silca (C18) sorbents. A fast screening LC/Orbitrap MS method was established for more than 400 pesticides, based on mass accuracy, isotope relative ion intensity and LC retention time from the established pesticide database. Of thirteen samples analyzed using this established fast screening method, carbendazim, imazalil, and pyrimethanil, which were pesticides registered for orange crop in Taiwan, were detected in 4 orange juice samples. Matrix matched calibration curves were used for quantification. The residues of these pesticides in juice samples ranged from 0.014 to 0.028 ppm, much lower than maximum residne limits (MRLs) of orange crops (3.0~7.0 ppm).