篇名 | 魚肉組織中丁香酚之QuEChERs萃取及液相層析串聯質譜法檢驗方法之開發 |
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卷期 | 52:2/3 |
並列篇名 | Development of QuEChERs-based Extraction and A Liquid Chromatographytandem Mass Spectrometry Method for Quantifying Eugenol Residues in Fish Tissues |
作者 | 趙偉博 、 黃志能 、 陳浩民 、 於柏伸 、 曾素香 |
頁次 | 059-065 |
關鍵字 | 魚肉組織 、 超高效液相層析串聯質譜儀 、 丁香酚 、 QuEChERs萃取 、 Fish tissue 、 Ultra high liquid chromatography/tandem mass spectrometer 、 Eugenol 、 QuEChERs extraction 、 Scopus 、 TSCI |
出刊日期 | 201404 |
本研究建立QuEChERs萃取方法並利用超高效液相層析串聯質譜 (ultra high liquid chromatography/tandem mass spectrometer, LC/MS/MS) 儀之負離子電灑法,以多重反應偵測 (multiple reaction monitoring, MRM) 模式分析魚肉 中之丁香酚。均質樣品用水分散後,加入1%醋酸之乙腈溶液配合QuEChERs萃取粉劑(硫酸鎂4 g、氯化鈉1 g、 檸檬酸三鈉二水結晶鹽1 g及檸檬酸氫二鈉半水結晶鹽0.5 g) 進行萃取,離心後之上清液經由primary secondary amine、C18及無水硫酸鎂淨化,並以ACQUITY UPLC HSS T3 C18 (1.8 μm, 2.1 × 100 mm) 管柱搭配甲醇及去離子水 做梯度流洗,再以串聯質譜儀分析,並運用基質對應檢量線 (matrix-matched calibration curve) 進行定量。結果顯 示,於空白魚類檢體中分別添加5、10及20 ng/g濃度之丁香酚標準品,其平均回收率為99.8-107.7%之間,變異 係數介於11.3-13.7%之間。本方法之定量極限為5 ng/g。
A QuEChERs (acronym of Quick, Easy, Cheap, Effective, Rugged, and Safe) extraction method based on ultra liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) in the negative mode using multiple reaction monitoring (MRM) was developed to quantify eugenol residues in fish tissues. The homogenized sample was dispersed in water, then extracted with acetonitrile containing 1% acetic acid, and salted out with QuEChERs extraction powder (containg 4 g magnesium sulfate, 1 g sodium chloride, 1 g trisodium citrate and 0.5 g disodium citrate sesquihydrate). The supernatant obtained from high speed centrifugation, was cleaned up using a dispersive solid-phase extraction (d-SPE) with primary secondary amine, C18 and anhydrous magnesium sulfate. Analysis was performed using liquid chromatography with an ACQUITY UPLC HSS T3 C18 Column (1.8 μm, 2.1 × 100 mm) coupled to an electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) with gradient elution of methanol and water. Quantitation was performed using a matrix-matched calibration curve. Recoveries at 5, 10 and 20 ng/g spiking levels ranged from 99.8 to 107.7% and the coefficients of variation were between 11.3 to 13.7%. The quantitation limit of this method is 5 ng/g.