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    题名: 開發綠色磁性金屬有機骨架材料結合磁性固相 萃取法檢測環境水樣中二苯甲酮殘留的研究
    作者: 李尚蓉;Li, Shang-Rong
    贡献者: 化學學系
    关键词: 超高效液相層析儀串聯四極桿飛行時間式質譜儀;二苯甲酮類化合物;金屬有機骨架;磁性固相萃取;(UHPLC-QTOF-MS);Benzophenones (BPs);metal-organic frameworks (MOFs);(magnetic solid phase extraction(MSPE)
    日期: 2024-06-04
    上传时间: 2024-10-09 15:19:40 (UTC+8)
    出版者: 國立中央大學
    摘要: 本研究開發一種靈敏、簡單、快速、方便、消耗較少量吸附材料、不須離心機械力輔助,且對環境友善的檢驗方法,用於檢測環境水樣中五種benzophenones (BPs)汙染物之殘留。
    環境水樣中以磁性金屬有機骨架當作吸附材料。金屬有機骨架中加入Fe3O4透過簡單的靜置組裝合成磁性金屬有機骨架(Fe3O4@ZIF-8),磁性吸附劑的優勢為簡單、高效和節省離心時間。本研究以磁性固相萃取法(Magnetic Solid Phase Extraction,MSPE)進行樣品前處理,以超高效液相層析儀串聯電灑游離法(+)四極桿飛行時間式質譜儀(UHPLC-ESI(+)-QTOF-MS)分析。
    前處理實驗中,先以單因子對實驗條件進行選擇及優化,再以實驗設計探討多因子間的交互關係,實驗設計只須較少的實驗次數,即可得到最優化的實驗條件,以此降低實驗時間和耗材成本。先以Multilevel categoric design (MLCD)實驗設計進行非數值因子的最佳化。再以Box-Behnkne Design (BBD) 實驗設計進行數值因子的最優化。
    本研究開發的方法之偵測極限(LOD)及定量極限(LOQ)分別介於 0.05-0.3 ng/mL 及 LOQ : 0.2-2 ng/mL。再以 Intra day & Inter day 檢測其精密度和再現性,相對標準偏差(RSD)皆小於8%,表示此方法有良好的再現性,且在環境水樣中檢測到benzophenones (BPs) 的殘留。研究結果得知本研究開發的方法是一種簡單、快速且相對環境友善的檢測方法。;This research developed a simple, efficient, and environmentally friendly analytical method for the determination of five frequently found benzophenones (BPs) residues in our aquatic environment, and no need for time-consuming centrifugal mechanical force assistance.
    A magnetic zeolitic imidazolate framework‑8 (Fe3O4@ZIF-8) was synthesized by a static self-assembled method and applied as an adsorbent for the magnetic solid phase extraction (MSPE) technique. MSPE was then coupled with ultra-high performance liquid chromatography electrospray ionization (+)-quadrupole time-of-flight mass spectrometry (UHPLC-ESI (+)-QTOF-MS) to determine five target BPs residues in water samples. Comparison with traditional dispersive micro solid-phase extraction, the magnetic adsorbent of MSPE is the key factor affecting the adsorption effect during a sample pretreatment due to the magnetic adsorbent is quickly separated from the sample solution by applying an external magnetic field (no centrifugation), allowing the simple and convenient isolation of analytes.
    One-factor-at-a-time approaches were conducted initially to select experimental conditions, and then experimental designs approaches were applied to explore the interaction between multiple experimental factors. Application of experimental designs minimized the number of experimental runs requiring to obtain the optimal conditions, thus reducing experimental time and the costs. In this study, multilevel categoric design (MLCD) was firstly used for the screening of non-numeric factors, and followed by Box-Behnken Design (BBD) for optimization of numeric factors. After optimization, the limits of detection (LOD) and limits of quantification (LOQ) of the method ranged between 0.050.3 ng/mL and 0.22 ng/mL, respectively. Precision was evaluated using intra-day and inter-day analyses, with relative standard deviations (RSD) of all below 8%, indicating good repeatability of the method. A preliminary analysis of the surface water revealed that 2- hydroxy-4-methoxybenzophenone (BP-3) was the most common BPs present in our aquatic environment, likely due to its widespread applications and slow rate of degradation.
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