本研究開發出一套簡單快速且符合綠色化學的萃取方法，用於檢測環境水樣中防腐劑Parabens的殘留。Parabens廣泛應用於個人護理產品中，其乃一種內分泌干擾物質，經使用後產生的民生廢水排放至自然環境，其殘留會對人類健康和生態環境帶來不良影響。 本研究使用的是近年十分熱門的吸附材料——金屬有機骨架材料(Metal Organic Frameworks, MOFs)，其具有高比表面積、良好的熱穩定性及多孔結構等特性。而本研究透過無溶劑法成功快速製備MIL-101(Cr)，作為分散式微固相萃取法(Dispersive micro solid phase extraction，簡稱D-µ-SPE)之吸附劑，其表現出良好的吸附效果和穩定性，並利用高效液相層析串聯電灑游離（-）-四極桿飛行時間式質譜儀(UHPLC-ESI（-）-QTOF-MS)進行後續的分析檢測。 藉由Multilevel categoric design(MLCD)和Box-Behnkne Design(BBD)中變異數分析(Analysis of variance, 簡稱ANOVA)，針對實驗條件進行優化，減少實驗時間和溶劑使用量，以檢測水樣中的7種Parabens。 本方法的偵測極限(LOD)為0.002-0.5 ng/mL，展現優異的靈敏度；在Intra-day和Inter-day的測試中相對標準偏差(RSD)低於8 %，萃取回收率介於61％-120%之間，表現出良好的再現性和穩定性，並於真實環境水樣中檢測到防腐劑MeP和PrP的微量殘留。 整體而言，本研究方法使用無溶劑合成的金屬有機骨架材料，並搭配分散式微固相萃取法，實驗過程大幅降低實驗時間和有機溶劑使用量，符合綠色化學之準則，是一種簡易、高效且對環境友善檢測防腐劑Parabens的分析方法。;Parabens are widely used in personal care products. They have been classified as endocrine disrupting chemicals (EDCs). Wastewater generated by the people′s livelihood is discharged into the natural environment, and the residues will have adverse effects on human health and the ecological environment. In this study, we prepared metal-organic frameworks (Metal Organic Frameworks, MOFs) as adsorbents, which is a group of popular novel adsorbents in recent years. MOFs have the characteristics of high surface area, good thermal stability and porous structure. In this study, MIL-101(Cr) was successfully and quickly prepared by a solvent-free method. As an adsorbent for dispersive micro solid phase extraction (D-µ-SPE), MIL-101(Cr) displayed good adsorption effect and stability. Ultrahigh-performance liquid chromatography and electrospray ionization (-)-quadrupole time-of-flight mass spectrometer (UHPLC-ESI(-)-QTOF-MS) was used for detection and quantitation. By means of Analysis of variance (ANOVA) in Multilevel categoric design (MLCD) and Box-Behnkne Design (BBD), the experimental conditions were optimized and the experimental time and solvent usage were reduced. The developed method was validated after optimization. The method provided low limit of detection (LOD), range from 0.002-0.5 ng/mL, and showed excellent sensitivity. The relative standard deviation (RSD) is less than 8% and the extraction recovery is range from 61% to 120% for both intra- and inter-day analysis, which revealed good reproducibility and stability. The method was applied for the detection of parabens residues in real water samples successfully.
