以震盪輔助-深共熔溶劑-液液微萃取法快速檢測環境水樣中微囊藻毒素殘留

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题名:	以震盪輔助-深共熔溶劑-液液微萃取法快速檢測環境水樣中微囊藻毒素殘留
作者:	陳詠志;chen, yung-chih
贡献者:	化學學系
关键词:	微囊藻毒素;深共熔溶劑;超高效液相層析串聯質譜儀;震盪式輔助-DES-液液微萃取法;Microcystin;Deep Eutectic Solvents;UHPLC-QTOF-MS;VA-DES-LLME
日期:	2019-07-16
上传时间:	2019-09-03 14:26:49 (UTC+8)
出版者:	國立中央大學
摘要:	優養化是水中植物、藻類過度繁殖所引起，不僅會造成水質惡化及惡臭，大量繁殖的藻類甚至會產生微囊藻毒素 (Microcystin)，而在多種異構體中 Microcystin-LR (MC-LR) 最為普遍且毒性最強。除了暴露於環境水體中，人類也可能透過食物鏈而接觸到微囊藻毒素，故有必要開發一套快速方法檢測水環境中 Microcystin 濃度。本研究開發出一套快速、有效、低花費、且對環境友善的萃取方法來檢測水中的微囊藻毒素濃度。利用簡單合成的方式，合成出新穎的綠色化學溶劑-深共熔溶劑（Deep Eutectic Solvents, 簡稱 DES）作為萃取劑，再利用震盪輔助-DES-液液微萃取(Vortex assisted-DES-liquid-liquid microextraction (VA-DES-LLME)) 進行樣品前處理，並結合超高效液相層析串聯質譜儀 (UHPLC- qTOF-MS) 做定量檢測。並利用實驗設計 (statistical experimental design) 法中的 Box-Behnken design (BBD) 及變異數分析 (analysis of variance, ANOVA) 來做VA-DES-LLME 最佳化的條件探討。萃取的最佳化條件為：將5 mL 去離子水或水樣放入尖底離心管中，溶液調成酸性，加入 900 µL DES 和 1.4 mL THF，使用 vortex 震盪 50 s ，以 5000 rpm 的轉速離心 5 分鐘，取上層溶液加入甲醇定容為 1 mL，取其中 2 µL 進樣 UHPLC- qTOF-MS 進行檢測。本實驗 MC-LR 及 MC-YR 線性範圍為 1-100 μg/L，決定係數皆 0.999 以上，定量極限 (LOQ) MC-LR 與 MC-YR 分別為 0.4 與 0.5 ng/mL，精密度以相對標準差 (RSD) 表示，皆小於 11%，準確度以回收率表示，在 100 至 126 %間，顯示此方法穩定且具有良好的再現性。然在目前所收集的環境水樣檢測中，微囊藻毒素的含量皆低於本方法的偵測極限。;The eutrophication is caused by the over-breeding of plants and algae in the rivers and lakes, which not only causes deterioration of water quality and leading to malodor, but also produces microcystins in various isoforms. Among them, the most common and toxic microcystins is Microcystin-LR (MC-LR). In addition to exposure to aquatic system, humans may also be exposed to microcystins through the food chain, so it is necessary to develop a rapid and reliable method for the determination of microcystin residues in surface water. This study developed a fast, efficient, low-cost and environmentally friendly extraction method to detect two common detected microcystins: MC-LR and MC-YR, in surface water samples. Firstly, using a simple method to produce deep eutectic solvents (DESs), a group of novel “green” solvents, as an extractant, and then Vortex assisted-DES-liquid- liquid microextraction (VA-DES-LLME) was employed for sample preparation and combined with Ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-qTOF-MS) was used for quantitative detection. The parameters of VA-DES-LLME were optimized by multivariate statistic Box-Behnken design (BBD) and analysis of variance (ANOVA). The optimal extraction conditions were: 5 mL of water sample was placed in a sharp-bottomed centrifuge tube, and the solution was made acidic (pH = 2). DES (900 μL) and THF (1.4 mL) were added, and vortexed for 50 s, and then centrifuged at 5000 rpm for 5 minutes. The supernatant was reconstituted with methanol to a volume of 1 mL, and then 2 μL of extractant was directly injected into UHPLC-qTOF-MS for quantitative detection. The linear ranges of MC-LR and MC-YR was 1-100 μg/L, the coefficient of determination (r2) was above 0.999, and the limit of quantitation (LOQ) of MC-LR and MC-YR were 0.4 and 0.5 ng/mL, respectively. The relative standard deviation (RSD) was less than 11%, and in terms of recovery, the accuracy were between 100% and 126%. This method displayed to be stable and has good reproducibility. Although, for the collected water samples, the content of MC-LR and MC-YR were lower than those of the LOQs of the method. The developed method is sensitive enough to meet the requirement of the World Health organization (WHO) proposed monitoring program. In this program, the maximum allowance concentration in drinking water of microcystins is 1.0 ng/mL
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