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    Please use this identifier to cite or link to this item: http://ir.lib.ncu.edu.tw/handle/987654321/71274


    Title: 以超音波輔助分散式液液微萃取結合同步衍生快速檢測水樣中防腐劑成分
    Authors: 謝智忠;Hsieh,Chih-Chung
    Contributors: 化學學系
    Keywords: 對羥基苯甲酸酯;超音波輔助分散式液液微萃取;同步衍生;氣相層析質譜儀;Parabens;UADLLME;in-situ derivatization;GC-MS
    Date: 2016-06-20
    Issue Date: 2016-10-13 12:39:27 (UTC+8)
    Publisher: 國立中央大學
    Abstract: 對羥基苯甲酸酯 (p-hydroxybenzoic acids, Parabens) 作為市面上的防腐劑已經有超過80年的歷史,常添加於沐浴乳、化妝品、藥品及食物中,其價格低廉、無氣味,不易變色、硬化或泥漿化,被世界廣泛接受。但最近研究顯示對羥基苯甲酸酯可能具有雌激素活性、致癌性、造成皮膚病變、刺激眼睛等,為潛在內分泌干擾物。因此,檢測對羥基苯甲酸酯在環境中的濃度是不可避免的趨勢。

    本研究開發出一套簡單有效、成本低且快速檢測的方法。使用超音波輔助分散式液液微萃取 (Ultrasonic-assisted dispersive liquid-liquid microextraction, UADLLME) 進行前處理,搭配同步 (in-situ) 衍生化,同時進行萃取及衍生,再利用GC-MS檢測水樣中對羥基苯甲酸酯的含量。

    超音波輔助分散式液液微萃取最佳化條件為:將600 μL 異丙醇、300 μL 二氯甲烷和20 μL MTBSTFA+1%TBDMSCl 快速注入含有0.5 g NaCl的 10 ml 水樣中,置於超音波震盪機震盪1 分鐘後,以 4500 rpm 速率離心 10 分鐘,分離有機層及水層,之後放入微波爐中,以 60 瓦的微波功率加熱 150 秒,使衍生更為完全。爾後,取出下層萃取液,進入 GC/MS 進行檢測。在 10-1000 ng/L 的濃度範圍內,檢量線迴歸係數皆大於 0.994;偵測極限 (LOD) 為 0.1-5 ng/L。精密度及準確度測試,其相對標準差 (RSDs) 皆小於 9%,顯示此方法具有良好的穩定性以及再現性。在國內不同水樣中測得的對羥基苯甲酸酯濃度介於 0.045~0.928 μg/L 之間。
    ;Alkyl p-hydroxybeznoate, also known as Parabens, was added in food, lotion, pharmaceutical and food as preservative for more than 80 years. Because of its odorless, low prices and difficult hardening, they were widely used worldwide. Recent studies show that parabens may contain estrogen, carcinogen activity and potential endocrine disrupter.
    A simple, efficient and rapid analysis method for the determination of parabens in aqueous sample is presented. The method involves one-step in-sample silylation coupled with ultrasonic-assisted dispersive liquid-liquid microextraction (UADLLME) prior to their determination by GC-MS.
    The optimal extraction condition involved the rapid injection of a mixture of 600μL of 2-propanol (as a dispersant), 300μL of dichloromethane (as an extractant) and 20μL MTBSTFA+1%TBDMSCl (as a derivatizing agent) into a 10 ml of water sample containing 0.5g of sodium chloride in a conical bottom glass tube. After ultrasonication for 1 min and centrifugation at 4500 rpm (10 min), the tube was microwave irradiated at 60W for 150 seconds to accelerate TMS-derivatization.
    The limit of quantitations (LOQs) were range between 0.1-5 ng/L. The precision for the analytes, as expressed with relative standard deviation (RSDs), were less than 9%, indicated that this method shows a good stability and reproducibility. In real sample, parabens were detected between 0.04~0.93 μg/L in river samples.
    Appears in Collections:[化學研究所] 博碩士論文

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