中文摘要：本文评估了一种环境友好且成本较低的生物吸附剂，并且首次在镍钛合金支撑的固相萃取中将其用作萃取剂，应用傅立叶变换红外光谱、热重分析和扫描电子显微镜对其进行表征，证实了这种生物吸附剂纤维与气相色谱电子捕获检测器联用检测水中δ-HCH、奥尔德林、七氯环氧化物、α-硫丹、异狄氏剂和4,4’- DDD等残留中的适用性，采用中心组合设计法同时对温度、萃取时间和离子强度等影响参数进行了优化，最佳条件为：80分钟萃取时间、80摄氏度、15%的氯化钠(w/v)。满意度分析结果显示：检测限为0.19-0.71ng/L，定量限为0.65-2.38 ng/L，通过江水和湖水样本不同浓度加标下的回收率分析发现，α-硫丹的回收率最低，为60%，最高为δ-HCH，回收率达113%，相对标准差都低于21%。N=3重复性评估中相对标准差低于14%。本文还将该涂层与市售DVB/Car/PDMS涂层进行对比，该涂层纤维在检测限水平和机械稳定性方面均表现满意，具有较高的应用潜力。
外文摘要：In this study, an environmentally friendly and low-cost biosorbent coating was evaluated, for the first time, as the extraction phase for solid-phase microextraction (SPME) supported on a nitinol alloy. The characterization of the new fiber was performed by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The applicability of the biosorbent-based fiber in the determination of delta-hexachlorocyclohexane, aldrin, heptachlor epoxide, alpha-endosulfan, endrin and 4,4'-DDD in water samples was verified, with separation/detection by gas chromatography coupled to electron capture detection (GC-ECD). The influencing parameters (temperature, extraction time and ionic strength) were optimized simultaneously using a central composite design. The optimum conditions were: extraction time of 80 min at 80 degrees C and sodium chloride concentration of 15% (w/v). Satisfactory analytical performance was achieved with limits of detection (LOD) between 0.19 and 0.71 ng L-1 and limits of quantification (LOQ) between 0.65 and 2.38 ng L-1. The relative recoveries for the analytes were determined using river and lake water samples spiked at different concentrations and ranged from 60% for alpha-endosulfan to 113% for delta-hexachlorocyclohexane, with relative standard deviations (RSD) lower than 21%. The fiber-to-fiber reproducibility (n = 3) was also evaluated and the RSD was lower than 14%. The extraction efficiency obtained for the proposed biosorbent coating was compared to a commercially available DVB/Car/PDMS coating. The proposed fiber provided very promising results, including LODs at the level of parts per trillion and highly satisfactory thermal and mechanical stability. (C) 2017 Elsevier B.V. All rights reserved.
外文关键词：Solid-phase microextraction, Bracts, Biosorbent, Organochlorine pesticides
作者：do Carmo, Sangela Nascimento; Merib, Josias; Dias, Adriana Neves; Stolberg, Joni; Budziak, Dilma; Carasek, Eduardo
作者单位：Univ Fed Santa Catarina, Dept Quim, BR-88040900 Florianopolis, SC, Brazil.
期刊名称：JOURNAL OF CHROMATOGRAPHY A
期刊影响因子：3.981
出版年份：2017
出版刊次：11
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