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采用低成本方法提高棒式吸附微萃取(BAµE)的分析通量,并结合使用由回收硅藻土制成的环保型可再生吸附剂相。

Low-cost approach to increase the analysis throughput of bar adsorptive microextraction (BAµE) combined with environmentally-friendly renewable sorbent phase of recycled diatomaceous earth.

作者信息

Mafra Gabriela, Oenning Anderson Luiz, Dias Adriana Neves, Merib Josias, Budziak Dilma, Silveira Cristian Berto da, Carasek Eduardo

机构信息

Universidade Federal de Santa Catarina, Departamento de Química, Florianópolis, Santa Catarina 88040-900, Brazil.

Instituto Federal Catarinense, Campus Brusque, 88350-300, Brazil.

出版信息

Talanta. 2018 Feb 1;178:886-893. doi: 10.1016/j.talanta.2017.10.022. Epub 2017 Oct 16.

DOI:10.1016/j.talanta.2017.10.022
PMID:29136910
Abstract

In this study, a novel apparatus for bar adsorptive microextraction (BAµE) using a voltage regulator was proposed as an alternative tool to improve the analysis throughput. In addition, recycled diatomaceous earth obtained as a brewery residue was employed as a biosorbent coating for the determination of methyl paraben, ethyl paraben, benzophenone and triclocarban in water samples by high-performance liquid chromatography-diode array detection (HPLC-DAD). The use of the extraction devices, comprised of floating adsorptive bars of 7.5mm length, in the extractions with magnetic stirrers linked to a voltage regulator enabled the analysis of multiple samples, simultaneously. The method optimization was carried out by univariate and multivariate analyses. The optimal conditions for the method were sample solution at pH 5, extraction time of 90min and liquid desorption in 100µL of acetonitrile:methanol (50:50, v/v) for 15min. The total sample preparation time was 17.5min per sample for a simultaneous batch of six extractions. The R values for the calibration curves obtained were higher than 0.9985. The limits of detection (LODs) varied from 0.19 to 2μgL and the limits of quantification (LOQs) ranged from 0.63 to 6.9μgL. The method was applied to freshwater samples collected from Peri Lagoon (Florianópolis, SC, Brazil) and the relative recoveries ranged from 63% to 124% with relative standard deviations (RSDs) of < 20% (n = 2). The RSD values for the reproducibility of the performance of the magnetic stirrers and inter-device extraction efficiency were lower than 14% (n = 3) and 11% (n = 3), respectively.

摘要

在本研究中,提出了一种使用电压调节器的新型棒状吸附微萃取(BAµE)装置,作为提高分析通量的替代工具。此外,将作为啤酒厂残渣获得的回收硅藻土用作生物吸附剂涂层,通过高效液相色谱 - 二极管阵列检测(HPLC - DAD)测定水样中的对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、二苯甲酮和三氯生。使用由7.5毫米长的浮动吸附棒组成的萃取装置,在与电压调节器相连的磁力搅拌器辅助下进行萃取,能够同时分析多个样品。通过单变量和多变量分析进行方法优化。该方法的最佳条件为:样品溶液pH值为5,萃取时间90分钟,用100微升乙腈:甲醇(50:50,v/v)进行15分钟的液体解吸。对于同时进行的六次萃取批次,每个样品的总样品制备时间为17.5分钟。获得的校准曲线的R值高于0.9985。检测限(LOD)在0.19至2微克/升之间变化,定量限(LOQ)在0.63至6.9微克/升之间。该方法应用于从佩里泻湖(巴西圣卡塔琳娜州弗洛里亚诺波利斯)采集的淡水样品,相对回收率在63%至124%之间,相对标准偏差(RSD)<20%(n = 2)。磁力搅拌器性能重现性和装置间萃取效率的RSD值分别低于14%(n = 3)和11%(n = 3)。

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