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1-丁基-3-氨丙基咪唑功能化氧化石墨烯作为一种纳米吸附剂,用于通过分散固相微萃取同时萃取类固醇和β-受体阻滞剂。

1-Butyl-3-aminopropyl imidazolium-functionalized graphene oxide as a nanoadsorbent for the simultaneous extraction of steroids and β-blockers via dispersive solid-phase microextraction.

作者信息

Serrano Maria, Chatzimitakos Theodoros, Gallego Mercedes, Stalikas Constantine D

机构信息

Department of Analytical Chemistry, University of Cordoba, 14071 Cordoba, Spain.

Laboratory of Analytical Chemistry, Department of Chemistry, University of Ioannina, 45110 Ioannina, Greece.

出版信息

J Chromatogr A. 2016 Mar 4;1436:9-18. doi: 10.1016/j.chroma.2016.01.052. Epub 2016 Jan 24.

Abstract

In this study, we describe the synthesis of graphene oxide functionalized with the ionic liquid 1-butyl-3-aminopropyl imidazolium chloride and its use as an adsorbent for the dispersive solid-phase microextraction (micro SPE) of four anabolic steroids and six β-blockers from aqueous samples of environmental importance, prior to their HPLC-diode array detector analysis. As the ionic liquid is covalently attached to graphene oxide sheets, it is made possible for it to participate in the dispersive micro SPE procedure. The limits of detection and limits of quantification of the proposed method were found to be in the range of 7-23ng/L and between 20 and 70ng/L, respectively. The linearity was satisfactory, with the determination coefficients to range from 0.9940 to 0.9998 while the within- and between-day relative standard deviation of the method ranged between 3.1 and 7.6% and from 4.0 to 8.5%, respectively. In order to test the applicability of the proposed method in real-life samples, the effluent from a municipal wastewater treatment plant as well as natural water samples from two rivers and a lake were collected and analyzed. After the analysis of samples, the effluent from municipal wastewater treatment plant was fortified with the analytes, at concentrations equal to 2 and 10 times the LOQs. Recoveries were calculated after subtracting the native (no-spike) concentrations of analytes, when needed. All the recoveries were in the range of 87-98%. A comparison study attests to the superiority of the developed nanomaterial over graphene oxide and graphene for the dispersive micro SPE of steroids and β-blockers.

摘要

在本研究中,我们描述了用离子液体1-丁基-3-氨丙基咪唑氯化物功能化的氧化石墨烯的合成,及其作为吸附剂用于从具有环境重要性的水样中分散固相微萃取(微固相萃取)四种合成代谢类固醇和六种β受体阻滞剂,然后进行高效液相色谱 - 二极管阵列检测器分析。由于离子液体共价连接到氧化石墨烯片上,使其能够参与分散微固相萃取过程。所提出方法的检测限和定量限分别在7 - 23 ng/L和20至70 ng/L范围内。线性良好,测定系数范围为0.9940至0.9998,而该方法日内和日间相对标准偏差分别在3.1%至7.6%和4.0%至8.5%之间。为了测试所提出方法在实际样品中的适用性,收集并分析了城市污水处理厂的出水以及两条河流和一个湖泊的天然水样。在样品分析后,向城市污水处理厂的出水中添加分析物,浓度等于定量限的2倍和10倍。必要时,在减去分析物的天然(未加标)浓度后计算回收率。所有回收率在87%至98%范围内。一项比较研究证明了所开发的纳米材料在类固醇和β受体阻滞剂的分散微固相萃取方面优于氧化石墨烯和石墨烯。

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