Department of Chemistry and the Key Laboratory of Analytical Sciences of the Ministry of Education, College of Chemistry and Chemical Engineering, Xiamen University, Xiamen 361005, China.
Anal Chim Acta. 2010 Sep 23;678(1):44-9. doi: 10.1016/j.aca.2010.08.008. Epub 2010 Aug 14.
In this paper, a novel graphene (G) based solid-phase microextraction (SPME) fiber was firstly prepared by immobilizing the synthesized G on stainless steel wire as coating. The new fiber possessed a homogeneous, porous and wrinkled surface and showed excellent thermal (over 330°C), chemical and mechanical stability, and long lifespan (over 250 extractions). The SPME performance of the G-coated fiber was evaluated in detail through extraction of six pyrethroid pesticides. Although the thickness of G-coated fiber was only 6-8 μm, its extraction efficiencies were higher than those of two commercial fibers (PDMS, 100 μm; PDMS/DVB, 65 μm). This high extraction efficiency may be mainly attributed to huge delocalized π-electron system of G, which shows strong π-stacking interaction with pyrethroid pesticide. The G-coated fiber was applied in the gas chromatographic determination of six pyrethroids, and their limits of detection were found to be ranged from 3.69 to 69.4 ng L(-1). The reproducibility for each single fiber was evaluated and the relative standard deviations (RSDs) were calculated to be in the range from 1.9% to 6.5%. The repeatability of fiber-to-fiber and batch-to-batch was 4.3-9.2% and 4.1-9.9%. The method developed was successfully applied to three pond water samples, and the recoveries were 83-110% at a spiking of 1 μg L(-1).
本文首次制备了一种新型的基于石墨烯(G)的固相微萃取(SPME)纤维,即将合成的 G 固定在不锈钢丝上作为涂层。新纤维具有均匀、多孔和褶皱的表面,表现出优异的热稳定性(超过 330°C)、化学稳定性和机械稳定性,使用寿命长(超过 250 次萃取)。通过对六种拟除虫菊酯农药的萃取,详细评价了 G 涂层纤维的 SPME 性能。尽管 G 涂层纤维的厚度仅为 6-8μm,但它的萃取效率高于两种商业纤维(PDMS,100μm;PDMS/DVB,65μm)。这种高萃取效率可能主要归因于 G 巨大的离域π-电子体系,它与拟除虫菊酯农药表现出强烈的π-堆积相互作用。将 G 涂层纤维应用于气相色谱法测定六种拟除虫菊酯,发现其检测限范围为 3.69-69.4ng/L。评估了每个单纤维的重现性,并计算了相对标准偏差(RSD),范围在 1.9%-6.5%之间。纤维间和批间的重复性分别为 4.3%-9.2%和 4.1%-9.9%。该方法成功应用于三个池塘水样,在 1μg/L 的加标水平下,回收率为 83%-110%。