Key Laboratory of Pesticide and Chemical Biology, Ministry of Education, Institute of Environmental Chemistry, College of Chemistry, Central China Normal University, Wuhan, 430079, China.
Key Laboratory of Pesticide and Chemical Biology, Ministry of Education, Institute of Environmental Chemistry, College of Chemistry, Central China Normal University, Wuhan, 430079, China.
J Chromatogr A. 2019 Mar 15;1588:17-24. doi: 10.1016/j.chroma.2018.12.034. Epub 2018 Dec 17.
A novel solid phase microextraction fiber named graphene oxide incorporated poly acrylamide-ethylene glycol dimethacrylate (GO-poly AM-EDGMA) monolithic fiber has been successfully prepared in a fused silica capillary tube (250 μm, i.d.) via thermally initiated polymerization using acrylamide (AM) as the monomer, ethylene glycol dimethacrylate (EGDMA) as the crosslinker, dimethylformamide dispersed by GO as porogens, and then obtained by removing 1 cm wall from one end of the fused silica capillary tube. The fiber has large surface area (536 m g), pore capacity (0.694 cm g) good thermal stability (up to 320 ℃), long service life and good reproducibility (RSD ＜5% throughout 110 times) which facilitated for high throughput headspace solid phase microextraction (HS-SPME) coupled to gas chromatograph (GC) analysis. The HS-SPME/GC method using the new fiber was evaluated by the determination of five organophosphate esters (OPEs) in soil samples coupled to flame photometric detector (FPD). The proposed HS-SPME-GC/FPD method yielded satisfactory limits of quantification (0.03 ng g∼0.24 ng g); linearity (≥0.99), good intra- and inter-day precision expressed as relative standard deviations for a single fiber were in the range of 5.2-9.0% and 4.8-9.0%, respectively, and fiber-to-fiber reproducibility was in the range of 5.9-9.7%. The method was applied for the analysis of OPEs in environmental soil samples and the relative recoveries were found to be in the range from 80.1 to 105.6%. Based on these features, the new fiber has great potential for widespread use as a high throughput trace analysis tool.
一种新型固相微萃取纤维，命名为氧化石墨烯聚丙烯酰胺-乙二醇二甲基丙烯酸酯（GO-poly AM-EDGMA）整体纤维，已成功地在熔融石英毛细管（250μm，内径）中通过热引发聚合制备，使用丙烯酰胺（AM）作为单体，乙二醇二甲基丙烯酸酯（EGDMA）作为交联剂，GO 分散的二甲基甲酰胺作为致孔剂，然后通过从熔融石英毛细管的一端去除 1cm 壁来获得。该纤维具有大的表面积（536m2/g）、孔容量（0.694cm3/g）、良好的热稳定性（高达 320℃）、长使用寿命和良好的重现性（整个 110 次测试中 RSD＜5%），有利于高通量顶空固相微萃取（HS-SPME）与气相色谱（GC）分析相结合。采用新纤维的 HS-SPME/GC 方法通过火焰光度检测器（FPD）测定土壤样品中的五种有机磷酸酯（OPEs）进行了评估。所提出的 HS-SPME-GC/FPD 方法得到了令人满意的定量限（0.03ng g～0.24ng g）；线性（≥0.99），良好的日内和日间精密度，用单个纤维表示的相对标准偏差范围分别为 5.2-9.0%和 4.8-9.0%，纤维间重现性范围为 5.9-9.7%。该方法用于分析环境土壤样品中的 OPEs，相对回收率范围为 80.1-105.6%。基于这些特点，新纤维具有作为高通量痕量分析工具广泛应用的巨大潜力。
