title: A novel graphene nanosheets coated stainless steel fiber for microwave assisted headspace solid phase microextraction of organochlorine pesticides in aqueous samples followed by gas chromatography with electron capture detection.
abstract: In this study, a novel graphene nanosheets (GNSs) coated solid phase microextraction (SPME) fiber was prepared by immobilizing microwave synthesized GNSs on a stainless steel wire. Microwave synthesized GNSs were verified by X-ray diffraction, field emission-scanning electron microscopy (FE-SEM) and transmission electron microscope (TEM). GNS-SPME fiber was characterized using FE-SEM and the results showed the GNS coating was homogeneous, porous, and highly adherent to the surface of the stainless steel fiber. The performance and feasibility of the GNS-SPME fiber was evaluated under one-step microwave assisted (MA) headspace (HS) SPME followed by gas chromatography with electron capture detection for five organochlorine pesticides (OCPs) in aqueous samples. Parameters influencing the extraction efficiency of MA-HS-GNS-SPME such as microwave irradiation power and time, pH, ionic strength, and desorption conditions were thoroughly examined. Under the optimized conditions, detection limits for the OCPs varied between 0.16 and 0.93 ng L(-1) and linear ranges varied between 1 and 1500 n gL(-1), with correlation coefficients ranging from 0.9984 to 0.9998, and RSDs in the range of 3.6-15.8% (n=5). In comparison with the commercial 100 μm polydimethylsiloxane fiber, the GNS coated fiber showed better extraction efficiency, higher mechanical and thermal stability (up to 290°C), longer life span (over 250 times), and lower production cost. The method was successfully applied to the analysis of real water samples with recoveries ranged between 80.1 and 101.1% for river water samples. The results demonstrated that the developed MA-HS-GNS-SPME method was a simple, rapid, efficient pretreatment and environmentally friendly procedure for the analysis of OCPs in aqueous samples.
authors.affiliation: Department of Chemistry, National Chung-Hsing University, Taichung 402, Taiwan.
authors.forename: Vinoth Kumar
authors.initials: VK
authors.lastname: Ponnusamy
authors.forename: Jen-Fon
authors.initials: JF
authors.lastname: Jen
mesh_terms: D002849:Chromatography, Gas / Q000379:methods*; D006108:Graphite / Q000737:chemistry*; D006843:Hydrocarbons, Chlorinated / Q000032:analysis / Q000302:isolation & purification*; D008855:Microscopy, Electron, Scanning; D008872:Microwaves; D049329:Nanostructures / Q000737:chemistry*; D010575:Pesticides / Q000032:analysis / Q000302:isolation & purification*; D015203:Reproducibility of Results; D045483:Rivers / Q000737:chemistry; D012680:Sensitivity and Specificity; D052617:Solid Phase Microextraction / Q000379:methods*; D013193:Stainless Steel / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis / Q000302:isolation & purification; D014961:X-Ray Diffraction
chemical_list: D006843:Hydrocarbons, Chlorinated; D010575:Pesticides; D014874:Water Pollutants, Chemical; D013193:Stainless Steel; D006108:Graphite