title: Micro-solid phase extraction followed by thermal extraction coupled with gas chromatography-mass selective detector for the determination of polybrominated diphenyl ethers in water.
abstract: A method of analyzing environmental contaminants in water based on micro-solid phase extraction (μ-SPE) followed by thermal extraction (TE) and a cold-trapping step, coupled with gas chromatography-mass selective detection (GC-MSD) was developed and validated. μ-SPE-TE- GC-MSD was employed in the determination of five polybrominated diphenyl ethers. The μ-SPE sorbent was chitosan-graphene oxide (CS-GO) composite, which was prepared by mixing CS and GO by means of ultrasonication. The CS in the composite was cross-linked with glutaraldehyde. After μ-SPE, the analytes in the extract were extracted thermally in a thermal desorption unit tube combined with a cooled injection system, coupled to GC-MSD. The extraction conditions were optimized for the detection of the target compounds in water. This method provided linearity ranges of between 0.1 and 20μgL(-1) (depending on the analytes), with coefficients of determination, r(2), ≥0.9982. The calculated relative recoveries were between 71.52 and 96.15% whereas precision (based on % relative standard deviations) was between 3.54 and 11.36%. The method showed limit of detection and limit of quantification ranges of between 0.007 and 0.016μgL(-1), and between 0.023 and 0.054μgL(-1), for the two groups of analytes, respectively. The method was applied to the determination of the target analytes in water.
authors.affiliation: Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, National University of Singapore, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore.
authors.forename: Nyi Nyi
authors.initials: NN
authors.lastname: Naing
authors.affiliation: Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, National University of Singapore, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore.
authors.forename: Sam Fong Yau
authors.initials: SF
authors.lastname: Li
authors.affiliation: Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, National University of Singapore, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore; Tropical Marine Science Institute, National University of Singapore, S2S, 18 Kent Ridge Road, Singapore 119227, Singapore. Electronic address: chmleehk@nus.edu.sg.
authors.forename: Hian Kee
authors.initials: HK
authors.lastname: Lee
mesh_terms: D048271:Chitosan / Q000737:chemistry; D003432:Cross-Linking Reagents / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry; D005976:Glutaral / Q000737:chemistry; D006108:Graphite / Q000737:chemistry; D055768:Halogenated Diphenyl Ethers / Q000032:analysis* / Q000302:isolation & purification*; D057230:Limit of Detection; D052617:Solid Phase Microextraction / Q000379:methods*; D013696:Temperature; D014867:Water / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis / Q000302:isolation & purification
chemical_list: D003432:Cross-Linking Reagents; D055768:Halogenated Diphenyl Ethers; D014874:Water Pollutants, Chemical; D014867:Water; D006108:Graphite; D048271:Chitosan; D005976:Glutaral
keywords: Chitosan-graphene oxide composite; Micro-solid phase extraction; Polybrominated diphenyl ethers; Thermal extraction