PMID- 26931424 OWN - NLM STAT- MEDLINE DCOM- 20160729 LR - 20181202 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1440 DP - 2016 Apr 1 TI - Magnetic micro-solid-phase-extraction of polycyclic aromatic hydrocarbons in water. PG - 23-30 LID - S0021-9673(16)30162-5 [pii] LID - 10.1016/j.chroma.2016.02.046 [doi] AB - A novel sorbent, magnetic chitosan functionalized graphene oxide (MCFG) was synthesized and used in the micro-solid-phase-extraction (mu-SPE) and gas chromatography-mass spectrometric (GC-MS) analysis of polycyclic aromatic hydrocarbons (PAHs) from water. Through the use of the magnetic sorbent, the mu-SPE device also functioned as a stir bar during extraction. Three types of MCFG were prepared using glutaraldehyde cross-linked chitosan and graphene oxide with different amounts of magnetic nanoparticles (Fe3O4) (0.05g, 0.07g and 0.1g). The material was characterized using Fourier transform infrared spectroscopy and field emission scanning electron microscopy. Parameters affecting the extraction such as the type of sorbent, extraction and desorption times, volume of sample solution and type of desorption solvent were optimized. Under the most favourable conditions, the highest extraction was obtained by using the composite prepared with 0.1g of Fe3O4. For the latter material as sorbent, the linearity of the analytes was in the range of 0.01 and 100mugL(-1) for naphthalene, fluoranthene and pyrene while acenaphthylene and phenanthrene exhibited linearity in the range of 0.05 and 100mugL(-1). For fluorene and anthracene, the linearity range was from 0.01 to 50mugL(-1). The coefficients of determination (r(2)) associated with the above linear ranges were higher than 0.987. The limits of detection from GC-MS analysis of the seven PAHs were in the range 0.2-1.8ngL(-1); limits of quantification were between 0.8 and 5.9ngL(-1) while the relative standard deviations (RSDs) varied from 2.1 to 8.2%. The recoveries of the method for the compounds at spiking levels of 1 and 5mugL(-1) were in the range 67.5-106.9% with RSDs below 15%. The enrichment factors were found to be in between 67 and 302. The developed method afforded an interesting and innovative approach using MCFG as an efficient and promising sorbent. CI - Copyright (c) 2016 Elsevier B.V. All rights reserved. FAU - Naing, Nyi Nyi AU - Naing NN AD - Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore. FAU - Yau Li, Sam Fong AU - Yau Li SF AD - Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore. FAU - Lee, Hian Kee AU - Lee HK AD - Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore. Electronic address: chmleehk@nus.edu.sg. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20160217 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Polycyclic Aromatic Hydrocarbons) RN - 0 (Water Pollutants, Chemical) RN - 059QF0KO0R (Water) RN - 7782-42-5 (Graphite) SB - IM MH - Gas Chromatography-Mass Spectrometry MH - Graphite/*chemistry MH - Limit of Detection MH - *Magnetics MH - Polycyclic Aromatic Hydrocarbons/*isolation & purification MH - Solid Phase Extraction/*methods MH - Spectroscopy, Fourier Transform Infrared MH - Water/*chemistry MH - Water Pollutants, Chemical/*isolation & purification OTO - NOTNLM OT - Gas chromatography-mass spectrometry OT - Graphene oxide OT - Magnetic chitosan OT - Micro-solid-phase-extraction EDAT- 2016/03/05 06:00 MHDA- 2016/07/30 06:00 CRDT- 2016/03/03 06:00 PHST- 2015/11/22 00:00 [received] PHST- 2016/02/14 00:00 [revised] PHST- 2016/02/15 00:00 [accepted] PHST- 2016/03/03 06:00 [entrez] PHST- 2016/03/05 06:00 [pubmed] PHST- 2016/07/30 06:00 [medline] AID - S0021-9673(16)30162-5 [pii] AID - 10.1016/j.chroma.2016.02.046 [doi] PST - ppublish SO - J Chromatogr A. 2016 Apr 1;1440:23-30. doi: 10.1016/j.chroma.2016.02.046. Epub 2016 Feb 17.