title: Graphene oxide-based dispersive solid-phase extraction combined with in situ derivatization and gas chromatography-mass spectrometry for the determination of acidic pharmaceuticals in water.
abstract: A fast and low-cost sample preparation method of graphene based dispersive solid-phase extraction combined with gas chromatography-mass spectrometric (GC-MS) analysis, was developed. The procedure involves an initial extraction with water-immiscible organic solvent, followed by a rapid clean-up using amine functionalized reduced graphene oxide as sorbent. Simple and fast one-step in situ derivatization using trimethylphenylammonium hydroxide was subsequently applied on acidic pharmaceuticals serving as model analytes, ibuprofen, gemfibrozil, naproxen, ketoprofen and diclofenac, before GC-MS analysis. Extraction parameters affecting the derivatization and extraction efficiency such as volume of derivatization agent, effect of desorption solvent, effect of pH and effect of ionic strength were investigated. Under the optimum conditions, the method demonstrated good limits of detection ranging from 1 to 16ngL(-1), linearity (from 0.01 to 50 and 0.05 to 50μgL(-1), depending on the analytes) and satisfactory repeatability of extractions (relative standard deviations, below 13%, n=3).
authors.affiliation: Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, T-Lab # 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, T-Lab # 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, T-Lab # 02-01, 5A Engineering Drive 1, Singapore 117411, Singapore. Electronic address: chmleehk@nus.edu.sg.
authors.forename: Hian Kee
authors.initials: HK
authors.lastname: Lee
mesh_terms: D004008:Diclofenac / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry; D006108:Graphite / Q000737:chemistry*; D007052:Ibuprofen / Q000032:analysis; D007660:Ketoprofen / Q000032:analysis; D009288:Naproxen / Q000032:analysis; D009994:Osmolar Concentration; D004364:Pharmaceutical Preparations / Q000032:analysis*; D052616:Solid Phase Extraction; D012997:Solvents / Q000737:chemistry; D014867:Water / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis
chemical_list: D004364:Pharmaceutical Preparations; D012997:Solvents; D014874:Water Pollutants, Chemical; D014867:Water; D004008:Diclofenac; D009288:Naproxen; D006108:Graphite; D007660:Ketoprofen; D007052:Ibuprofen
keywords: Acidic pharmaceuticals; Amine functionalized graphene; Dispersive solid phase extraction; In situ derivatization