title: Preparation of poly(trimethyl-2-methacroyloxyethylammonium chloride-co-ethylene glycol dimethacrylate) monolith and its application in solid phase microextraction of brominated flame retardants.
abstract: A capillary poly(trimethyl-2-methacroyloxyethylammonium chloride-co-ethylene glycol dimethacrylate) monolith was in situ synthesized by thermally initiated free radical co-polymerization using trimethyl-2-methacroyloxyethylammonium chloride (MATE) and ethylene glycol dimethacrylate (EGDMA) as functional monomer and cross-linker, respectively. N,N-dimethylformamide and polyethylene glycol 6000 were used as solvent and porogen, respectively. The morphology and porous structure of the resulting monoliths were assessed by scanning electron microscope. In order to prepare practically useful poly(MATE-co-EGDMA) monoliths with low flow resistance and good mechanical strength, some parameters such as PEG-6000 to DMF ratio, total monomer to porogen ratio, and crosslinker to monomer ratio were optimized systematically. Moreover, the extraction mechanism was evaluated using two series of compounds, alkylbenzenes and weak acids, as model compounds on poly(MATE-co-EGDMA) monoliths as liquid chromatographic stationary phase. Finally, the monoliths were applied as the solid phase microextraction medium, and a simple off-line method for simultaneous determination of three brominated flame retardants, 2,4,6-tribromophenol (TBP), tetrabromobisphenol A (TBBPA) and 4,4'-dibrominated diphenyl ether (DBDPE), in environmental waters was developed by coupling the polymer monolith microextraction to HPLC with UV detection. The regression equations for these three brominated flame retardants showed good linearity from their limit of quantification to 5000ng/mL. The limits of detection were 0.20, 0.15 and 0.10ng/mL for TBP, TBBPA and DBDPE, respectively. The recovery of the proposed method was 78.7-106.1% with intra-day relative standard deviation of 1.3-4.4%.
authors.affiliation: State Key Laboratory of Analytical Chemistry for Life Science, School of Chemistry & Chemical Engineering and Center of Materials Analysis, Nanjing University, 22 Hankou Road, Nanjing 210093, China.
authors.forename: Ting-ting
authors.initials: TT
authors.lastname: Yang
authors.forename: Lin-feng
authors.initials: LF
authors.lastname: Zhou
authors.forename: Jun-qin
authors.initials: JQ
authors.lastname: Qiao
authors.forename: Hong-zhen
authors.initials: HZ
authors.lastname: Lian
authors.forename: Xin
authors.initials: X
authors.lastname: Ge
authors.forename: Hong-yuan
authors.initials: HY
authors.lastname: Chen
mesh_terms: D002851:Chromatography, High Pressure Liquid; D004126:Dimethylformamide / Q000737:chemistry; D005026:Ethylene Glycols / Q000737:chemistry*; D005411:Flame Retardants / Q000032:analysis / Q000302:isolation & purification*; D005618:Fresh Water / Q000737:chemistry; D055768:Halogenated Diphenyl Ethers / Q000032:analysis / Q000302:isolation & purification*; D006863:Hydrogen-Ion Concentration; D057927:Hydrophobic and Hydrophilic Interactions; D057230:Limit of Detection; D016014:Linear Models; D010539:Permeability; D011109:Polymethacrylic Acids / Q000138:chemical synthesis / Q000737:chemistry*; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction / Q000295:instrumentation* / Q000379:methods; D014874:Water Pollutants, Chemical / Q000032:analysis / Q000302:isolation & purification
chemical_list: D005026:Ethylene Glycols; D005411:Flame Retardants; D055768:Halogenated Diphenyl Ethers; D011109:Polymethacrylic Acids; D014874:Water Pollutants, Chemical; D004126:Dimethylformamide