title: Determination of glutaraldehyde in water samples by headspace solid-phase microextraction and gas chromatography-mass spectrometry after derivatization with 2,2,2-trifluoroethylhydrazine.
abstract: A simple and convenient headspace solid-phase microextraction (HS-SPME) gas chromatography mass spectrometry (GC-MS) method was described for the determination of glutaraldehyde in water. Glutaraldehyde in water reacted with 2,2,2-trifluoroethylhydrazine (TFEH) in a headspace vial and the formed TFEH derivatives were vaporized and adsorbed onto a fiber. The optimal HS-SPME conditions were achieved with a 50/30μm-divinylbenzene-carboxen-polydimethylsiloxane fiber, 0.06% 2,2,2-TFEH, 25% salt, an extraction/derivatization temperature of 80°C, a heating time of 30min, and a pH of 6.5. The desorption was performed for 1min at 240°C. Under the established conditions, the lowest limits of detection were 0.3μg/L and 0.1μg/L in 6.0mL of surface water and drinking water, respectively, and the intra- and inter-day relative standard deviation was less than 9.1% at concentrations of 50, 100 and 500μg/L. The calibration curve showed good linearity with R=0.9995 and R=0.9993 in surface water and drinking water, respectively. This method is simple, amenable to automation and environmentally friendly.
authors.affiliation: Department of Environmental Science, Kongju National University, Kongju, 314-701, Republic of Korea.
authors.forename: Hye-In
authors.initials: HI
authors.lastname: Kang
authors.affiliation: Department of Environmental Education, Kongju National University, Kongju, 314-701, Republic of Korea. Electronic address: hshin@kongju.ac.kr.
authors.forename: Ho-Sang
authors.initials: HS
authors.lastname: Shin
mesh_terms: D004129:Dimethylpolysiloxanes; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D005976:Glutaral / Q000032:analysis*; D006834:Hydrazines / Q000737:chemistry*; D007202:Indicators and Reagents; D011145:Polyvinyls; D052617:Solid Phase Microextraction / Q000379:methods; D013696:Temperature; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D004129:Dimethylpolysiloxanes; D006834:Hydrazines; D007202:Indicators and Reagents; D011145:Polyvinyls; D014874:Water Pollutants, Chemical; C445089:poly(dimethylsiloxane-divinylbenzene); D005976:Glutaral
keywords: Gas chromatography–mass spectrometry; Glutaraldehyde; Headspace solid-phase microextraction