title: Determination of nitrate esters in water samples Comparison of efficiency of solid-phase extraction and solid-phase microextraction.
abstract: This paper deals with comparison of efficiency of extraction techniques (solid-phase extraction, SPE and solid-phase microextraction, SPME) used for extraction of nitrate esters (ethyleneglycoldinitrate, EGDN and nitroglycerin, NG), representing the first step of the method of quantitative determination of trace concentrations of nitrate esters in water samples. EGDN and NG are subsequently determined by means of high-performance liquid chromatography with ultraviolet detection (HPLC-UV). Optimization of SPE and SPME conditions was carried out using model water samples. Seven SPE cartridges were tested and the conditions were optimized (type of sorbent, type and volume of solvent to be used as eluent). For both nitrate esters the limit of detection (LOD) and the limit of quantification (LOQ) obtained using SPE/HPLC-UV were 0.23 microg mL(-1) and 0.70 microg mL(-1), respectively. Optimization of SPME conditions: type of SPME fibre (four fibres were tested), type and time of sorption/desorption, temperature of sorption. PDMS/DVB (polydimethylsiloxane/divinylbenzene) fibre coating proved to be suitable for extraction of EGDN and NG. For this fibre the LOD and the LOQ for both nitrate esters were 0.16 microg mL(-1) and 0.50 microg mL(-1), respectively. Optimized methods SPE/HPLC-UV and SPME/HPLC-UV were then used for quantitative determination of nitrate esters content in real water samples from the production of EGDN and NG.
authors.affiliation: University of Pardubice, Faculty of Chemical Technology, Department of Analytical Chemistry, 532 10 Pardubice, Czech Republic.
authors.forename: Vera
authors.initials: V
authors.lastname: Jezová
authors.forename: Jan
authors.initials: J
authors.lastname: Skládal
authors.forename: Ales
authors.initials: A
authors.lastname: Eisner
authors.forename: Petra
authors.initials: P
authors.lastname: Bajerová
authors.forename: Karel
authors.initials: K
authors.lastname: Ventura
mesh_terms: D000327:Adsorption; D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D004952:Esters / Q000032:analysis* / Q000302:isolation & purification; D009566:Nitrates / Q000032:analysis* / Q000302:isolation & purification; D005996:Nitroglycerin / Q000032:analysis / Q000302:isolation & purification; D015203:Reproducibility of Results; D052617:Solid Phase Microextraction / Q000379:methods*; D012997:Solvents; D013696:Temperature; D013997:Time Factors; D014867:Water / Q000737:chemistry*
chemical_list: D004952:Esters; D009566:Nitrates; D012997:Solvents; D014867:Water; D005996:Nitroglycerin