title: Optimisation of a selective method for the determination of organophosphorous triesters in outdoor particulate samples by pressurised liquid extraction and large-volume injection gas chromatography-positive chemical ionisation-tandem mass spectrometry.
abstract: A selective analytical method for the determination of nine organophosphate triesters and triphenylphosphine oxide (TPPO) in outdoor particulate matter is presented. It involves a fully automated pressurised liquid extraction (PLE) step, integrating an alumina clean-up process, and subsequent determination by large-volume injection gas chromatography-positive chemical ionisation-tandem mass spectrometry (LVI-GC-PCI-MS/MS). The extraction variables (solvent, amount of adsorbent, temperature, time and number of cycles) were optimised using a multicriteria strategy which implements a desirability function that maximises both extraction and clean-up efficiencies while searching for the best-compromise PLE conditions. The final method affords quantification limits of between 0.01 and 0.3 microg g(-1) and recoveries of >80%, with the exceptions of the most polar analytes, TCEP and TPPO (~65%) for both urban dust and PM10 samples. Moreover, the method permitted the levels of these compounds in dust deposited outdoors (between LOD and 0.5 microg g(-1) for TEHP) and PM10 samples (between LOD and 2.4 microg m(-3) for TiBP) to be measured and reported for the first time.
authors.affiliation: IUMA-University Institute of Environment, University of A Coruña, Pazo da Lóngora, Liáns, Oleiros (A Coruña), Spain. jbquintana@udc.es
authors.forename: José Benito
authors.initials: JB
authors.lastname: Quintana
authors.forename: Rosario
authors.initials: R
authors.lastname: Rodil
authors.forename: Purificación
authors.initials: P
authors.lastname: López-Mahía
authors.forename: Soledad
authors.initials: S
authors.lastname: Muniategui-Lorenzo
authors.forename: Darío
authors.initials: D
authors.lastname: Prada-Rodríguez
mesh_terms: D000327:Adsorption; D000393:Air Pollutants / Q000032:analysis; D002849:Chromatography, Gas / Q000379:methods*; D004784:Environmental Monitoring / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D007477:Ions; D013058:Mass Spectrometry / Q000379:methods*; D008956:Models, Chemical; D009943:Organophosphorus Compounds / Q000032:analysis / Q000737:chemistry*; D011312:Pressure; D015203:Reproducibility of Results; D012107:Research Design; D012984:Software; D012997:Solvents / Q000032:analysis; D013696:Temperature
chemical_list: D000393:Air Pollutants; D007477:Ions; D009943:Organophosphorus Compounds; D012997:Solvents