Journal
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
Volume 388, Issue 5-6, Pages 1283-1293Publisher
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-007-1338-4
Keywords
organophosphorous triesters; flame retardants; plasticizers; urban dust; particulate matter; PM10; pressurised liquid extraction; accelerated solvent extraction; GC-MS; experimental design; multicriteria optimisation; desirability function
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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 mu g g(-1) and recoveries of > 80%, with the exceptions of the most polar analytes, TCEP and TPPO (similar to 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 mu g g(-1) for TEHP) and PM10 samples (between LOD and 2.4 mu g m(-3) for TiBP) to be measured and reported for the first time.
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