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

Quintana, José Benito; Rodil, Rosario; López-Mahía, Purificación; Muniategui-Lorenzo, Soledad; Prada-Rodríguez, Darío
July 2007
Analytical & Bioanalytical Chemistry;Jul2007, Vol. 388 Issue 5/6, p1283
Academic Journal
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 μg 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 μg g−1 for TEHP) and PM10 samples (between LOD and 2.4 μg m−3 for TiBP) to be measured and reported for the first time.


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