Optimisation of a matrix solid-phase dispersion method for the determination of organophosphate compounds in dust...

A fast and inexpensive sample preparation procedure based on the matrix solid-phase dispersion (MSPD) technique is proposed for the isolation of several organophosphate esters (mainly employed as flame retardants and plasticizers) from indoor dust samples. Extraction and clean-up were carried out in a single step and target compounds were determined by gas chromatography (GC) with nitrogen-phosphorus detection (NPD). The main parameters affecting extraction yield and selectivity, such as type and amount of dispersant material, clean-up co-sorbent and extraction solvent, were evaluated and optimised. Under final conditions, 0.5 g of dust were dispersed with equal amounts of anhydrous sodium sulphate and Florisil, and loaded on the top of a polypropylene cartridge containing 0.5 g of alumina. The dispersed sample was washed with 2 mL of n-hexane to remove the least polar interferences and analytes were eluted with 3 mL of acetone. Recoveries of the proposed method for spiked samples ranged from 80 to 116%, and the day-to-day variability remained between 5 and 10%. Data on levels of organophosphate species in dust from private houses and vehicle cabins are provided. In both cases, the lowest concentrations corresponded to the short chain, non-chlorinated, alkyl organophosphates, whereas mean values above 1 microg g(-1) were measured for the rest of analytes.