Simultaneous determination of thirteen organophosphate esters in settled indoor house dust and a comparison between two sampling techniques

• Thirteen organophosphate esters (OPEs) were simultaneously measured in house dust.
• GC/PCI–MS/MS may be one of the best methods for OPE analysis in house dust.
• Valuable data for potential certification of OPEs in NIST SRM 2585 were generated.
• Use of household vacuum is a cost-effective alternative to standardized sampling.

An analytical method for the simultaneous determination of 13 organophosphate esters (OPEs) in house dust was developed. The method is based on solvent extraction by sonication, sample cleanup by solid phase extraction (SPE), and analysis by gas chromatography–positive chemical ionization–tandem mass spectrometry (GC/PCI–MS/MS). Method detection limits (MDLs) ranged from 0.03 to 0.43 μg/g and recoveries from 60% to 118%. The inter- and intra-day variations ranged from 3% to 23%. The method was applied to dust samples collected using two vacuum sampling techniques from 134 urban Canadian homes: a sample of fresh or “active” dust (FD) collected by technicians and a composite sample taken from the household vacuum cleaner (HD). Results show that the two sampling methods (i.e., FD vs HD) provided comparable results. Tributoxyethyl phosphate (TBEP), triphenyl phosphate (TPhP), tris(chloropropyl) phosphate (TCPP), tri(2-chloroethyl) phosphate (TCEP), tris(dichloro-isopropyl) phosphate (TDCPP), tricresyl phosphate (TCrP), and tri-n-butyl phosphate (TnBP) were detected in the majority of samples. The most predominant OPE was TBEP, with median concentrations of 31.9 μg/g and 22.8 μg/g in FD and HD samples, respectively, 1 to 2 orders of magnitude higher than other OPEs. The method was also applied to the analysis of OPEs in the National Institute of Standards and Technology (NIST) standard reference material (NIST SRM 2585, organic contaminants in house dust). The results from SRM 2585 may contribute to the certification of OPE concentration values in this SRM.