Development and validation of a multi-residue method for the simultaneous analysis of brominated and organophosphate flame retardants, organochlorine pesticides, and polycyclic aromatic compounds in household dust

Abstract

Household dust is a sink for multiple toxic chemicals with known or suspected potential health effects. However, most dust exposure studies focus on a few chemicals, which may limit overall understanding of human exposure characteristics because people spend most of their time indoors. This paper describes the development and evaluation of a multi-residue analysis of 20 organochlorine pesticides (OCPs), 15 polycyclic aromatic hydrocarbons (PAHs), 8 polybrominated diphenyl ether congeners (PBDEs), 3 hexabromocyclododecane (HBCDs), 8 synthetic musks (Musks), and 7 organophosphate esters (OPEs) in indoor dusts. After extraction with acetone/hexane (v/v, 1 : 1), all target compounds were fractionated with a Florisil solid-phase extraction (SPE) cartridge into two fractions: PAHs, PBDEs, HBCDs, OCPs and Musks, which were eluted with hexane/dichloromethane, and OPEs eluted with ethyl acetate. Further clean-up using acidified silica 44% cartridges was then performed to enable determination of PBDEs and HBCDs. Instrumental analysis of the target chemicals was performed using gas chromatography (GC) or liquid chromatography (LC) coupled with mass spectrometry (MS) or tandem mass spectrometry (MS/MS). A newly-optimized GC-MS/MS method was employed for the simultaneous determination of PAHs, OCPs, and Musks. The lower limit of quantification (LOQ) values of PAHs, OCPs, and Musks were 0.14–0.92 ng g⁻¹, 0.06–0.38 ng g⁻¹ and 0.07–0.40 ng g⁻¹, respectively. PBDEs were quantified by GC-MS with electron capture negative ionization, and HBCDs and OPEs by LC-MS/MS with electrospray ionization (ESI) in negative and positive ion mode, respectively. Recovery experiments showed that the average recoveries and relative standard deviations were 99–113% and 1–14% for PBDEs, 89–105% and 1–6% for HBCDs, 71–120% and 3–17% for PAHs, 71–112% and 2–17% for OCPs, 77–120% and 2–13% for Musks, and 80–127% and 1–14% for OPEs. Validation experiments showed that the method achieved good accuracy. The developed method was used to analyze SRM 2585 and real indoor dust samples to demonstrate its suitability for routine analysis. The target contaminants were widely detected in SRM 2585 and indoor dust collected from Wuhan of Central China, with PAHs the major species, followed by OPEs, OCPs, and PBDEs.