Development of Analytical Method for OPFRs in Particle Air Samples

TPS 691: Methods of measurement, design and data analysis, Exhibition Hall, Ground floor, August 28, 2019, 3:00 PM - 4:30 PM Organophosphate flame retardants (OPFRs) are used to improve fire resistance in many products such as furniture and electronics. In Europe and other country, because polybrominated diphenyl ethers (PBDEs) were banned, OPFRs production and application has increased as PBDE substitutes. However the safety of these compounds to people and environment is not elucidated. Because physico-chemical properties of flame retardants tend to accumulate on organic carbon rich matter, they have been detected in sewage sludge, sediments or dust. The object of this study was to develop and validate a method based on Liquid chromatography mass spectrometry (LC-MS) for simultaneous extraction and analysis of 16 OPFRs in air samples. Target compounds were 16 including TBeP, TEP, TnBP, TCPP TPHP etc. Samples were quartz fiber filter (QFF). All target compounds were extracted by sonication with methyl tert-butyl ether. We analyzed with LC-MS and ion mode was negative ion multiple reaction monitoring mode. Mobile phase A was 10 mM ammonium acetate 0.1% formic acid in water and mobile phase B was 0.1% formic acid in methanol (MeOH). To Spiking with target analytes at 3 points (2, 10, 50 ng/g) in blank samples, method validation was repeated 6 time for 3 days and the limit of detection (LOD) was calculated according to the US FDA method. Accuracy and precision was calculated by recovery and standard deviation. Range of accuracy was 87~123% and range of precision was 1.2~15.4 excepting TBeP, TMP and TiPP. Range of R2 was 0.9996~0.9999 and range of LOD was 0.12~2.1 ng/g. A simple sonicate extraction analysis method for simultaneous detection of 16 OPFRs in air samples was developed and validated. The method can extract both alkyl and aryl groups compound in QFF. The proposed method requires little solvents and is very rapid and does not need any other pretreatments of samples before extraction.