Solid-phase extraction of seventeen alternative flame retardants in water as determined by ultra-high-performance liquid chromatography-tandem mass spectrometry.


Shanghai Pudong New Area Centre for Disease Control and Prevention, Fudan University Pudong Institute of Preventive Medicine, Shanghai 200136, China. Electronic address: [Email]


Flame retardants have evoked public concerns owing to their extensive usage in consumer products and potential adverse effects on human health. In this study, a rapid and sensitive solid-phase extraction-ultra-high-performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS) method was developed to determine hexabromocyclododecane (HBCD), tetrabromobisphenol-A (TBBPA), six bromophenols (BPs), and nine organophosphate flame retardants (OPFRs) in water. Because of the differences in elution conditions and ionization modes for group 1 (HBCD, TBBPA, and the BPs) and group 2 (OPFRs), we had to run them twice under the different conditions to analyse group 1 and group 2 using UPLC-MS/MS. The method detection limits were 0.1-2.5 ng/L, linearity range was 0.1-100.0 ng/L for group 1 (HBCD, TBBPA, and the BPs). The method detection limit was 0.10 ng/L, and the linearity range was 0.25-250 ng/L for the OPFRs. First, the pH values of the water samples were adjusted to the range of 2-3. Then, the acidified water samples were extracted by hydrophilic-lipophilic-balance solid phase extraction (HLB-SPE) cartridges, which were eluted with 12 mL of acetonitrile. Finally, the recoveries of HBCD, TBBPA, and the BPs were 76.2-98.1%, and the relative standard deviations (RSDs, n = 5) were 2.0-28.5%. Regarding the OPFRs, the recoveries were 72.4-110.3%, and the RSDs were 0.6-6.9%. The stability experiment showed that the concentration differences were less than 15%, meeting the requirement for quality control samples. This proposed method was successfully applied to surface water, ground water, raw water, finished water, tap water, and bottled water samples.


Alternative flame retardants,Bromophenols,Hexabromocyclododecane,Organophosphates,Ultra-high-performance liquid chromatography-tandem mass spectrometry,Water,

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