Determination of Hexabromocyclododecane Diastereomers in Soil by Ultra Performance Liquid Chromatography-Electrospray Ion Source/Tandem Mass Spectrometry

A new method has been developed to the trace level measurement of α-, β-, and γ-HBCD (hexabromocyclododecane) diastereomers (C12H18Br6) in soil samples by accelerated solvent extraction-ultra performance liquid chromatography-electrospray ion source-triple quadrupole mass spectrometry (ASE-UPLC-ESI-MS/MS). Soil samples were extracted with 3:1 hexane/acetone (V/V) and was further cleaned with a multilayer silica column (15 mm i.d.) filled from the bottom with 6 g of activated silica, 3 g of H2SO4/silica 44% (w/w), and 3 g dried Na2SO4. Quantification of α-, β-, and γ-HBCD diastereomers in samples was performed by the internal standard method. The recovery of triplicate blank soil samples was (104.6 ± 3.7)% for the spiked level of 54 ng ΣHBCD. The concentrations of ΣHBCD in soil samples collected near a HBCD manufactory ranged from 2.8–144.5 ng g−1 (dry weight). The diastereomer profile of HBCD in the soil samples was dominated by γ-HBCD (73.7 ± 4.7)% and followed by α-HBCD (14.6% ± 3.4)% and β-HBCD (11.7 ± 1.7)%.