Analytical Method for Determination of Hexabromocyclododecanes (HBCDs) in Water Samples using Solid-Phase Extraction and Liquid-Liquid Extraction

,; ,; ,; ,; ,; ,; ,; ,; ,

Research article

Journal of the Korean Society for Environmental Analysis 2016;19(2):80-89.

고상추출법과 액액추출법을 이용한 수질 시료 중 Hexabromocyclododecanes (HBCDs) 분석법 연구

이두희¹, 김일규¹, 도영선¹, 정인영², 김혁¹, 이혜리³, 최종우³, 이원석², 박상아¹

¹국립환경과학원
²국립환경연구원
³국립환경과학원 환경측정분석센터

Abstract

In this study, we evaluated analytical methods for the determination of three hexabromocyclododecane diastereomers (α, β, γ-HBCD) using solid-phase extraction (SPE) and liquid-liquid extraction (LLE). Instrumental analysis was conducted using high-performance liquid chromatography with a triple-quadrupole mass spectrometer (LC/MS/MS), and the hydrophilic-lipophilic balance (HLB) cartridge was used for SPE. SPE showed the highest recovery when using ethyl acetate as the eluent, and 40% methanol was used as the clean-up solvent. In LLE, a multilayer column using AgNO3 showed a low recovery rate. The respective method detection limits (MDLs) and the limits of quantitation (LOQs) of HBCDs in water were 0.068-0.145 ng/L and 0.217- 0.462 ng/L for SPE, and 0.043-0.293 ng/L and 0.135-0.932 ng/L for LLE. The accuracy ranged from 96.3% to 104.3% for SPE and 99.3% to 101.2% for LLE. The precision values for both SPE and LLE were less than 5.98%

Key Words: Hexabromocyclododecane, Water, Solid phase extraction, Liquid-liquid extraction