고상추출법과 액액추출법을 이용한 수질 시료 중 Hexabromocyclododecanes (HBCDs) 분석법 연구
Analytical Method for Determination of Hexabromocyclododecanes (HBCDs) in Water Samples using Solid-Phase Extraction and Liquid-Liquid Extraction
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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%
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%
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