Combining microwave-assisted extraction and liquid chromatography-ion-trap mass spectrometry for the analysis of hexabromocyclododecane diastereoisomers in marine sediments

Hsin Hung Wu, Hsin Chang Chen, Wang Hsien Ding

Research output: Contribution to journalArticlepeer-review

27 Scopus citations

Abstract

An efficient microwave-assisted extraction (MAE) procedure coupled with high performance liquid chromatography-electrospray-ion-trap mass spectrometry (HPLC-ESI-ITMS) has been evaluated to determine hexabromocyclododecane diastereoisomers (α-, β- and γ-HBCD) in marine sediments. The composition of the LC mobile phase (consisting of water, methanol and acetonitrile) and the parameters of electrospray ionization (ESI) were evaluated to obtain chromatographic baseline separation and high sensitivity for the detection of these diastereoisomers. The effects of various operating parameters on the quantitative extraction of the HBCDs through MAE were systematically investigated. The three diastereoisomers were then quantitated by HPLC-ITMS employing ESI operated in the negative ionization mode. The HBCDs were extracted from the sediments through MAE using 40 mL of acetone/n-hexane (1/3, v/v) at 90 °C for 12 min. The limits of quantitation (LOQ) ranged from 25 to 40 pg/g (dry weight) in 5 g of the sediment samples. The recoveries of the HBCDs in spiked sediment samples ranged from 68 to 91% (relative standard derivation: 2-11%). The extraction efficiency of the MAE technique was also compared with Soxhlet extraction and pressurized liquid extraction.

Original languageEnglish
Pages (from-to)7755-7760
Number of pages6
JournalJournal of Chromatography A
Volume1216
Issue number45
DOIs
StatePublished - 6 Nov 2009

Keywords

  • Hexabromocyclododecane
  • Liquid chromatography
  • Mass spectrometry
  • Microwave-assisted extraction
  • Sediment analysis

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