Solid-phase extraction combined with headspace single-drop microextraction of chlorophenols as their methyl ethers and analysis by high-performance liquid chromatography-diode array detection.

Published on Jan 15, 2011in Talanta5.339
· DOI :10.1016/J.TALANTA.2010.11.003
Nisha Sharma5
Estimated H-index: 5
(Rani Durgavati University),
Archana Jain23
Estimated H-index: 23
(Rani Durgavati University)
+ 1 AuthorsKrishna K. Verma24
Estimated H-index: 24
(Rani Durgavati University)
Abstract Solid-phase extraction (SPE) of phenol and chlorophenols, their derivatization to methyl ethers, headspace single-drop microextraction (HS-SDME) of methyl ethers using 1-butanol as extraction solvent, and direct transfer of the drop into the injector for high performance liquid chromatography with diode array detection (HPLC-DAD) have been reported. A flanged-end polytetrafluoroethylene sleeve, 3 mm × 0.5 mm, placed at the tip of the syringe needle, allowed the use of 10 μL solvent drop for extraction. The procedure has been optimized for variables involved in SPE and HS-SDME. A rectilinear relationship was obtained between the amount of chlorophenols and peak area ratio of their methyl ethers/internal standard (4-methoxyacetophenone) in the range 0.01–10 mg L−1, correlation coefficient in the range 0.9956–0.9996, and limit of detection in the range 1.5–3.9 μg L−1 when HS-SDME alone was used for sample preparation. When using coupled SPE and HS-SDME, the linear range obtained was 0.1–500 μg L−1, correlation coefficient in the range 0.9974–0.9998, and the limit of detection in the range 0.04–0.08 μg L−1. Spiked real samples have been analyzed with adequate accuracy, and application of the method has been demonstrated for the analysis of chlorophenols formed upon bamboo pulp bleaching.
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