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 |
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Authors: | Sharma Nisha Jain Archana Singh Vandana Kumari Verma Krishna K |
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Affiliation: | Department of Chemistry, Rani Durgavati University, Pachpedi, Jabalpur 482001, Madhya Pradesh, India |
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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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Keywords: | Chlorophenols Derivatization Methyl ethers Combined solid-phase extraction Headspace single-drop microextraction High-performance liquid chromatography-diode array detection |
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