title: 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.
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 × 0.5mm, 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.
authors.affiliation: Department of Chemistry, Rani Durgavati University, Pachpedi, Jabalpur 482001, Madhya Pradesh, India.
authors.forename: Nisha
authors.initials: N
authors.lastname: Sharma
authors.forename: Archana
authors.initials: A
authors.lastname: Jain
authors.forename: Vandana Kumari
authors.initials: VK
authors.lastname: Singh
authors.forename: Krishna K
authors.initials: KK
authors.lastname: Verma
mesh_terms: D002733:Chlorophenols / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation*; D004566:Electrodes; D008738:Methyl Ethers / Q000737:chemistry*; D015203:Reproducibility of Results; D052616:Solid Phase Extraction / Q000379:methods*; D014867:Water / Q000737:chemistry
chemical_list: D002733:Chlorophenols; D008738:Methyl Ethers; D014867:Water