Citation: SUN Jianzhi, HE Hui, LIU Shuhui. Determination of three chlorophenols in red wine by sweeping-micellar electrokinetic chromatography coupled with dispersive liquid-liquid microextraction and reversed phase liquid-liquid microextraction[J]. Chinese Journal of Chromatography, ;2014, 32(3): 256-262. doi: 10.3724/SP.J.1123.2013.11004 shu

Determination of three chlorophenols in red wine by sweeping-micellar electrokinetic chromatography coupled with dispersive liquid-liquid microextraction and reversed phase liquid-liquid microextraction

SUN Jianzhi ¹ ,
HE Hui ¹ ,
LIU Shuhui ^1,2,,

1.
1. College of Science, Northwest Agriculture & Forestry University, Yangling 712100, China;

Corresponding author: LIU Shuhui,
Received Date: 4 November 2013
Available Online: 10 December 2013
Fund Project: 西北农林科技大学引进人才专项基金项目(Z111021005). (Z111021005)

A method of dispersive liquid-liquid microextraction (DLLME) and reversed phase liquid-liquid microextraction (RP-LLME) procedures coupled with sweeping-micellar electrokinetic chromatography (sweeping-MEKC) was established to extract and determine the three chlorophenols (CPs) including pentachlorophenol (PCP), 2,4,6-trichlorophenol (TCP) and 2,4-dichlorophenol (DCP) in red wine. The influences of the parameters of two extraction steps and the electrophoresis conditions were investigated. The optimum extraction conditions were as follows: for DLLME, 3.5 mL red wine sample (pH 3.0, 120 g/L NaCl), 300 μL hexane (extraction solvent), extraction for 3 min, centrifugation for 3 min at 5000 r/min; for RP-LLME, 25 μL 0.16 mol/L NaOH solution, extraction for 2 min, centrifugation for 2 min at 5000 r/min. The optimum running buffer (pH 2.3) was an aqueous solution containing 25 mmol/L NaH₂PO₄, 100 mmol/L sodium dodecyl sulfate (SDS) and 30% (v/v) acetonitrile. The optimum on-line concentration conditions were as follows: sample matrix, 80 mmol/L NaH₂PO₄; hydrodynamic injection of 20 s at 20.67 kPa (3 psi). Under the optimum conditions, the excellent linearity was obtained over the range of 0.5-100 μg/L (r≥0.9910) for PCP and TCP, and 1.5-80 μg/L (r≥0.9851) for DCP. The limits of detection (S/N=3) were in the range of 0.035-0.114 μg/L. The average recoveries were in the range of 75.2%-104.7% with the relative standard deviations (RSDs) not more than 6.17%. The results indicated that the proposed method may find wide applications for the determination of trace CPs in various sample matrixes and other weak acidic organic contaminants.
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