Determination of phthalic acid esters in Chinese white spirit using dispersive liquid-liquid microextraction coupled with sweeping β-cyclodextrin-modified micellar electrokinetic chromatography

摘要

A simple method that consumes low organic solvent is proposed for the analysis of phthalic acid esters in Chinese white spirit using dispersive liquid-liquid microextraction coupled with sweeping-micellar electrokinetic chromatography. Tetrachloromethane and white-spirit-containing ethanol were used as the extraction and dispersing solvents,respectively. The electrophoresis separation buffer was composed of 5 mM β-cyclodextrin,50 mM sodium dodecyl sulfate and 25 mM borate buffer (pH 9.2) with 9% acetonitrile,enabling the baseline resolution of the analytes within 13 min. Under the optimum conditions,satisfactory linearities (5-1000 ng/mL, r ≥ 0.9909), good reproducibility (RSD ≤ 6.7% for peak area, and RSD ≤ 2.8% for migration time), low detection limits (0.4-0.8 ng/mL) and acceptable recovery rates (89.6-105.7%) were obtained. The proposed method was successfully applied to 22 Chinese white spirits, and the content of dibutyl phthalate in 55% of the samples exceeded the Specific Migration Limit of 0.3 mg/kg established by the domestic and international regulations.