Determination of ethylenethiourea residues in tea using precolumn derivatization with ultra-performance liquid chromatography-tandem mass spectrometry

Abstract

A method based on precolumn derivatization along with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of ethylenethiourea residues in tea. The sample was extracted using acetonitrile; the extracting solution was purified by matrix-dispersed solid phase extraction and precolumn derivatization using 9-fluorenylmethyl chloroformate (FMOC-CL). The UPLC separation was carried out on an Acquity BEH C18 column (100 mm×2.1 mm, 1.7 μm) and quantified using the isotope internal standard method. The mobile phase was 0.1% (v/v) formic acid and acetonitrile. For tea samples, the detection limit of this method was 1.3 μg/kg and the limit of quantitation was 4.2 μg/kg. The recoveries were in the range 97.7%-107.5% with relative standard deviation (RSD) of 2.1%-10.0% (n=6). The linear correlation coefficient (r) was 0.9993 over the concentration range 1.0-203.4 μg/L. This method showed high sensitivity, good reproducibility, and qualitative and quantitative accuracy, and could be suitable for the detection of ethylenethiourea residues in tea.