Rapid and sensitive determination of multiple endocrine-disrupting chemicals by ultrasound-assisted in situ derivatization dispersive liquid-liquid microextraction coupled with ultra-high-performance liquid chromatography/tandem mass spectrometry.

Abstract

Endocrine-disrupting chemicals (EDCs) in environment samples and food stuffs are an increasing serious public health issue due to their potency to interfere and deregulate several aspects of the endocrine system. Because of their extremely low abundance, it remains a challenging task to develop a sensitive detection method. 4'-Carbonyl chloride rosamine (CCR) was used as a derivatization reagent for EDCs for the first time. A new ultrasound-assisted in situ derivatization/dispersive liquid-liquid microextraction (UA-DLLME with in situ derivatization) method for multiple EDCs including five estrogens, two alkylphenols, eight bisphenols, seven parabens and triclosan coupled with ultra-high-performance liquid chromatography/tandem mass spectrometry (UHPLC/MS/MS) has been developed and validated. The ionization efficiency of EDCs was greatly enhanced through the introduction of a permanent charged moiety of CCR into the derivatives during electrospray ionization (ESI)-MS analysis. The main variables potentially affecting the UA-DLLME with in situ derivatization process are optimized. The recoveries and matrix effects of 23 EDCs for the spiking samples were in the range of 83.0-116.0% and 85.8-114.6%, respectively. Good method reproducibility was achieved. The limits of detection (LODs) for 23 EDCs were 0.05-0.40ng/L and 0.03-0.25ng/g (dry weight, d.w.) for environment samples and food stuffs, respectively. The proposed method has been demonstrated to be suitable for simultaneous determination of multiple EDCs in real samples with high sensitivity, speediness, and good sample clean-up ability. Copyright © 2017 John Wiley & Sons, Ltd.