Abstract

In this study, a vortex-assisted three-phase hollow fiber liquid-phase microextraction (VA-HF-LPME) coupling with high performance liquid chromatography (HPLC) method was developed for determination of three synthetic endocrine disrupting compounds[EDCs, bisphenol-A (BPA), bisphenol-AF (BPAF) and tetrabromobisphenol-A (TBBPA)] in milk samples. Vortex provided effective and mild mixing of the sample solution and increased the contact between analytes and boundary layers of the hollow fibre, thereby enhancing mass transfer rate and leading to high extraction efficiency of the target analytes. The influencing parameters of VA-HF-LPME sample preparation method, such as organic solvents (acceptor phase), pH of sample solution (donor phase), sample volume, concentration of NaOH, extraction time, and ionic strength were systematically optimized. The instrumental calibration curves of BPA, BPAF and TBBPA show good linear relations (R2 > 0.9988) in the concentration range of 0.5-200, 0.5-200 and 1.0-250 µg L-1, respectively. The relative standard deviations (RSD, n = 5) were 1.3-3.7%. The limits of detection (LOD, S/N = 3) were in the range of 0.16-0.35 µg L-1 and the limits of quantification (LOQ, S/N = 10) were in the range of 0.51-1.12 µg L-1. The proposed method was successfully applied to the extraction of EDCs in milk samples.

Highlights

  • During the past years, endocrine disruptors (EDs) have been attracting much more attention because of their possible negative effects on human health.[1]

  • Several extraction approaches have been developed such as solid-phase extraction (SPE),[11] accelerated solvent extraction (ASE),[12] vortex-assisted liquid-liquid microextraction (VALLME)[13] and dispersive liquid-liquid microextraction (DLLME).[14]

  • 8.0 mL of prepared milk spiked with 5 μg mL–1 of each endocrine disrupting compounds (EDCs) were used for the study

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Summary

Introduction

Endocrine disruptors (EDs) have been attracting much more attention because of their possible negative effects on human health.[1]. Various methods have been developed for the analysis of EDCs such as liquid chromatographymass spectrometry (LC-MS or LC-MS-MS),[5] gas chromatography-mass spectrometry (GC-MS or GC‐MS‐MS).[6,7,8] High performance liquid chromatography (HPLC) and capillary electrophoresis (CE) with different detectors have extensive applications for simultaneous determination of various EDCs in liquid samples.[9,10]. Owing to their low concentrations and complicated matrix effects, an effective pretreatment approach is very important for the analysis of these compounds. Compared with conventional extraction methods, microextraction approaches are much simpler, more rapid and environment friendly.[15,16,17,18,19]

Objectives
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Results

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