Abstract

Bar adsorptive microextraction combined with liquid desorption followed by high performance liquid chromatography with diode array detection (BAµE-LD/HPLC-DAD) is proposed for the determination of trace levels of five phenol compounds (3-nitrophenol, 4-nitrophenol, bisphenol-A, 4-n-octylphenol and 4-n-nonylphenol) in surface water matrices. By using a polystyrene-divinylbenzene copolymer (PS-DVB) sorbent phase, high selectivity and efficiency is achieved even against polydimethylsiloxane through stir bar sorptive extraction. Assays performed by BAµE(PS-DVB)-LD/HPLC-DAD on 25 mL water samples spiked at the 10.0 µg/L levels yielded recoveries over 88.0% ± 5.7% for all five analytes, under optimized experimental conditions. The analytical performance showed good precision (RSD < 15%), detection limits of 0.25 µg/L and linear dynamic ranges (1.0–25.0 μg/L) with determination coefficient higher than 0.9904. By using the standard addition method, the application of the present method to surface water matrices allowed very good performances at the trace level. The proposed methodology proved to be a suitable alternative to monitor phenol compounds in surface water matrices, showing to be easy to implement, reliable, sensitive and requiring a low sample volume.

Highlights

  • Phenol compounds such as nitrophenols, bisphenols and alkylphenols are classified as potential endocrine disruptor chemicals and often detected in the environment [1]

  • The most widely used methodologies for the determination of trace levels of phenol compounds is solid phase extraction followed by gas chromatography (GC) after derivatization [3,10]

  • Solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE) with in-situ derivatization followed by GC coupled to mass spectrometry (GC-MS) analysis, or LC-MS without the derivatization step had been proposed to monitor the class of compounds [4,11,12,13,14,15]

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Summary

Introduction

Phenol compounds such as nitrophenols, bisphenols and alkylphenols are classified as potential endocrine disruptor chemicals and often detected in the environment [1]. Our group has introduced a novel static microextraction technique, bar adsorptive microextraction (BAμE), that uses nanostructured materials, and have demonstrated it to be a remarkable alternative for trace analysis of medium-polarity to polar compounds in aqueous media [16,17]. This new analytical approach operates under the floating sampling technology and has demonstrated great advantages compared to other sorption-based methods (e.g., SBSE). The optimization, validation, application and comparison with others sorbent-based techniques are addressed

Instrumental Conditions
Selection of the Sorbent Phase
Optimization of the Recovery Assays
Application to Real Matrices
Chemicals and Samples
Preparation of the Microextraction Bars
Recovery Assays and Method Validation
Instrumentation Settings
Conclusions
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