The present study describes a rapid and solvent-free procedure for the determination of 4-tert-octylphenol (4-t-OP) and 4-nonylphenol isomers (4-NPs) in aqueous samples. The method involves one-step in situ acetylation, coupled with microwave-assisted headspace solid-phase microextraction (MA-HS-SPME) prior to their determination using gas chromatography-mass spectrometry (GC-MS). The effects of various derivatization and extraction parameters were systematically investigated and optimized. Under optimized conditions, 300 �L of acetic anhydride mixed with 1 g of potassium hydrogencarbonate and 2 g of sodium chloride in a 20-mL water sample were efficiently extracted by a 65 �m polydimethylsiloxane-divinylbenzene (PDMS-DVB) fiber that was located in the headspace when the system was microwave irradiated at 80 W for 5 min. The limits of quantification (LOQs) were 5 and 50 ng/L for 4-t-OP and 4-NPs, respectively. A standard addition method was used to quantitate 4-t-OP and 4-NPs, and the concentrations ranged from 120 to 930 ng/L in various environmental samples. This in situ acetylation MA-HS-SPME appears to be a good alternative extraction method for the determination of 4-t-OP and 4-NPs in environmental samples; it is a simple, effective, low-cost, and eco-friendly analytical method.

One-step in situ acetylation coupled with microwave-assisted headspace solid-phase microextraction for the rapid determination of alkylphenols in aqueous samples

243rd National Meeting (2012)

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