摘要: A rapid and solvent‐free procedure for the determination of 4‐tert‐octylphenol and 4‐nonylphenol isomers in aqueous samples is described. The method involves in‐situ acetylation and microwave‐assisted headspace solid‐phase microextraction prior to their determination using gas chromatography–ion trap mass spectrometry operated in the selected ion storage mode. The dual experimental protocols to evaluate the effects of various derivatization and extraction parameters were investigated and the conditions optimized. Under optimized conditions, 300 μL of acetic anhydride mixed with 1 g of potassium hydrogencarbonate and 2 g of sodium chloride in a 20 mL aqueous sample were efficiently extracted by a 65 μm polydimethylsiloxane‐divinylbenzene fiber that was located in the headspace when the system was microwave irradiated at 80 W for 5 min. The limits of quantitation were 5 and 50 ng/L for 4‐tert‐octylphenol and 4‐nonylphenol isomers, respectively. The precision for these analytes, as indicated by relative standard deviations, were less than 8% for both intra‐ and inter‐day analysis. Accuracy, expressed as the mean extraction recovery, was between 74 to 88%. A standard addition method was used to quantitate 4‐tert‐octylphenol and 4‐nonylphenol isomers, and the concentrations ranged from 120 to 930 ng/L in various environmental water samples. 其他題名: J. Sep. Science 出版者: Weinheim: Blackwell Publishing Ltd 出版日期: 2012-08 出處: Journal of separation science, 2012-08, Vol.35 (16), p.2122-2130 資源來源: Wiley Online Library All Journals 版權: 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim 版權: 2014 INIST-CNRS 版權: 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. 版權: 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim 識別號: ISSN: 1615-9306 識別號: ISSN: 1615-9314 識別號: EISSN: 1615-9314 識別號: DOI: 10.1002/jssc.201200146 識別號: PMID: 22899640