▎ 摘 要
Phthalate esters PAEs) are a group of serious environmental pollutants, which lead to carcinogenicity or tumorigenicity in human body. In this study, a rapid, sensitive and green method by graphene oxide coated hollow fiber membrane extraction GO-HFME) coupled with supercritical fluid chromatography SFC) was proposed for the determination of 11 phthalate esters in bottled beverages. Graphene oxide GO) was prepared and coated onto a porous hollow fiber membrane HFM) to reinforce the efficiency of membrane extraction. The modified hollow fiber membrane was employed for the extraction of phthalate esters from bottled beverages prior to the determination by the supercritical fluid chromatography with UV detection. To achieve the maximum extraction efficiency, several parameters were investigated including GO concentration, extraction time, desorption solution and desorption time. SFC variables including stationary phase, modifier composition and percentage, column temperature, flow rate and backpressure were studied to improve the separation conditions. Under these optimized conditions, all the studied 11 phthalate esters were well separated and simultaneously determined in 7 min by SFC. The performance of the developed method was evaluated. Good linearity was observed R >= 0.999) in the range of 0.02-10.0 mu g/mL with limit of detection LOD, S/N = 3) ranging from 1.5 to 3.0 ng/mL. Recoveries of all the PAEs for the spiked samples were between 92.1% and 99.3% with satisfactory relative standard deviations RSD) less than 5.9%. The proposed method is time-saving, green, simple and robust, which will be an alternative way to the analysis of PAEs in real samples. (C) 2018 Elsevier B.V. All rights reserved.