超临界流体色谱法同时测定海洋水体及沉积物中的4种双酚

Simultaneous measurement of bisphenols in seawater and marine sediment by supercritical fluid chromatography

在超临界流体色谱分析条件下,建立了由液液萃取与超临界流体色谱(supercritical fluid chromatography,SFC)同时测定海洋水体中双酚A (BPAF)、双酚AF (BPA)、双酚C (BPC)、四溴双酚A(TBBPA) 4种内分泌干扰物的方法。实验结果表明,当SFC流动相为超临界态二氧化碳和甲醇,检测波长为230 nm,柱温为36℃、流速为2.0 mL·min^(-1)、系统背压为12 MPa时,5 min内即可实现对双酚类化合物的分离。在线性浓度范围内,双酚类化合物的线性相关系数均高于0.998 9,检出限为0.03~0.06 mg·L^(-1),4种双酚类化合物在实际样品中的加标回收率为85.7%~112.0%,相对标准偏差均小于10.3%。本文方法可简便快速地检测海洋水体中的双酚,灵敏度和选择性较高,对研究和追踪海洋环境中双酚类化合物的分布具有重要意义。

An analytical method based on liquid-liquid phase extraction(LLE)coupled with supercritical fluid chromatography(SFC)is proposed for the simultaneous measurement of four bisphenols(bisphenol A,bisphenol AF,bisphenol C and tetrabromobisphenol A)in marine environmental samples.The related parameters of SFC are investigated in this paper.Under the optimum conditions of supercritical CO2 mixed methanol modifier as mobile phase,230 nm as detection wavelength,the 4 bisphenols could be separated completely within 5 minutes(flow rate:2.0 mL·min^(-1),temperature:36°C,backpressure:12 MPa).Bisphenols exhibited satisfactory linearity with correlation coefficients higher than 0.9989.The limits of detection are 0.03-0.06 mg·L^(-1),respectively.The proposed method was validated by the measurement of 4 bisphenols in marine samples with good spiked recoveries ranged between 85.7%and 112.0%with the relative deviations all were less than 10.3%.This method is convenient,fast,sensitive,accurate and selective,and is of great significance for tracking the distribution of endocrine disrupting compounds in the marine environment.