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

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。

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

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 0.998 9.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.