Indian River Research and Education Center, University of Florida/IFAS, 2199 South Rock Road, Fort Pierce, FL 34945-3138, USA.
J Chromatogr A. 2012 Oct 5;1258:128-35. doi: 10.1016/j.chroma.2012.08.033. Epub 2012 Aug 17.
A gas chromatography/mass spectrometry (GC/MS)-based isotope dilution technique was developed for determination of environmental estrogens in vegetables and fruits. The isotopically labeled standards of related environmental estrogens were used as the isotope dilution standards (IDS) to form the following analyte/surrogate pairings: octylphenol/(13)C6-4-n-nonylphenol, 4-n-nonylphenol/(13)C6-4-n-nonylphenol, 4-nonylphenol/(13)C6-4-n-nonylphenol, bisphenol A/(13)C12-bisphenol A, estrone/(13)C6-estrone, 17-α-estradiol/(13)C6-β-estradiol, 17-β-estradiol/(13)C6-β-estradiol, 17-α-ethynylestradiol/(13)C2-17-α-ethynylestradiol, and estriol/D4-estriol. Plant samples were homogenized and extracted ultrasonically with acetone. Acid pretreatment greatly increased peak intensities for the analytes. Acid hydrolysis pretreatment was important for liberating conjugates of estrogenic contaminants in plant materials. Recoveries of the spiked analytes were greater than 90%. Method limits of detection (LOD) ranged from 0.01 to 0.20 μg kg(-1) while limits of quantification (LOQ) ranged from 0.04 to 0.60 μg kg(-1). Bisphenol, nonylphenol, and natural estrogens were detected in vegetable and fruit samples obtained from local markets, illustrating the feasibility of this method for determining trace estrogenic contaminants in vegetables and fruits. The method has significant environmental implications in terms of the simultaneous analysis of estrogenic contaminants in vegetables and fruit.
建立了一种基于气相色谱/质谱（GC/MS）的同位素稀释技术，用于测定蔬菜和水果中的环境雌激素。使用相关环境雌激素的同位素标记标准品作为同位素稀释标准品（IDS），形成以下分析物/替代物对：辛基酚/（13）C6-4-壬基酚、4-壬基酚/（13）C6-4-壬基酚、4-壬基酚/（13）C6-4-壬基酚、双酚 A/（13）C12-双酚 A、雌酮/（13）C6-雌酮、17-α-雌二醇/（13）C6-β-雌二醇、17-β-雌二醇/（13）C6-β-雌二醇、17-α-乙炔基雌二醇/（13）C2-17-α-乙炔基雌二醇和雌三醇/D4-雌三醇。植物样品经匀浆后用丙酮超声提取。酸预处理极大地增加了分析物的峰强度。酸水解预处理对于释放植物材料中雌激素污染物的结合物非常重要。加标分析物的回收率大于 90%。方法检出限（LOD）范围为 0.01 至 0.20 μg kg(-1)，定量限（LOQ）范围为 0.04 至 0.60 μg kg(-1)。从当地市场获得的蔬菜和水果样品中检测到双酚、壬基酚和天然雌激素，表明该方法可用于测定蔬菜和水果中痕量雌激素污染物。该方法在同时分析蔬菜和水果中的雌激素污染物方面具有重要的环境意义。
