【摘要】 对水产品中辛基酚(OP)、壬基酚(NP)和双酚A(BPA)测定的前处理方法进行优化,建立凝胶渗透色谱-固相萃取-气相色谱-质谱分析(GPC-SPE-GC-MS)方法。样品经乙酸乙酯超声提取,凝胶渗透-HLB固相萃取净化,七氟丁酸酐衍生化,进行GC-MS分析检测。结果表明:OP、NP、BPA在HP-5MS柱上有良好分离,方法检出限分别为0.2、0.1、0.1μg/kg,平均回收率OP不低于83.4%,NP不低于80.5%,BPA不低于81.3%,相对标准偏差范围为3.73%~9.19%。该方法应用于莱州湾部分水产品样品分析检测,简单便捷、灵敏度高,适用于水产品中OP、NP和BPA的检测。更多还原

【Abstract】 On the basis of optimized sample pretreatment conditions, a method for the determination of octylphenol(OP), nonylphenol(NP) and bisphenol A(BPA) in aquatic products has been developed by gel permeation chromatography(GPC) coupled with solid phase extraction(SPE) and gas chromatography-mass spectrometry(GC-MS). The analytes were extracted with ethyl acetate and purified seuquentially by gel permeation chromatography a nd HLB solid phase extraction cartridges. After derivatization with heptafluorobutyrican anhydride(HFBA), the derivatives were determined by GCMS. The results showed that the derivatives of the analytes were well separated by an HP-5MS column, and the limits of detection for OP, NP and BPA were 0.2, 0.1 μg/kg and 0.1 μg/kg, respectively. The average recovery rates were more than 83.4%, 80.5% and 81.3%, respectively, with relative standard deviation(RSD) ranging from 3.73% to 9.19%. The method has been used to determine seafood samples from Laizhou Bay with high sensitivity and reliability.更多还原