水产品中六溴联苯测定方法的建立及应用分析

建立水产品中痕量水平六溴联苯（hexabromobiphenyls，HexaBBs）的气相色谱检测方法，并对HexaBBs在不同水产品中的蓄积差异性进行特征分析。对前处理方法的提取试剂、超声时间、固相萃取小柱以及毛细管色谱柱的类型进行优化。结果表明，乙酸乙酯为提取试剂、超声时间为10 min，采用硅胶柱净化，经配有DB-17MS色谱柱的气相色谱分析效果最佳。5 种HexaBBs在0.20～10.00 ng/mL质量浓度范围内线性关系良好，线性相关系数均大于0.998，方法检出限为0.50 μg/kg，定量限为1.00 μg/kg。在1.00、5.00 μg/kg水平下加标回收率在77.15%～118.14%之间，相对标准偏差在0.56%～13.32%之间。本方法可用于定量分析水产品中残留的痕量HexaBBs，并且发现HexaBBs在不同营养级的水产品间存在蓄积性差异。

Development and Application of a Method for Determination of Hexabromobiphenyls in Aquatic Products

An analytical method was established for the determination of trace levels of hexabromobiphenyls (HexaBBs) in aquatic products by gas chromatography (GC) and the accumulation characteristics of HexaBBs in different aquatic products were analyzed. Important operating parameters were optimized, including extraction solvents, ultrasonic treatment time, types of solid-phase extraction (SPE) column and types of capillary column. Satisfactory results were achieved when the sample was ultrasonically extracted with ethyl acetate for 10 minutes, purified on a silica gel SPE cartridge, and detected by GC with an DB-17MS column. The linearity of the calibration curves for five HexaBBs was good in the range of 0.20–10.00 ng/mL, with correlation coefficients R2 greater than 0.998. The limits of detection and quantification of the proposed method were 0.50 and 1.00 μg/kg, respectively. The recoveries ranged from 77.15% to 118.14%, with relative standard deviations (RSD) in the range of 0.56%–13.32% at spiked levels of 1.00 and 5.00 μg/kg. This method could be used for the quantitative analysis of HexaBB residues in aquatic products, and the accumulation characteristics of HexaBBs in aquatic products from different trophic levels were found to be different from each other.