食品科学 ›› 2021, Vol. 42 ›› Issue (14): 293-300.doi: 10.7506/spkx1002-6630-20191226-322

• 安全检测 • 上一篇    下一篇

水产品中六溴联苯测定方法的建立及应用分析

张龙飞,于慧娟,田良良,方长玲,黄冬梅,乔艺飘,史永富   

  1. (1.上海海洋大学食品学院,上海 201306;2.中国水产科学研究院东海水产研究所,农业农村部水产品质量监督检验测试中心(上海),上海 200090)
  • 发布日期:2021-07-27
  • 基金资助:
    农业部公益性行业(农业)科研专项(201503108);2018年农业行业标准制定项目

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

ZHANG Longfei, YU Huijuan, TIAN Liangliang, FANG Changling, HUANG Dongmei, QIAO Yipiao, SHI Yongfu   

  1. (1. College of Food Science and Technology, Shanghai Ocean University, Shanghai 201306, China; 2. Fishery Products Quality Inspection and Test Centre (Shanghai), Ministry of Agriculture and Rural Affairs, East China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Shanghai 200090, China)
  • Published:2021-07-27

摘要: 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。

关键词: 水产品;六溴联苯;分析;气相色谱;蓄积差异

Abstract: 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.

Key words: aquatic products; hexabromobiphenyls; analysis; gas chromatography; difference in accumulation characteristics

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