海鱼自然基质中汞和砷质量控制样品研制及在能力验证中应用

Preparation of natural-matrix quality control materials for determining Hg and As in marine fish and its usage in proficiency testing

目的研制汞、砷质量控制样品,对承担国家食品安全风险监测工作的各级疾病预防控制机构实施能力验证计划。方法采用直接测汞(DMA)法和电感耦合等离子体质谱(ICP-MS)法分别测定广东省采集的16种海鱼肌肉中汞和砷含量,确定以深海网箱养殖的单条大型鞍带石斑鱼为原料,然后经选取肌肉、干燥、脱脂、粉碎等步骤制成鱼肉粉样品。采用单因子方差分析样品均匀性和t检验检查稳定性。结果所制备鱼肉粉样品的均匀性和稳定性均良好。采用该样品对193个实验室实施能力验证计划,检测总汞和总砷满意率分别为81.1%和80.2%,其中采用DMA测定总汞和ICP-MS测定总砷的满意率最高。结论该鱼肉粉样品可作为质量控制样品应用于实验室检测汞、砷能力验证。本研究可为海产食品基质标准物质的研制以及相关食品安全国家标准的修订提供科学参考。

Objective To prepare the quality control materials（ QCMs） of mercury,arsenic in marine fish and implement the proficiency test in the centers for disease control and prevention that are responsible for national food safety risk monitoring. Methods Sixteen species of marine fish were collected from Guangdong Province and the total mercury and arsenic in these samples were determined using direct mercury analyzer（ DMA） and inductively coupled plasma mass spectrometry（ ICP-MS） respectively. Epinephelus lanceolatus was selected to prepare the QCMs,which was cultivated in deep sea cages. The procedure of preparing QCMs included freeze mincing the muscle,drying,degreasing,comminution and seal package. One way ANOVA was used for evaluating the homogeneity of QCMs,and t test for the stability. Results The experimental result showed that the Epinephelus oanceolutus QCMs remained well homogeneous and stable. The QCMs were used for proficiency testing which 193 laboratories had taken part in,the satisfactory performance rates of total mercury and arsenic were 81. 1% and 80. 2% respectively. DMA for mercury determination and ICP-MS for arsenic determination were the most efficient method. Conclusion The fish powder QCMs were suitable for total mercury,arsenic in food proficiency testing. This research provide method ology reference for both preparation of seafood based QCMs and edition of national food safety standard.