对海鱼粉中总砷含量的不同消解、检测方法对比探讨

Discussion on digestion methods and detection methods of total arsenic in marine-fish powder

目的对国家食品安全风险评估中心下发的HMRL1601海鱼粉质控样品中总砷含量进行测定,探讨最优检测方法。方法对国家标准方法推荐的电感耦合等离子体质谱法、原子荧光法的前处理条件进行优化,使用优化后的最佳条件检测并进行比对。结果采用原子荧光法检测总砷时,湿法消解比微波消解前处理效果好,而在使用湿法消解-AFS法时,采用硝酸-高氯酸-硫酸体系消解效果好;对于电感耦合等离子体质谱法测定样品中的总砷,微波消解比压力罐消解前处理效果好;2种方法进行比较时,微波消解-电感耦合等离子体质谱法测定的海鱼粉中总砷含量较为准确,而湿法消解-原子荧光法检测的结果相对偏低。结论相较于湿法消解-原子荧光法,微波消解-电感耦合等离子体质谱法更适合测定海鱼粉类有机砷含量较高的样品。

Objective To explore an optimum detection method for determining the content of total arsenic in the marine-fish powder（ HMRL1601） samples processed by China National Center for Food Safety Risk Assessment. Methods The pretreatment conditions of inductively coupled plasma-mass spectrometry andatomic fluorescence recommended by the present national standards were optimized,and the optimized conditions were applied for detection and compared with the method before optimization.Results When using atomic fluorescence method to detect the total arsenic,wet digestion was better than microwave on the pretreatment. But in the application of wet digestion-AFS method,the nitric acid-perchloric acid-sulfuric acid system was better. For the determination of total arsenic in samples by inductively coupled plasma mass spectrometry,microwave digestion was better than the pressure tank digestion on pretreatment. Microwave digestion with inductively coupled plasma-mass spectrometry can be suitable for the routine analysis of total arsenic in marine-fish powder,due to its accuracy and precision. While the detection results by wet digestion with atomic fluorescence spectrometer was relatively low. Conclusion Compared with wet digestion-atomic fluorescence method,microwave digestion with inductively coupled plasma-mass spectrometry can be more suitable for the detection of total arsenic in marine-fish powder.