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目的通过湿法消解海产品的研究,建立科学准确稳定的海产品中总砷测定的分析方法。方法采取硝酸、高氯酸和硫酸混合体系并通过优化条件进行消解样品,利用氢化物原子荧光光谱法进行测定。结果砷在0μg/L~40μg/L浓度范围内呈良好线性关系,相关系数均大于0.999,测定相对标准偏差小于2.3%,通过对能力验证CNAS T0508鱼粉考核样、国家标准物质GBW08521紫菜以及国家标准物质GBW08573黄鱼的方法验证,检测结果均在标准参考值允许范围内,考核样鱼粉(7.12 mg/kg)检测值得到满意结果,检测值为7.22 mg/kg,回收率为91.71%~99.19%,黄鱼标准物质(5.08 mg/kg)检测值为5.10 mg/kg,回收率为102.25%~105.94%,紫菜标准物质(41 mg/kg)检测值为41.64 mg/kg,回收率为92.26%。结论该方法操作简便、准确灵敏,特别适用于实验室对海产品中总砷的测定。
Objective To establish a scientific and accurate method for the determination of total arsenic in seafood by wet digestion of seafood. Methods A mixture of nitric acid, perchloric acid and sulfuric acid was used to digest samples under optimized conditions and the determination was carried out by hydride generation atomic fluorescence spectrometry. Results Arsenic was linear with the concentration range of 0μg / L ~ 40μg / L, the correlation coefficient was greater than 0.999, and the relative standard deviation of determination was less than 2.3%. Through the verification of CNAS T0508 fish meal, the national standard GBW08521 seaweed and the national standard The test results of the substance GBW08573 were validated in the standard reference value. The test results of the sample fish meal (7.12 mg / kg) showed satisfactory results with the detection value of 7.22 mg / kg and the recoveries of 91.71% -99.19% The detection value of standard substance of yellow croaker (5.08 mg / kg) was 5.10 mg / kg, the recovery rate was 102.25% -105.94%, the standard value of seaweed (41 mg / kg) was 41.64 mg / kg and the recovery rate was 92.26%. Conclusion The method is simple, accurate and sensitive, especially suitable for laboratory determination of total arsenic in seafood.