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目的:建立宁德大黄鱼中硒的微波消解氢化物原子荧光光谱测定方法。方法:样品经微波消解,在铁氰化钾—盐酸体系中,用硼氢化钾作还原剂,采用氢化物原子荧光光谱法测定。结果:硒浓度在0~50μg/L的范围内线性良好,相关系数r=0.9998,方法检出限为0.15μg/L,样品检出限0.019 mg/kg,相对标准偏差0.91%~4.22%,回收率94%~104%。结论:方法灵敏度高,准确度好,精密度高,干扰少,简便适用,适合大黄鱼中硒的测定。
Objective: To establish a method for determination of selenium in Ningde big yellow croaker by microwave digestion hydride atomic fluorescence spectrometry. Methods: Samples were digested by microwave and potassium borohydride as reductant in potassium ferricyanide - hydrochloric acid system and determined by hydride atomic fluorescence spectrometry. Results: The calibration curve was linear in the range of 0-50 μg / L with a correlation coefficient of 0.9998. The detection limit was 0.15 μg / L, the detection limit was 0.019 mg / kg, the relative standard deviation was 0.91% -4.22% Recovery 94% ~ 104%. Conclusion: The method has the advantages of high sensitivity, good accuracy, high precision, less interference and simple and convenient application, suitable for the determination of selenium in large yellow croaker.