目的:建立大黄鱼中砷汞的微波消解氢化物原子荧光光谱同时测定方法。方法:样品经微波消解,在硫脲—抗坏血酸—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同时测定。结果:砷浓度在0~20μg/L的范围内线性良好,相关系数r=0.9997,方法检出限为0.057μg/L,样品检出限5.7μg/kg,相对标准偏差0.88%~2.38%,回收率95.6%~98.6%;汞浓度在0~2.0μg/L的范围内线性良好,相关系数r=0.9999,方法检出限为0.004μg/L,样品检出限0.4μg/kg,相对标准偏差0.91%~1.58%,回收率92.0%~96.0%。结论:方法灵敏度高,准确度好,精密度高,干扰少,简便适用,适合大黄鱼中砷汞的同时测定。 Objective: To establish a method for simultaneous determination of arsenic and mercury in large yellow croaker by microwave digestion and hydride generation atomic fluorescence spectrometry. Methods: The sample was digested by microwave, thiourea - ascorbic acid - hydrochloric acid system, with potassium borohydride as reducing agent, simultaneous determination of hydride atomic fluorescence spectrometry. Results: The calibration curve was linear in the range of 0 ~ 20μg / L with a correlation coefficient of 0.9997. The detection limit was 0.057μg / L, the detection limit was 5.7μg / kg, the relative standard deviation was 0.88% -2.38% The recoveries ranged from 95.6% to 98.6%. The calibration curve was linear over the range of 0-2.0 μg / L with a correlation coefficient of 0.9999. The detection limit was 0.004 μg / L and the detection limit was 0.4 μg / kg. The relative standard Deviation 0.91% ~ 1.58%, recovery 92.0% ~ 96.0%. Conclusion: The method has the advantages of high sensitivity, good accuracy, high precision, less interference and simple application. It is suitable for simultaneous determination of arsenic and mercury in large yellow croaker.