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目的优化湿法消解-原子荧光光谱法的实验条件,建立高效准确的海产品总砷含量检测方法。方法烘干后的样品经优化的硝酸、高氯酸和硫酸混合酸体系加热消解后,经硫脲-抗坏血酸还原,通过原子荧光光谱法进行测定。结果所建立的总砷含量检测法加标回收率94%~102%,相对标准偏差1.8~2.6%;在1~40.0μg/L的浓度范围内,相关系数r为0.9994,方法检测限低至0.004mg/kg,且试样检测结果与ICP-MS方法结果比对一致。结论该方法灵敏度高,准确性好,且极大地提高了检测效率,整个测定过程仅需1.5h,可满足大批量海产品总砷的测定。
Objective To optimize the experimental conditions of wet-digestion-atomic fluorescence spectrometry and establish a high-accuracy and accurate method for the determination of total arsenic in seafood. The dried samples were heated and digested by the mixed acid system of nitric acid, perchloric acid and sulfuric acid, then reduced by thiourea-ascorbic acid and determined by atomic fluorescence spectrometry. Results The total recovery of arsenic was 94% -102% and the relative standard deviation was 1.8-2.6%. The correlation coefficient r was 0.9994 in the concentration range of 1 ~ 40.0μg / L. The method detection limit was as low as 0.004mg / kg, and the sample test results and ICP-MS method results match. Conclusion The method has high sensitivity and good accuracy, and greatly improves the detection efficiency. The whole measurement process takes only 1.5 hours to meet the determination of total arsenic in large quantities of seafood.