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目的建立氢化物发生原子荧光测定昆布中无机砷含量(亚砷酸盐As(III)和砷酸盐As(V))的方法。方法采用1%硝酸90℃水浴提取昆布中的无机砷,5%双氧水氧化As(III)成As(V)。以强阴离子交换固相萃取(SPE)技术消除一甲基砷酸(MMA)、二甲基砷酸(DMA)的干扰,无机砷以As(V)形式洗脱,氢化物发生原子荧光法(HG-AFS)测定无机砷。结果线性范围为0~20μg/L,线性相关系数0.999 7,加样回收试验低、中、高浓度平均回收率分别为83%、90%、92%,样品7次测定RSD为5.3%,方法检出限0.046μg·L-1。测定结果与液相色谱-电感耦合等离子体质谱法(LC-ICP-MS)结果比对满意。结论本方法操作简便,仪器配置要求低,满足分析测试要求,适用于一般实验室昆布中无机砷的测定。
AIM: To establish a method for the determination of inorganic arsenic (As (III) and As (V) As) in khumbu by atomic fluorescence spectrometry. Methods The inorganic arsenic in kelp cloth was extracted with 1% nitric acid at 90 ℃ and As (V) was oxidized by 5% hydrogen peroxide. The interference of monomethyl arsenic acid (MMA) and dimethyl arsenate (DMA) was eliminated by strong anion exchange solid phase extraction (SPE). The inorganic arsenic was eluted with As (V) and the hydride generation atomic fluorescence HG-AFS) for the determination of inorganic arsenic. The results showed that the linear range was 0 ~ 20μg / L and the linear correlation coefficient was 0.999 7. The average recoveries of low, medium and high concentration in the recovery test were 83%, 90% and 92%, respectively. The RSD of the samples was 5.3% The detection limit was 0.046μg · L-1. The results are in good agreement with the results of liquid chromatography-inductively coupled plasma mass spectrometry (LC-ICP-MS). Conclusion The method is simple and easy to operate, the instrument configuration requirements are low, meet the analysis and testing requirements, applicable to the determination of inorganic arsenic in the general laboratory kelp.