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目的建立高效液相色谱-原子荧光光谱法测定大米中不同形态砷的检测方法。方法样品经0.15 mo/lL硝酸溶液热浸提后离心过滤,提取液以液相色谱分离后进原子荧光光谱仪测定,按保留时间定性,外标法定量。结果该方法的三价砷(AsⅢ)、五价砷(AsⅤ)、一甲基砷(MMA)和二甲基砷(DMA)的线性范围为0~100μg/L,相关系数0.9990以上,检出限为0.005~0.008μg/ml,精密度相对标准偏差(RSD)<6%,用于实际样品的加标回收率为79%~120%。结论该方法操作简单,可靠,结果准确,适合于大米中4种砷形态的测定。
Objective To establish a method for the determination of different forms of arsenic in rice by high performance liquid chromatography-atomic fluorescence spectrometry. Methods The samples were hot-leached with 0.15 mol / l L nitric acid solution and centrifuged. The extracts were separated by liquid chromatography and then determined by atomic fluorescence spectrometry. The samples were characterized by retention time and quantified by external standard method. Results The linear range of As Ⅲ, AsⅤ, MMA and DMA was 0 ~ 100 μg / L and the correlation coefficient was 0.9990. Limit of 0.005 ~ 0.008μg / ml, precision relative standard deviation (RSD) <6%, for the actual sample spike recovery of 79% to 120%. Conclusion The method is simple, reliable and accurate. It is suitable for the determination of four kinds of arsenic in rice.