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依据GB 5009.11-2014检测稻谷中无机砷含量,对采用液相色谱—原子荧光光谱(LC-AFS)法测定稻谷中无机砷应注意的问题进行探讨,通过在实验中解决样品提取及仪器操作等过程中遇到的问题,减少实验中产生的误差,使As(Ⅲ)和As(Ⅴ)在0~80 ng/m L范围内线性良好,相关系数均为0.9993,总无机砷的最低检出限为0.01mg/kg,按0.16、0.32、0.64 mg/kg三个添加水平测定加标回收率在85.3%~114.0%之间,6次重复测定的As(Ⅲ)、DMA、MMA、As(Ⅴ)4个参数的RSD值分别为2.0%、4.0%、7.5%和11.2%,提高了检验结果的准确度和精密度。
Based on the detection of inorganic arsenic in rice by GB 5009.11-2014, the problems of inorganic arsenic in rice by liquid chromatography-atomic fluorescence spectrometry (LC-AFS) should be discussed. By solving the problems in sample extraction and equipment operation, (Ⅲ) and As (Ⅴ) in the range of 0 ~ 80 ng / m L, the correlation coefficient was 0.9993, the lowest detection rate of total inorganic arsenic The recoveries of As (Ⅲ), DMA, MMA, As (Ⅲ) were determined to be 0.01 mg / kg at the recoveries of 85.3% -114.0% at the three addition levels of 0.16,0.32,0.64 mg / Ⅴ) The RSD values of the four parameters were 2.0%, 4.0%, 7.5% and 11.2% respectively, which improved the accuracy and precision of the test results.