摘要
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0.15mol/L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予荧光光谱仪测定,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,相火系数0.9990以上,检出限为0.005-0008μg/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 methcxt to determinate arsenic of different forms in rice by high performancc liquid chromatography(HPLC) - hydride generation (HG) - atomic fluorescence spectrophotometry(AFS). Methods The samples were hot - dipped in 0.15 mol/L nitric acid solution, extracted, centrifuged and filtrated. Then the extract was subjected to scpa ration and determination of different arsenic forms by liquid chromatography and atomic fluorescence spectrometry, respectively, using retention time for qualitative assay and external reference method for quantitative assay. Results The linear range of arsenite (AsⅢ), arsenate (AsV), monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA) was 0 100 μg/L. The co efficient was above 0. 9990. The detection limit was 0. 005 0. 008μg/ml. The relative standard deviation (RSD) of the preci sion was less than 6%. And the recovery rate of standard addition applied to the sample was 79% - 120%. Conclusions Arsenic detection by HPLC- AFS is a simple, reliable and accurate method. It can be used to analyze four arsenic species in rice.
出处
《实用预防医学》
CAS
2013年第1期98-100,共3页
Practical Preventive Medicine