摘要
建立了一种快速、准确、灵敏的高效液相色谱-原子荧光联用(HPLC-AFS)测定条斑紫菜中无机砷含量的方法。通过对仪器最佳参数和前处理方法进行优化结果表明,条斑紫菜以10%HCL70℃水浴提取1.5h,再用20%H2O2稀释一倍将As(Ⅲ)转化成As(V),可最大限度提取到无机砷;采用混合磷酸盐作流动相等度洗脱,在浓度为1-50μg/L的范围内,As(Ⅲ)、DMA、MMA、As(V)的标准曲线均具有良好的线性关系,相关系数大于0.999,无机砷的仪器检出限为1.13μg/L,方法检出限为0.023mg/kg;采用总砷提取率和砷形态加标回收率考察方法的准确性,总砷的提取率在87%以上,加标回收率在90%以上。该方法简便易行,灵敏度高,准确性好,可应用于条斑紫菜中无机砷含量的测定。
A method for determination of inorganic arsenic in Porphyra yezoensis by high performance liquid chromatography and hydride generation atomic fluorescence spectrometry was developed. The samples were extracted with 10%HCL at 70℃ ,then the extracts were oxidized with hydrogen peroxide to transform As(Ⅲ) into As(V).The conditions and parameters of both HPLC and AFS were optimized. The results showed that the linear range for As(V) was all between 1 to 50 μg/L with linear cofficients more than 0.999, instrument detection limit was 1.13μg/L and the method detection limit was 0.023mg/kg for inorganic arsenic. The extraction efficiency of total arsenic was more than 87% and the recoveries of standard addition were above 90%. The proposed method is simple, accurate and efficient and has been applied successfully in the determination of inorganic arsenic analysis in Porphyra yezoensis
出处
《现代科学仪器》
2017年第1期88-94,共7页
Modern Scientific Instruments
基金
江苏省农业自主创新项目[CX(13)3039]、江苏省大型仪器平台新方法开发项目(BZ201304)、国家海洋公益性行业科研专项(201105023)、(2013418007-1)资助