原子荧光形态分析仪测定植物类海产品中砷形态化合物

Speciation of arsenic compounds in plant seafood by atomic fluorescence spectometry

目的:建立了离子交换色谱-氢化物发生双道原子荧光联用同时测定4种As形态的方法。方法:研究采用高效液相色谱-氢化物发生-原子荧光光谱砷形态分析在线联用系统,实现了在线分离分析4种砷的形态化合物(AsⅢ,DMAⅤ,MMAⅤ和AsⅤ)。结果:优化了各种实验参数。在优化的实验条件下,采用PRP-Xl00阴离子交换分析柱可以在12 min内分离、检测As的四种形态。在8%HCl和2%(m/V)KBH4的氢化物反应条件下,进样量100μl,各形态的检出限为:As(Ⅲ)0.48μg/L、DMA0.56μg/L、MMA0.44μg/L、As(V)0.52μg/L,各形态的精密度RSD(n=7)均小于5%(2.9%～4.9%)。当各As形态浓度范围为5μg/L～100μg/L时各形态均可得到良好的线性关系,线性相关系数均大于0.9992。结论:本法简便、快速、准确.灵敏度和精密度高。适用于植物类海产品中砷形态化合物的测定。

Objective：To establish a method for the determination of four arsenic species by the combination of Ion exchange chromatography and hydride generation atomic fluorescence spectrometry.Methods： In this research,an on-line system of HPLC and hydride generation atomic fluorescence spectrometry was used for arsenic speciation.It has realized on-line separation and analysis of four arsenic species（AsⅢ,DMAⅤ,MMAⅤ and AsⅤ）.Results： Various experimental parameters were optimized.Four arsenic species were separated by PRX-X100 anion exchange column and determined within 12 minutes in optimal conditions.Under the hydride reaction condition of 8%HCl and 2%（m/V）KBH4 with 100 μl injection volume,the detection limits of various forms were 0.48 μg/L for As（Ⅲ）,0.56 μg/L for DMA,0.44 μg/L for MMA and 0.52 μg/L for As（V）.The precision RSD of various forms was 5%（n=7）.The linear relationship was good in the range of 5 μg/L～100 μg/L content of various forms（r0.9992）.Conclusion： This method is simple,convenient,rapid and accurate with high sensitivity and precision.It was suitable for speciation of arsenic compounds in plant seafood