摘要
建立了高效液相色谱–原子荧光分光光度法测定海产品中无机砷(As V,AsⅢ)、有机砷(DMA,MMA,AsB)含量的方法。样品经含10%(体积分数)HCl的提取液振荡提取、离心分离、二路形态分析预处理、高效液相色谱分离,用原子荧光光度计检测As(Ⅲ),DMA,MMA,As(V);四路条件(过氧化氢氧化和开启紫外灯)形态分析预处理装置处理,高效液相色谱分离,原子荧光光度计测定AsB。As(Ⅲ)线性范围为0～100.00μg/L,r2=0.999 7;DMA线性范围为0～100.00μg/L,r2=0.999 3;MMA线性范围为0～100.00μg/L,r2=0.999 0;As(V)线性范围为0～100.00μg/L,r2=0.999 1;AsB线性范围为0～200.00μg/L,r2=0.999 4。3个样品加标回收率为As(Ⅲ)86.7%～89.4%,DMA 111.2%～117.0%,MMA 109.7%～111.6%,As(V)83.8%～90.7%,AsB 88.3%～90.4%。用该方法测定虾仁(干)5个价态测定结果的相对标准偏差为3.07%～9.93%(n=6)。5个价态的检出限(S/N=2)为As(Ⅲ)0.29μg/L,DMA 0.36μg/L,MMA 0.27μg/L,As(V)0.56μg/L,AsB 1.46μg/L。该方法适用于海产品中As(Ⅲ),DMA,MMA,As(V),AsB含量的测定。
The method for the determination of inorganic arsenic（AsV, As Ⅲ ）, organic arsenic（DMA,MMA,AsB）in seafood by HPLC-AFS was established. The samples were surged and distilled with a mixed solution of 10% （volum ratio） HCl, separated in a centrifuge, then As（ Ⅲ ）, DMA, MMA, As（V）were determined by second road speciation analysis of pretreatment device and HPLC-AFS; AsB was determined by four road （ hydrogen peroxide oxidation and UV light was turned ） speciation analysis of pretreatment device and HPLC-AFS. The linear range was 0-100.00 μg/ L for As （Ⅲ ）, DMA, MMA,As（ V ）; 0-200.00 μg/L for AsB, and correlation coefficients r： were 0.999 7, 0.999 3, 0.999 0, 0.9991, 0.999 4 respectively. The three samples recoveries were 86.7%-89.4% for As（ Ⅲ ）, 1 11.2%--117.0% for DMA, 109.7%-111.6% for MMA, 83.8%-90.7% for AsV, 88.3%-90.4% for AsB. The relative standard deviation of determination results of shrimp （dry） samples of 5 valence states was 3.07%-9.93%（n=6）, and detection limit （S/N=2） of the method were 0.29,0.36,0.27, 0.56,1.46 μg/L for As（ Ⅲ ）, DMA,MMA, As（V）, AsB, respectively. The method is suitable for determination of As （Ⅲ ）, DMA, MMA, As （V）, AsB in seafood.
出处
《化学分析计量》
CAS
2013年第1期11-14,共4页
Chemical Analysis And Meterage
基金
广西科技基础条件平台建设项目(07-105-002-01)
