【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。更多还原

【Abstract】 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,A(s V);0–200.00 μg/L for AsB,and correlation coefficients r2were 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),111.2%–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.更多还原