建立了高效液相色谱一原子荧光分光光度法测定海产品中无机砷(AsV,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,r20.9997;DMA线性范围为0~100.00μg/L,r2=0.9993;MMA线性范围为0-100.00/ag/L,r20.9990;As(V)线性范围为0—100.00μg/L,,=0.9991;AsB线性范围为0-200.00μg/L,r2=0.9994。3个样品加标回收率为As(Ⅲ)86.7%-89.4%,DMA111.2%~117.0%,MMA109.7%~111.6%,As(V)83.8%-90.7%,AsB88-3%~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%∽=6)。5个价态的检出限(S/N=2)为As(Ⅲ)0.29gg/L,DMA0.36gg/L,MMA0.27gg/L,As(V)0.56μg/L,AsB1.46μg/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.