【作者】 尚德荣； 宁劲松； 赵艳芳； 郭莹莹； 翟毓秀； 王军； 盛晓风；

【Author】 SHANG,De-Rong1,2 ZHAI,Yu-Xiu1,2 Guo,Ying-Ying3 NING,Jin-Song1,2 ZHAO, Yan-Fang1,2 WANG,Jun3 SHENG,Xiao-Feng1,2 (1 Yellow Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences;Key Laboratory for Sustainable Utilization of Marine Fisheries Resources,Ministry of Agriculture,Qingdao 266071)(2.National Center for Quality Supervision and Test of Aquatic Products,Qingdao 266071,China) 3.Seafood Safety Laboratory,Ocean University of China,Qingdao 266003,China)

【机构】 中国水产科学研究院黄海水产研究所农业部海洋渔业资源可持续利用重点开放实验室； 国家水产品质量监督检验中心； 中国海洋大学水产品安全实验室；

【摘要】 通过比较总砷提取率、加标回收率和砷形态的转化,实验了不同条件下对4种砷形态化合物亚砷酸盐(AsⅢ)、二甲基砷化合物(DMA)、一甲基砷化合物(MMA)、砷酸盐(AsV)依次分离分析的影响,优化了提取剂及提取剂的浓度、提取时间及其仪器条件,建立了一种新的海藻中无机砷含量的测定方法:用1.2 mol/L HCl提取后再用双氧水氧化;pH=6.0的15 mmol/L(NH4)2HPO4溶液为流动相,采用等度高效液相色谱-氢化物发生原子荧光(HPLC-HG-AFS)测定,4种砷形态的线性相关系数均≥0.999;检出限为: AsⅢ0.6ng/mL;DMA 1.0ng/mL;MMA 0.9 ng/mL;AsV 2.6ng/mL。相对标准偏差均<4.0。该联用系统灵敏度高、准确性好,分别分析了藻类不同砷形态化合物。更多还原

【Abstract】 By comparing the total arsenic extraction efficiency,spiked recovery and the transformation of arsenic species,the influences of different conditions on analyzing four arsenical species(including AsⅢ,DMA,MMA and AsⅤ)were determined,and the concentration of extraction reagents,the extraction time and instrument conditions were optimized.A new method to determine the content of inorganic arsenic in seaweed was obtained:firstly the seaweeds were extracted with 1.2mol/L HCl,then the extracts were oxidized with hydrogen peroxide,and finally were analyzed by isocratic high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry(HPLC-HG-AFS) under the condition of 15 mmol/L(NH4) 2HPO4 flow phase(pH=6.0).The linear correlation coefficient for 4 arsenical species were all≥0.999,and the detection limits were 0.6ng/mL for AsⅢ,1.1ng/mL for DMA,0.9 ng/mL for MMA and 2.6ng/mL for AsⅤrespectively.The relative standard deviation was<4.0.The high sensitivity and good accuracy of the system in analyzing the different arsenic species in seaweeds were obtained.更多还原