Hirata Shizuko, Toshimitsu Hideki, Aihara Masato
Biomass Technology Research Laboratory, National Institute of Advanced Industrial Science and Technology, 2-2-2 Hiro-suehiro, Kure 737-0197, Japan.
Anal Sci. 2006 Jan;22(1):39-43. doi: 10.2116/analsci.22.39.
Arsenic speciation analysis in marine samples was performed using high performance liquid chromatography (HPLC) with ICP-MS detection. The separation of eight arsenic species viz. arsenite (As(III)), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), arsenate (As(V)), arsenobetaine, trimethylarsine oxide (TMAO), arsenocholine and tetramethylarsonium ion (TeMAs) was achieved on a Shiseido Capcell Pak C18 column by using an isocratic eluent (pH 3.0), in which condition As(III) and MMA were co-eluted. The entire separation was accomplished in 15 min. The detection limits for 8 arsenic species by HPLC/ICP-MS were in the range of 0.02 - 0.10 microg L(-1) based on 3sigma of blank response (n=9). The precision was calculated to be 3.1-7.3% (RSD) for all eight species. The method then successfully applied to several marine samples e.g., oyster, scallop, fish, and shrimps. For the extraction of arsenic species from seafood products, the low power microwave digestion was employed. The extraction efficiency was in the range of 52.9 - 112.3%. Total arsenic concentrations were analyzed by using the microwave acid digestion. The total arsenics in the certified reference materials (DORM-2 and TORT-2) were analyzed and agreed with the certified values. The concentrations of arsenics in marine samples were in the range 6.6 - 35.1 microg g(-1).
采用高效液相色谱（HPLC）与电感耦合等离子体质谱（ICP-MS）检测联用的方法对海洋样品中的砷形态进行分析。在资生堂Capcell Pak C18柱上，使用等度洗脱液（pH 3.0）实现了8种砷形态即亚砷酸盐（As(III)）、一甲基砷酸（MMA）、二甲基砷酸（DMA）、砷酸盐（As(V)）、砷甜菜碱、三甲基氧化砷（TMAO）、砷胆碱和四甲基砷离子（TeMAs）的分离，在此条件下As(III)和MMA共洗脱。整个分离过程在15分钟内完成。基于空白响应的3倍标准偏差（n = 9），HPLC/ICP-MS对8种砷形态的检测限在0.02 - 0.10 μg L⁻¹范围内。所有8种形态的精密度计算为3.1 - 7.3%（相对标准偏差）。该方法随后成功应用于几种海洋样品，如牡蛎、扇贝、鱼类和虾类。对于从海产品中提取砷形态，采用了低功率微波消解。提取效率在52.9 - 112.3%范围内。通过微波酸消解分析总砷浓度。对有证标准物质（DORM-2和TORT-2）中的总砷进行了分析，结果与认定值一致。海洋样品中砷的浓度在6.6 - 35.1 μg g⁻¹范围内。
