摘要
1.000 0g样品经38 mL的0.5 mmol·L^(-1)(NH_4)_2CO_3溶液-甲醇(99+1)混合液(pH 8.5)超声萃取2h后,加入乙酸2mL,用水定容至50mL,离心后,上清液在Hamilton PRPX100阴离子分析柱(250mm×4mm,10μm)上分离,以0.5mmol·L^(-1)碳酸铵溶液-甲醇(99+1)混合液为流动相A(pH 8.5),50mmol·L^(-1)碳酸铵溶液-甲醇(99+1)混合液(pH 8.5)为流动相B进行梯度洗脱,9种砷形态化合物在20 min内达到完全分离,经电感耦合等离子体质谱法测定。9种砷形态化合物的质量浓度在一定范围内与峰面积呈线性关系,测定下限(10S/N)在50~100μg·kg^(-1)之间。加标回收率在74.0%~109%之间,测定值的相对标准偏差(n=6)在5.4%~13%之间。方法用于海产品中9种砷形态化合物的测定,结果表明样品中的砷主要以无毒的砷甜菜碱形式存在。
After 1.000 0g of the sample was ultrasonically extracted with 38 mL of a mixed solution （pH 8.5）of 0.5mmol·L^-1（NH4）2CO3 solution and methanol （99＋1） for 2h,2mL of acetic acid was added into the extract and the solution was diluted to 50 mL with water.After centrifugation,the supernatant was seperated on a Hamilton PRP-X100 anion analytical column（250 mm×4 mm,10μm）,with a mixture （pH 8.5）of 0.5mmol·L^-1（NH4）2CO3 solution and methanol （99＋1） as mobile phase A,and a mixture （pH 8.5） of 50mmol·L^-1（NH4）2CO3 solution and methanol （99＋1） as mobile phase B,for gradient elution.Nine arsenic species were separated within 20 mins and detemined by ICP-MS.Linear relationships were found between the peak areas and the mass concentrations of nine arsenic species in definite ranges,with lower limits of determination （10S/N） in the range of 50-100μg·kg^-1.Recovery obtained by standard addition method were in the range of74.0%-109%,and RSDs （n=6） were in the range of 5.4%-13%.The proposed method was used to analyze marine products and it was found that the main arsenic specie in the sample was non-toxic arsenic betaine.
出处
《理化检验（化学分册）》
CSCD
北大核心
2017年第9期1087-1093,共7页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
广东出入境检验检疫局科研计划项目(2014GDK33)
