作　　者： ; ; ;

机构地区： 宁波大学材料科学与化学工程学院宁波市新型功能材料及其制备科学国家重点实验室培育基地

出　　处： 《分析测试学报》 2009年第8期940-943,共4页

摘　　要： 建立了微波消解-固相萃取／石墨炉原子吸收法富集并测定米面中痕量铍的方法。采用微波消解制样，7．（2’-胂酸基-5’-羧酸）苯偶氮-8-羟基喹啉-5-磺酸（H2L）与Be^2＋螯合形成BeL络合物，C18固相萃取柱（C18-SPE）富集BeL，石墨炉原子吸收法测定C18柱洗脱液中的BeL。最佳实验条件为：采用50μL pH3．0的50g/LH2L水溶液与样品中的铍螯合15min，水相上柱，用2mL50％（体积分数）甲醇溶液洗脱。结果表明，方法的线性范围为0．05～14μg/L，检出限为0．02μg/L，对实际米面样品测定的加标回收率为90％-110％，可用于食品等复杂基质中痕量铍的测定。 A graphite furnace atomic absorption spectrometry（ GF -AAS） method for the determination of Be^2＋ in food sample was established by pre-extraction using 7-（ 2＇-arsenazo acid-5＇-carboxylic acid） phenylazo-8-hydroxyl-quinoline-5-sulfonic acid（H2L） as extraction agent. The separation and enrichment of Be ion in food samples was performed on a C18-solid phase extraction（ Cls-SPE） column. The optimum experimental conditions were using 50 μL 50 g/L H2L to react with Be ion in pH 3.0 buffer for 15 rain, with flow rate of 1.5 mL/min. The analyte was eluted by 2.0 mL 50% （ by volume） methanol solution. The calibration curve showed a good linearity over the Be concentration in the range of 0.05 - 14 μg/L with a detection limit of 0. 02 μg/L. The method was applied to the determination of Be in rice and flavor samples and the results obtained were in good agreement with those of ICP - AES method. The method was probably employed in the determination of Be^2＋ in food with complex matrix.

关 键 词： 微波消解 固相萃取 石墨炉原子吸收光谱法 米面 铍

领　　域： [理学] [理学]