离子交换色谱-氢化物发生原子荧光法测定水产品中硒的形态  

Speciation analysis of selenium in aquatic products by ion exchange chromatography-hydride generationatomic fluorescence sectrometry

作　　者：谢小雪[1] 叶明德[1] 陈丹飞 陈露霞[1] 

机构地区：[1]温州大学化学与材料工程学院,温州325035

出　　处：《分析试验室》2014年第2期241-243,共3页Chinese Journal of Analysis Laboratory

摘　　要：建立了利用离子交换色谱-原子荧光联用技术同时测定水产品中3种硒形态的方法，研究了仪器的工作条件、载流、KBH。浓度对硒荧光信号值的影响。采用HamiltonPRPX-100色谱柱（250×4．1mm，10μm），以30mmol／LNH4H2P04为流动相，可以在10min内同时分离、检测了硒代胱氨酸SeCys、硒代蛋氨酸SeMet和Se（IV）。当3种形态的质量浓度范围为0～80μg／L时，各形态均得到良好的线性关系，线性相关系数均大于0．9990，各形态的检出限分别为SeCys1．66μg／L，SeMet0．91μg/L，Se（IV）1．10μg/L，相对标准偏差RSD均小于5％（n=11）。在最佳条件下，应用该方法测定了水产品中的硒形态，3种硒形态化合物加标回收率在87．3％～102．6％之间。方法可满足水产品中硒形态的定量分析。A sensitive analytical method was developed for for speciation of selenomethionine（SeMet） and seienate （ Se （ IV ） ） by ion chromatography conjugated Selenocystine （ SeCys ）, hydride generation-atomic fluorescence spectrometry（IC-HG-AFS）. The effects of conditions of instrument, current-carrying and potassium borohydride concentration on fluorescence single value of selenium species were optimized. An Anion-exchange column （PRP-X100） with eluent of 30 mmol/L NH4 H2PO4 was employed to separate these three species with in 10 min. On the optimized conditions, linear relationships between values of fluorescence intensity and mass concentration of selenium species were found in the same range of 0 ~ 80μg/L, with the correlative coefficients more than 0. 9990. The detection limits （3s/k） of SeCys, SeMet, Se （ 1V ） were 1.66, 0. 91, 1.10 μg/L, respectively, and the relative standard deviations （ n = 11 ） for the selenium species were all less than 5%. Applying the present procedure to the speciation analysis of selenium in aquatic products, the spiked recoveries from 87.3% to 102. 6% were obtained.

关 键 词：硒形态分析 离子交换色谱 氢化物发生-原子荧光光谱 

分 类 号：O657.3[理学—分析化学]