微波辅助萃取-液质联用技术测底泥砷、硒的化学形态  

Simultaneous speciation of arsenic and selenium by high-performance liquid chromatography on-line with in ductively coupled plasma collision cell mass spectrometry in sediment samples

作　　者：彭岚[1] 谈明光[1] 李玉兰[1] 张桂林[1] 陈建敏[1] 金婵[1] 李燕[1] 

机构地区：[1]中国科学院上海应用物理研究所

出　　处：《分析试验室》2006年第5期10-14,共5页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金重大项目(10490182);中国科学院知识创新工程重要方向性项目(KJCX2-SW-No1)

摘　　要：建立了用反相离子对色谱和电感耦合等离子体质谱的联用技术同时测定As（Ⅲ）、 As（Ⅴ）、 MMA、 DMA、 Se（Ⅳ）、 Se（Ⅵ）、 SeMet和SeCys的砷、硒化学形态分析方法. 分别从流动相pH值、离子对试剂的浓度、甲醇量和流速4个方面进行了分离测定条件的优化. 利用碰撞池技术（CCT）较好地解决了^40Ar^35Cl^＋复合离子对^75As的干扰, 并使^80Se的测定成为可能, 有效地提高了灵敏度. 将该方法应用于上海市苏州河底泥样品的微波辅助萃取液的形态分析中, 砷和硒的检出限分别达到0.4～1.3 和0.5～1.9 μg/L.An ion-pair RP - HPLC coupled with hexapole ICP - MS method has been developed for simultaneous determination of arsenic and selenium compounds. Optimum separations of arsenite, arsenate, monomethylarsonate, dimethylarsinate, selenite, selenate, selenocystine and selcnomethionine are achieved by appropriated adjusting the pH, ion-pairing reagent concentration, methanol content and flow rate. The hexapole collision cell technique （CCT） is employed for the elimination of the polyatomic interferences of the argon chloride （^40Ar ^35 Cl^＋ ） and ^40At ^40Ar^＋ , when arsenic and selenium are determined using their major isotopes by ICP - MS. The extraction of arsenic and selenium species from sediment samples of Suzhou river followed a microwave-assisted extraction procedure, and the extracts were then analysed by HPLC - ICP - MS for speciation. Detection limits are in the range of 0.4 - 1.3 μg/L arsenic and 0.5 - 1.9 μg/L selenium for various species.

关 键 词：化学形态 碰撞池 液质联用 砷 硒 

分 类 号：O657.7[理学—分析化学]