摘要
对巯基棉分离硒的方法进行了改进,建立了一种IMEP-17人血清样品中痕量硒的同位素稀释电感耦合等离子体质谱测量方法。采用微波消解-巯基棉分离对人血清样品进行前处理,通过对巯基棉分离血清中硒的条件优化,结果表明,柱条件为5 mol/L HCl、解脱Se条件为1 mL重蒸HNO3、巯基棉最佳用量为0.14 g时,能够有效分离出人血清样品中的Na、Mg、K、Ca等碱金属和碱土金属,同时硒的回收率最高,达到92%以上。将该前处理方法应用到同位素稀释电感耦合等离体质谱法中,平行取样6次,测量结果的平均值为(0.07747±0.00046)μg/g,在标准值(0.07896±0.0027)μg/g的不确定度范围内。
A method for the determination of selenium in serum samples ( IMEP- 17) by Isotope Dilution- Inductively has been developed. The serum selenium is first digested by International Measurement Evaluation Programme Coupled Plasma-Mass Spectrometry (ID-ICP-MS) microwave treatment and then chemically purified before analysis by using sulphydryl cotton. The optimum conditions were found to be as follows: (1) The sulphydryl cotton column is prewashed with 5 mol/L hydrochloric acid; (2) Se is desorbed by adding 1 mL of concentrated nitric acid and (3) the optimum amount of sulphydryl cotton is 0.14 g. This preconcentration step is required in order to remove matrix-interfering elements, such as Na, Mg, K and Ca. The recovery of selenium is above 92 %. The proposed ID-ICP-MS method has been used to determine Se in reference serum materials and the results of six independent measurements (average value is (0. 07747 ± 0. 00046) μg/g) showed good agreement with the certified value((0.07896 ± 0.0027)μg/R).
出处
《北京化工大学学报(自然科学版)》
EI
CAS
CSCD
北大核心
2007年第3期293-295,共3页
Journal of Beijing University of Chemical Technology(Natural Science Edition)
关键词
同位素稀释质谱法
多接收电感耦合等离子体质谱
微波消解
巯基棉
硒
人血清
isotope dilution mass spectrometry
multiple collector inductively couple mass spectrometry
microwave digestion
sulphydryl cotton
selenium
serum