On-line preconcentration and determination of cobalt by DPTH-gel chelating microcolumn and flow injection inductively coupled plasma atomic emission spectrometry

被引:16
|
作者
Zougagh, M [1 ]
Rudner, PC [1 ]
de Torres, AG [1 ]
Pavón, JMC [1 ]
机构
[1] Univ Malaga, Fac Sci, Dept Analyt Chem, E-29071 Malaga, Spain
关键词
cobalt; flow injection; on-line preconcentration; DPTH-gel microcolumn; ICP-AES; biological samples;
D O I
10.1007/s00216-003-2213-6
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
This paper reports the development of a new methodology for the determination of cobalt in biological samples by using a flow injection system with loaded DPTH-gel as solid phase to preconcentrate analytes. The procedure is based on the on-line preconcentration of cobalt on a microcolumn of 1,5-bis(di-2-pyridyl)methylene thiocarbohydrazide immobilized on silica gel (DPTH-gel). The trapped cobalt is then eluted with 1% tartaric acid and 1% citric acid (7.1 mL) and determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The analytical figures of merit for the determination of cobalt are as follows: detection limit (3S), 8.5 ng mL(-1); precision (RSD), 5.8% for 100 ng mL(-1) of cobalt; enrichment factor, 13 (using 7.3 mL of sample); sampling frequency, 40 h(-1) using a 60-s preconcentration time. For a 120-s preconcentration time (14.6 mL of sample volume) a detection limit of 5.7 ng mL(-1), an RSD under 5% at 50 ng mL(-1), an enrichment factor of 25, and a sampling frequency of 24 h(-1) were reported. The precision and accuracy of the method were checked by analysis of biological certified reference materials.
引用
收藏
页码:423 / 428
页数:6
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