Quantitative capillary electrophoresis ion spray tandem mass spectrometry determination of EDTA in human plasma and urine

被引:73
作者
Sheppard, RL [1 ]
Henion, J [1 ]
机构
[1] CORNELL UNIV,ITHACA,NY 14850
关键词
D O I
10.1021/ac9700686
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A quantitative method has been developed for the determination of EDTA in human plasma and urine, The samples are prepared with automated anion-exchange solid-phase extraction using 100 mu L of human plasma. The extracts are analyzed by capillary electrophoresis/mass spectrometry using selected reaction monitoring in the negative ion mode. Lace-volume injections (10% of the CE capillary volume) are used to improve the concentration level of detection via field-amplified sample injection. The first reported validation of a CE/MS/MS technique was carried out for this method. Using a C-13 stable-label isotope for the internal standard, the lower level of detection and lower level of quantitation were determined to be 7.3 and 14.6 ng/mL EDTA in human plasma, respectively. The injection precision had a relative standard deviation (RSD) of 6.1%. The intra-assay precision was less than 15% RSD, The intra-assay accuracy was less than +/-12% bias from the nominal concentration, The interassay precision was less than 18% RSD and the interassay accuracy was less than +/-9% bias from the nominal concentration.
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页码:2901 / 2907
页数:7
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