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Quantitative Capillary Electrophoresis/Ion Spray Tandem Mass Spectrometry Determination of EDTA in Human Plasma and Urine

1997; American Chemical Society; Volume: 69; Issue: 15 Linguagem: Inglês

10.1021/ac9700686

1520-6882

Robin L. Sheppard, Jack D. Henion,

Environmental Chemistry and Analysis

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 μL of human plasma. The extracts are analyzed by capillary electrophoresis/mass spectrometry using selected reaction monitoring in the negative ion mode. Large-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 13C 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.