Arid
DOI10.1155/2012/975824
Analysis of Digoxin and Metildigoxin in Whole Blood Using Solid-Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry
Melo, Paula1,2; Machado, Rita3; Teixeira, Helena M.1,2,4,5
通讯作者Teixeira, Helena M.
来源期刊INTERNATIONAL JOURNAL OF ANALYTICAL CHEMISTRY
ISSN1687-8760
EISSN1687-8779
出版年2012
英文摘要

A simple and rapid UPLC/MS/MS method has been developed and validated for the analysis of digoxin and metildigoxin in whole blood. Samples were prepared by SPE extraction with Oasis HLB columns. Separation was achieved with an ACQUITY UPLC HSS T3 column (2.1 x 100; 1.8 mu m), at 35 degrees C. The mobile phase consisted of acetonitrile (70%) and ammonium formate 5 mM (30%). Total run time was 1.5 min operating at isocratic mode with a flow rate of 0.3 mL/min. Mass spectrometry detection was performed by positive mode electrospray, on the ammonium adducts with two transitions for each analyte and one for the IS (d(3)-digoxin). The method proved to be specific and linear over the range (0.3-10) ng/mL. This technique also showed high sensitivity with a 0.09 ng/mL LOD and a 0.28 ng/mL LOQ, for both substances. Percentage recovery ranged from 83 to 100% for digoxin and from 62 to 94% for metildigoxin. The intra- and interday precision CV were <= 10%.


类型Article
语种英语
国家Portugal
收录类别SCI-E
WOS记录号WOS:000323442000001
WOS关键词LC-MS ASSAY ; QUANTITATIVE-DETERMINATION ; CARDIAC-GLYCOSIDES ; HUMAN PLASMA ; URINE ; QUANTIFICATION
WOS类目Chemistry, Analytical
WOS研究方向Chemistry
资源类型期刊论文
条目标识符http://119.78.100.177/qdio/handle/2XILL650/172903
作者单位1.Natl Inst Legal Med, North Branch, P-4050167 Oporto, Portugal;
2.Forens Sci Ctr CENCIFOR, P-3000213 Coimbra, Portugal;
3.Univ Coimbra, Fac Sci & Technol, P-3030790 Coimbra, Portugal;
4.Univ Porto, Fac Med, P-4099002 Oporto, Portugal;
5.Univ Coimbra, Fac Med, P-3000548 Coimbra, Portugal
推荐引用方式
GB/T 7714
Melo, Paula,Machado, Rita,Teixeira, Helena M.. Analysis of Digoxin and Metildigoxin in Whole Blood Using Solid-Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry[J],2012.
APA Melo, Paula,Machado, Rita,&Teixeira, Helena M..(2012).Analysis of Digoxin and Metildigoxin in Whole Blood Using Solid-Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry.INTERNATIONAL JOURNAL OF ANALYTICAL CHEMISTRY.
MLA Melo, Paula,et al."Analysis of Digoxin and Metildigoxin in Whole Blood Using Solid-Phase Extraction and Liquid Chromatography Tandem Mass Spectrometry".INTERNATIONAL JOURNAL OF ANALYTICAL CHEMISTRY (2012).
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