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Liquid chromatographic analysis of the anticancer alkaloid luotonin A and some new derivatives in human serum samples
Author(s) -
GonzálezRuiz Víctor,
Mussardo Pierluigi,
Corda Elisa,
Girotti Stefano,
Olives Ana I.,
Martín María Antonia
Publication year - 2010
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201000175
Subject(s) - chromatography , chemistry , resolution (logic) , elution , high performance liquid chromatography , ether , gradient elution , detection limit , alkaloid , tetrahydrofuran , quantitative analysis (chemistry) , diethyl ether , reversed phase chromatography , organic chemistry , artificial intelligence , solvent , computer science
The quantitation of the natural cytotoxic and anti‐inflammatory alkaloid luotonin A and five recently synthesized derivatives is described, constituting the first report of a HPLC method for the analysis of these compounds in human serum samples. The conditions for the chromatographic separation were optimized and the method was validated for the analysis of these compounds in biological samples according to international guidelines. An RP‐HPLC method with fluorimetric detection and a C 18 stationary phase was applied. Different ACN/water mobile phases were assayed, including 0–4% of a mobile phase modifier such as tetrahydrofuran, dioxane or tert ‐butyl methyl ether. Isocratic and gradient elution conditions are compared. The influence of pH on the efficiency and resolution of the separation was also considered. The developed method was applied to the determination of luotonins in pooled human serum samples by gradient elution RP‐HPLC using a simple cleanup procedure. The proposed chromatographic method exhibits satisfactory analytical figures of merit, with LOD from 1.0×10 −10 to 2.0×10 −10 M, intraday and interday precision below 6% except for the concentration level closest to LOD, and good agreement between experimental and theoretical concentrations. Therefore, the developed method is suitable, reliable, rapid, and simple.