Artículos de revistas
Fast analysis of beta-ecdysone in Brazilian ginseng (Pfaffia glomerata) extracts by high-performance liquid chromatography using a fused-core column
Registro en:
Analytical Methods. Royal Soc Chemistry, v. 6, n. 8, n. 2452, n. 2459, 2014.
1759-9660
1759-9679
WOS:000333524200005
10.1039/c3ay42276c
Autor
Rostagno, MA
Debien, ICN
Vardanega, R
Nogueira, GC
Barbero, GF
Meireles, MAA
Institución
Resumen
Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) The recent development of fused-core technology in HPLC columns is enabling faster and highly efficient separations. This technology was evaluated for the development of a fast analysis method for beta-ecdysone in extracts of Pfaffia glomerata. A step-by-step strategy was used to optimize temperature (30-55 degrees C), flow rate (1.0-2.0 mL min(-1)), mobile phase composition (mixtures of water and methanol or acetonitrile) and equilibration time (1-5 min). A gradient method has been developed using two solvents: 0.1% acetic acid in water and 0.1% acetic acid in acetonitrile. Optimized conditions provided a method for the separation of beta-ecdysone in approximately 2 min with a total analysis time (sample-to-sample) of 9 min, including the return to initial conditions and the re-equilibration of the column. Evaluation of chromatographic performance revealed excellent intraday and interday reproducibility (>99.5%), resolution (2.78), selectivity (1.13), and peak symmetry (1.09) while presenting low limits of detection (0.20 mg L-1) and quantitation (0.67 mg L-1). The robustness of the method has also been calculated according to the concentration/dilution of the sample. Several sample solvents were evaluated and the best chromatographic results were obtained using 80% methanol in water. Finally, the developed method was validated with different extracts of Pfaffia glomerata samples. 6 8 2452 2459 Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) FAPESP [2012/10685-8, 2013/04304-4, 2013/15049-5] CNPq [470916/2012-5, 560914/2010-5, 140282/2013-0, 151165/2010-6]