Fast analysis of beta-ecdysone in Brazilian ginseng (Pfaffia glomerata) extracts by high-performance liquid chromatography using a fused-core column

Author(s)

Rostagno, Mauricio A. ^[1] ; Debien, Isabel C. N. ^[1] ; Vardanega, Renata ^[1] ; Nogueira, Gislaine C. ^[1] ; Barbero, Gerardo F. ^[2] ; Meireles, M. Angela A. ^[1]

Affiliation

^[1] Univ Estadual Campinas, UNICAMP, Sch Food Engn, LASEFI, DEA, FEA, BR-13083862 Campinas, SP - Brazil

^[2] Univ Cadiz, Agrifood Campus Int Excellence CeiA3, Fac Sci, Analyt Chem Dept, Cadiz 11510 - Spain

• Document type: Journal article
• Source: ANALYTICAL METHODS; v. 6, n. 8, p. 2452-2459, 2014.
• Web of Science Citations: 10

Abstract

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. (AU)

• FAPESP's process: 13/04304-4 - Development of integrated systems for the analysis of bioactive compounds in natural products employing supercritical technology
• Grantee: Maurício Ariel Rostagno
• Support Opportunities: Research Grants - Young Investigators Grants
• FAPESP's process: 12/10685-8 - Combination and coupling of processes for the production and encapsulation of value-added vegetal extracts: technical and economic evaluation
• Grantee: Maria Angela de Almeida Meireles Petenate
• Support Opportunities: Regular Research Grants
• FAPESP's process: 13/15049-5 - Development of integrated systems for the analysis of bioactive compounds in natural products employing supercritical technology
• Grantee: Maurício Ariel Rostagno
• Support Opportunities: Scholarships in Brazil - Young Researchers