HSCCC Straightforward Fast Preparative Method for Isolation of Two Major Cytotoxic Withanolides from Athenaea fasciculata (Vell.) I.M.C. Rodrigues & Stehmann

Athenaea fasciculata belongs to the Solanaceae family and is a promising source of cytotoxic withanolides known as aurelianolides A and B. In the last years, the pharmacological studies of these aurelianolides on different leukemia cell lines have stimulated new studies on their potential as alterna...

Full description

Saved in:
Bibliographic Details
Published inPlants (Basel) Vol. 13; no. 21; p. 3039
Main Authors Marques, André Mesquita, Brito, Lavínia de Carvalho, Figueiredo, Maria Raquel
Format Journal Article
LanguageEnglish
Published Basel MDPI AG 01.11.2024
MDPI
Subjects
Acetic acid
Adsorption
Analysis
Antineoplastic drugs
Aureliana
aurelianolides
Cancer
CCC
Chemotherapy
Chromatography
Cytotoxicity
Drug development
Ethyl acetate
Hexanes
Leukemia
Liquid chromatography
Magnetic resonance spectroscopy
Methods
n-Hexane
Natural products
NMR spectroscopy
Nuclear magnetic resonance spectroscopy
Oncology, Experimental
Oxidation
Purity
Reproducibility
separations
Solvents
Toxicity
Tumor cell lines
Brazil
Online AccessGet full text

Cover

More Information
Summary:Athenaea fasciculata belongs to the Solanaceae family and is a promising source of cytotoxic withanolides known as aurelianolides A and B. In the last years, the pharmacological studies of these aurelianolides on different leukemia cell lines have stimulated new studies on their potential as alternative candidates for new lead anticancer drugs. However, the obtention of these two pure compounds by traditional preparative is a costly and long time-consuming process, which is performed in several steps. This study aimed to propose a straightforward approach for isolating aurelianolides A and B using high-speed countercurrent chromatography (HSCCC). In this study, among 10 different solvent systems, the system composed of n-hexane/ethyl acetate/methanol/water 3:6:2:1 (v/v/v/v) was chosen for optimization. This HEMWat system was optimized to 4:8:2:4 (v/v/v/v) and chosen for HSCCC separation in a tail-to-head elution mode. After the HSCCC scale-up procedure, a withanolides mixture (200.0 mg) was separated within 160 min in a single-step purification process. In total, 78.9 mg of aurelianolide A (up to 95.0% purity) and 54.3 mg of aurelianolide B (up to 88.5% purity) was obtained by this fast sequential liquid–liquid partition process. The isolated withanolides were identified by 1H and 13C NMR spectroscopy (this method has proven to be faster and more efficient than classical procedures (CC and Prep-TLC)).
ISSN:2223-7747
2223-7747
DOI:10.3390/plants13213039