Published:Journal of Chromatographic Science,
ISSN 0021-9665Volume
38, Number 4, April 2000, pp. 174–180
Analysis
and Quantitation of Rotenoids and Flavonoids in Derris (Lonchocarpus urucu)
by High-Temperature High-Resolution Gas ChromatographyAlberto
dos Santos Pereira, Maria Angelis Afonso Serrano, Francisco Radler de Aquino
Neto, and Angelo da Cunha Pinto Instituto de Química, Universidade Federal do Rio
de Janeiro, Ilha do Fundão, Centro de Tecnologia, Bloco A, Sala 607,
21949-900, Rio de Janeiro, Brazil Dulcineia Furtado Texeira and Benjamin Gilbert Laboratório de Química de Produtos
Naturais, Far-Manguinhos, Fundação Oswaldo Cruz, 21041-250, Rio
de Janeiro, Brazil
A glass capillary
column coated with PS-086 (15% phenyl–80% methylpolysiloxane, 15 m x 0.30-mm
i.d., 0.1-µm film thickness) is used to analyze extracts from Lonchocarpus
urucu (Derris urucu). Several secondary metabolites (8 flavonoids, 10 rotenoids)
are characterized without derivatization, and the rotenoids are quantitated
by high-temperature high-resolution gas chromatography (HTHRGC) and HTHRGC coupled
with mass spectrometry (HTHRGC–MS). The limit of detection in flame ionization
detection of rotenone is approximately 0.5 µg/mL, and the limit of quantitation
was 2 µg/mL. Derris urucu bark is an excellent source of rotenone
isomers (80 mg/g), deguelin (30 mg/g), and rotenolone (26 mg/g). Single solvent
extractions (hexane, methylene dichloride, acetone, or methanol) are not able
to fully extract the flavonoids and rotenoids. Complete extraction is achieved
using a mixture of methanol–methylene dichloride (1:1), indicating a complex
association of these compounds with the plant tissue. HTHRGC and HTHRGC–MS
are shown to be quick and informative tools for the rapid analysis of crude
extracts without the need for prior derivatization and fractionation.
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