Sociedade Brasileira de Espectrometria de Massas – BrMASS
NAT – NATURAL PRODUCTS
Study and Characterization by Direct Infusion Electrospray
Ionization Mass Spectrometry of Rubus imperialis (Rosaceae) Crude
Extract
Paulo C. P. Rosa1,2, Carla C.S.S. Pereira2, Márcio A. Andréo3, Nilson A.
Assunção3, Fernando A. Fonseca3, Fábio F. Perazzo3
[email protected]
1
Faculdade de Ciências Médicas – UNICAMP, Campinas, SP, Brasil. 2Programa
de Pós-graduação e Biociências e Tecnologia de Produtos Bioativos,
Departamento de Biologia Vegetal, Instituto de Biologia, UNICAMP, Campinas,
SP, Brasil. 3Instituto Ciências Ambientais, Químicas e Farmacêuticas,
Universidade Federal de São Paulo - UNIFESP, Diadema, SP, Brasil.
Rubus imperialis, known popularly as “amora-do-mato” or “amora-branca” in Brazil, is
being well-distributed in South of Brazil and is frequently used in traditional medicine
as a remedy to treat diabetis and dolorous process. R. imperialis presents
hypoglycaemic, cytotoxic and antinociceptive actions and antimicrobial activity[1-3].
Phytochemical studies carried out with these plants indicate the presence of steroids,
triterpene and ellagic acid derivatives. Niga-ichigoside F1, showed marked
antinociception and its mechanism of action appears to be related to the dopaminergic,
cholinergic, glutamatergic, and tachykininergic and oxinitrergic systems[4]. Crude
extract from raíces de Rubus imperialis samples were dissolved in methanol with 0.1%
formic acid or in methanol:water (1:1) solution with 0.1% ammonium hydroxide. The
solutions were directly infused into the ESI ion source of the mass spectrometer. ESIMS and ESI-MS/MS spectra were acquired in the positive ESI(+)-MS ion mode for the
acidified solution and in the negative ESI(-)- MS ion mode for the alkalized solution.
The mass spectra were considered very distinctive, showing characteristic sets of ions
for the sample. In the negative ion mode, were detected the triterpene tomentic acid
(m/z 487), confirmed by fragments 485 m/z [M-2H]-; 459 m/z [M-H-CO]- and 441 m/z
[M –2H – CO2]- and an ellagic acid derivative (503 m/z). When using the positive ion
mode, was identified triterpene niga-ichigoside F1 (m/z 667)[2,5]. The directly infused
by ESI ion source of the mass spectrometer is a technique which needs a small portion
of sample, with a simple sample preparation in a quick analysis process. The technique
and method employed confirmed effective characterization of markers in the sample of
R. imperialis.
[1] Bella Cruz, A. et al., Acta Farm. Bonaerense 2006, 25 (2): 256-259.
[2] Kim, Y.H, Kang, S.S., Arch. Pharm. Res. 1993, 16 (2):109-113.
[3] Niero R, Kanegusuku M, Souza MM, Yunes RA, Cechinel-Filho V., Therapie. 2002 MayJun;57(3):242-5.
[4] Kanegusuku, M. et al., Biol. Pharm. Bull. 2007. 30(5) 999—1002.
[5] Filho, V.C., Química Nova, 2000, 23(5): 680-685.
5º Congresso BrMass – 07 a 11 de Dezembro de 2013