Extraction of Bidens pilosa L. oil using supercritical fluid: biological activity and mathematical modeling

Submitted by Jorge Silva (jorgelmsilva@ufrrj.br) on 2021-08-24T20:58:58Z No. of bitstreams: 1 2018 - Ramon Gredilha Paschoal.pdf: 2464690 bytes, checksum: 9f0f8b6abcfd1a5d9daa897b202a1de7 (MD5) Made available in DSpace on 2021-08-24T20:58:58Z (GMT). No. of bitstreams: 1 2018 - Ramon Gredilha Paschoal.pdf: 2464690 bytes, checksum: 9f0f8b6abcfd1a5d9daa897b202a1de7 (MD5) Previous issue date: 2018-04-18 CNPq - Conselho Nacional de Desenvolvimento Cient?fico e Tecnol?gico FAPERJ (Funda??o Carlos Chagas Filho de Amparo ? Pesquisa do Estado do Rio de Janeiro) Fiotec (Funda??o para o Desenvolvimento Cient?fico e Tecnol?gico em Sa?de) Bidens pilosa L. (Asteraceae), better known as Black Jack, is a plant popularly used in the treatment of malaria, inflammation and various types of tumors, and is now widely disseminated throughout the tropical and subtropical region of the world. Among the several components present in the extract of this plant, the presence of flavonoids, polyacetylenes and terpenes are abundant, suggesting that most biological activities are directly linked to the presence of these metabolites. The selective extraction of these compounds with supercritical fluid is an alternative technology to the problems found in the conventional extractions, since there is a strong solvation power, and does not require the use of organic solvents. Therefore, this study had as objective the extraction of the high aggregated value substances present in this plant using supercritical CO2 in different pressure and temperature conditions. For this, 8 g of previously dried and milled Bidens pilosa leaves were fed in an extractor with 42 mL of volume. The unity also contained a high pressure pump, and a micrometric valve for sample removal. Different operating conditions were investigated (150 bar - 60 ?C; 179 bar - 46 ?C; 179 bar - 74 ?C; 250 bar - 40 ?C; 250 bar - 80 ?C; 321 bar - 46 ?C; 321 bar - 74 ?C and 350 bar - 60 ?C and 250 bar - 60 ?C), according to an experimental design. It was observed that the extraction yield increased with increasing pressure. According to the results, the best extraction condition was 321 bar and 74 ?C, obtaining a yield of 0.082% (6.6 mg). The analyses of the extracted oils were performed using high performance liquid chromatography (HPLC-DAD) and gas chromatography (GC-MS). Under conditions of 321 bar at 74 ?C and 250 bar at 40 ?C, signals were found showing ultraviolet spectra of terpenes characteristics of essential oils. The extracts analyzed showed promising inhibition in two tumor cell lines used, melanoma, SK-MEL-28 (68%) and leukemia, K562 (90%), both at a concentration of 150 ?g/mL. Subsequently, the experimental data were modeled by the models of Esquivel et al. (1999), Reverchon e Osseo (1994), Zekovi? et al. (2003), Sovov? (1999), Brunner (1984) and Kandiah e Spiro (1999), showing good correlation. The models of Chrastil (1982), Adachi e Lu (1983), Del Valle e Aquilera (1988) and Gordillo (1999) were able to represent the behavior of the solubility of the oils in different conditions of temperature and pressure. A Bidens pilosa L. (Asteraceae), mais conhecida como pic?o-preto, ? uma planta popularmente usada no tratamento da mal?ria, inflama??es e diversos tipos de tumores e, atualmente, se encontra amplamente disseminada por toda a regi?o tropical e subtropical do mundo. Dentre os diversos componentes do extrato dessa planta, destaca-se a presen?a de flavonoides, poliacetilenos e terpenos, cuja abund?ncia sugere que a maioria das atividades biol?gicas estejam diretamente ligadas a presen?a desses metab?litos. Na busca pela extra??o e obten??o seletiva desses compostos, a extra??o com fluido supercr?tico ? uma tecnologia alternativa aos problemas encontrados nas extra??es convencionais, visto que h? um forte poder de solvata??o n?o necessitando da utiliza??o de solventes org?nicos. Diante do que foi exposto, este estudo teve como objetivo extrair prioritariamente as subst?ncias de alto valor agregado presentes nessa planta, utilizando CO2 supercr?tico, em diferentes condi??es de press?o e temperatura. Para isso, 8 g de folhas de Bidens pilosa, previamente secos e mo?dos, foram alimentados a um extrator de 42 mL. A unidade experimental ainda consiste de uma bomba de alta press?o e uma v?lvula microm?trica para remo??o da amostra. Foram investigadas diferentes condi??es operacionais (150 bar - 60 ?C; 179 bar - 46 ?C; 179 bar - 74 ?C; 250 bar - 40 ?C; 250 bar ? 80?C; 321 bar - 46 ?C; 321 bar - 74 ?C, 350 bar - 60 ?C e 250 bar - 60 ?C), de acordo com um planejamento experimental. Observou-se que o rendimento do extrato aumentou com o aumento da press?o. De acordo com os resultados, a melhor condi??o para extra??o foi a 321 bar e 74 ?C, capaz de obter um rendimento de 0,082% (6,6 mg). As an?lises dos ?leos extra?dos foram realizadas utilizando cromatografia l?quida de alta efici?ncia (CLAE-DAD) e cromatografia gasosa (CG-EM). Nas condi??es de 321 bar a 74 ?C e 250 bar a 40 ?C foram encontrados sinais que apresentaram espectros ultravioleta de terpenos caracter?sticos de ?leos essenciais. Os extratos analisados mostraram ser promissores inibidores nas duas linhagens de c?lulas tumorais utilizadas, a de melanoma, SK-MEL-28 (68%) e a de leucemia, K562 (90%), ambos em concentra??o de 150 ?g/mL. Posteriormente, os dados experimentais foram correlacionados aos modelos de Esqu?vel et al. (1999), Reverchon e Osseo (1994), Zekovi? et al. (2003), Sovov? (1999), Brunner (1984) e Kandiah e Spiro (1999), apresentando bom comportamento. Os modelos de Chrastil (1982), Adachi e Lu (1983), Del Valle e Aquilera (1988) e Gordillo (1999) conseguiram representar o comportamento da solubilidade dos ?leos com a varia??o de temperatura e press?o, corroborando os dados experimentais.