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Master's Dissertation
DOI
https://doi.org/10.11606/D.75.2015.tde-17082015-143533
Document
Author
Full name
Gabriela Ribeiro Silva
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Carlos, 2015
Supervisor
Committee
Yariwake, Janete Harumi (President)
Araujo, Angela Regina
Cavalheiro, Alberto Jose
Title in Portuguese
Estudo de alcaloides dos frutos de Passiflora alata e de Passiflora edulis por SBSE, CLAE-Flu e identificação por CLUE-EM
Keywords in Portuguese
alcaloides harmânicos
CLUE-EM/EM
Passiflora alata
Passiflora edulis
SBSE/CLAE-Flu
Abstract in Portuguese
O maracujá, nome popular atribuído ao fruto das diversas espécies do gênero Passiflora, da família Passifloraceae, é amplamente comercializado e consumido no mundo, sendo o Brasil um dos maiores produtores do fruto. Alguns estudos apontam possível toxicidade relacionada às espécies de Passiflora, principalmente P. incarnata. No entanto, há pouco conhecimento acerca das espécies P. edulis e P. alata, sobretudo em relação à polpa e sementes. Os extratos da polpa e das sementes dos frutos dessas duas espécies de "maracujá", Passiflora alata e Passiflora edulis, foram estudados com o objetivo de identificar alcaloides harmânicos, pelo preparo das amostras por extração por sorção em barra magnética recoberta com polidimetilsiloxano (SBSE-PDMS) e SBSE recoberta com polietilenoglicol silicone (SBSE-EG Silicone) e análise por cromatografia líquida de alta eficiência com detector por fluorescência (CLAE-Flu) e cromatografia líquida de ultra eficiência acoplada à espectrometria de massas sequencial (CLUE-EM/EM). A análise dos alcaloides harmana e harmina nos extratos da polpa de P. alata foi feita por meio do método de adição de padrão e mostrou menor quantidade destes alcaloides, em comparação com os resultados da análise dos extratos da polpa dos frutos de P. edulis, no trabalho de Pereira e colaboradores. As análises CLUE-EM e CLUE-EM/EM possibilitaram a identificação dos alcaloides nos extratos: nas sementes de P. alata, os alcaloides harmana, harmina, harmol, harmalol e harmalina foram identificados, enquanto que na polpa, harmana e harmina tiveram a confirmação da sua presença. Nos extratos da polpa dos frutos de P. edulis observou-se os alcaloides harmana, harmina e harmalina. E nas sementes de P. edulis harmina foi encontrada, porém há indícios da presença de harmana. A literatura sobre as barras de SBSE-EG Silicone Twister&®; não relata nenhum estudo relacionado ao seu uso para extração e concentração de alcaloides harmânicos nos extratos de P. alata e P. edulis. Por isso foi proposto inicialmente a aplicação do planejamento fatorial fracionário para otimização do método de extração, utilizando os padrões comerciais dos alcaloides harmana e harmina. O planejamento experimental revelou as variáveis principais e seus níveis de importância, e a partir destes resultados foi realizado o estudo cinético dos tempos de extração e de dessorção das barras de SBSE-EG Silicone. Porém, os resultados mostraram que as barras de SBSE-EG Silicone não são adequadas para a extração dos alcaloides harmana e harmina, uma vez que a recuperação obtida foi baixa, na ordem de 30%.
Title in English
Alkaloids studies from Passiflora alata and Passiflora edulis fruits analyzed by SBSE, CLAE-Flu, and identified by CLUE-EM.
Keywords in English
harman alkaloids
Passiflora alata
Passiflora edulis
SBSE/HPLC-Flu
UHPLC-MS/MS.
Abstract in English
"Maracujá" is the popular name given to the fruit of several species of Passiflora genus, from Passifloraceae family, it is widely commercialized and consumed around the world, and Brazil is one of the largest producers of this fruit. Some studies pointed out the possible toxicity related to Passiflora species, mainly P. incarnata. Although, there is a lack of knowledge about the P. edulis and P. alata species, especially with regards to the pulp and seeds. The extracts of pulp and seeds from the "maracujá" species Passiflora alata and Passiflora edulis, were studied in order to identify harman alkaloids. The samples were prepared by extraction with sorptive stir bar coated with polydimethylsiloxane (SBSE-PDMS) and SBSE coated with polyethylene glycol silicon (SBSE-EG Silicone). The samples were analyzed by high performance liquid chromatography with fluorescence detector (HPLC-Flu), and ultra-high pressure liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Harmane and harmine alkaloids in P. alata pulp extracts were analyzed using the standard addition method and the results showed a lower amount of these alkaloids, compared with the test results for the extracts from the P. edulis pulp in the work of Pereira et al. UHPLC-MS and UHPLC-MS/MS analysis enabled to identify the alkaloids amount present in the extracts. In the P. alata seeds extract the following alkaloids were identified harmane, harmine, harmol, harmalol and harmaline, while in the pulp extract, harmane and harmine were confirmed. In the extracts of P. edulis pulp the alkaloids identified were harmane, harmine and harmaline. And in the P. edulis seeds extract the harmine alkaloid was found, some indications of the presence of harmana were observed. The literature about SBSE-EG Silicone Twister® bars reports no study related to their use for extraction and concentration of harman alkaloids in P. alata and P. edulis. Thus, it was initially proposed the application of fractional factorial design to optimize the extraction method using commercial standards of harmane and harmine alkaloids. The experimental design revealed the main variables and their importance levels, and from these results kinetic studies were performed for the extraction and desorption times of SBSE-EG Silicone bars. However, the results showed SBSE-EG Silicone bars are not suitable for the extraction of harmane and harmine alkaloids, since the recovery obtained was low, on the order of 30%.
 
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Publishing Date
2015-08-18
 
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