Resumo A oleorresina bruta não volátil das espécies de Burseraceae (breu), um produto florestal não madeireiro da Amazônia, ainda carece de métodos para seu controle de qualidade, embora suas atividades farmacológicas tenham sido associadas aos principais triterpenos α-amirina (αAA), β-amirina, α-amirenona, β-amirenona e lupeol (LU). Sua caracterização química tem sido geralmente determinada por cromatografia gasosa (CG), utilizando colunas com fases de baixa polaridade, que são ineficazes na separação de αAA e LU. O presente estudo teve como objetivo desenvolver um método de CG para caracterizar e quantificar triterpenos em breu comercial com boa seletividade e resolução. Colunas com fases de diferentes polaridades (DB-35, DB-1701, DB-17HT e DB-Innowax) foram testadas, e DB-17HT separou αAA e LU sem supressão de sinal ou alta retenção de outros constituintes. Esta coluna permitiu a quantificação de triterpenos do breu utilizando detecção de ionização de chama e colesterol como padrão de referência. A boa similaridade entre as curvas de calibração do colesterol e αAA foi verificada. Padronizações interna e externa levaram a quantificações diferentes (p < 0,05), mas a última apresentou menor desvio (RSD ≤ 3%). Este trabalho fornece um método de CG reprodutível para o controle de qualidade do breu comercial, evidenciando claramente a presença do lupeol e permitindo a quantificação precisa dos principais triterpenos.

Abstract Crude non-volatile oleoresin from Burseraceae species (breu), a non-timber forest product of the Amazon, still lacks methods for its quality control even though its pharmacological activities have been associated to the major triterpenes α-amyrin (αAA), β-amyrin, α-amyrenone, β-amyrenone and lupeol (LU). Its chemical characterization has usually been determined by gas chromatography (GC) using columns with phases of low polarity, which are ineffective in the separation of αAA and LU. The present study aimed to develop a GC method to characterize and quantify triterpenes in commercial breu with good selectivity and resolution. Columns with phases of different polarity (DB-35, DB-1701, DB-17HT and DB-Innowax) were tested, and DB-17HT separated αAA and LU without signal suppression or high retention of other constituents. This column allowed the quantification of breu triterpenes using flame ionization detection and cholesterol as a reference standard. Good similarity between the calibration curves of cholesterol and αAA was verified. Internal and external standardizations led to different (p < 0.05) quantifications, but the latter showed less deviation (RSD ≤ 3%). This work provides a reproducible GC method for the quality control of commercial breu, clearly evidencing the presence of lupeol and allowing the accurate quantification of major triterpenes.

Copaiba oil-resin, extracted from the trunk of Copaifera, and traditionally used in folk medicine in the treatment of various disorders, has been shown to be an effective antiinflamatory, antitumor, antitetanus, antiseptic and antiblenorrhagea agent. As, there are few studies evaluating its genotoxicity, this aspect of the commercial oil-resin, and its volatile and resinous fractions, were evaluated in mice by comet assay and micronucleus (MN) test. A single dose of oil resin, volatile or resin fractions (500; 1,000 or 2,000 mg/kg b.w.) was administered by gavage. The chemical compositions of Copaiba oil resin and its fractions was analyzed by gas chromatography. According to comet assaying, treatment with either one did not increase DNA damage, and as to MN testing, there was no alteration in the incidence of micronucleated polychromatic erythrocytes. Chromatographic analysis of the oil-resin itself revealed sesquiterpenes, diterpenic carboxylic acid methyl esters and high levels of β-caryophyllene. Thus, it can be assumed that the oil resin and volatile and resinous fractions from the commercial product are not genotoxic or mutagenic.