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Caracterização e controlo de qualidade da fração volátil dos óleos essenciais resinosos de Terebintina
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Os óleos essenciais (OEs) são misturas complexas de compostos voláteis extraídos de plantas, compostos sobretudo por terpenóides (monoterpenos e sesquiterpenos), e reconhecidos pelas suas propriedades bioativas. Um estudo observacional está a testar o óleo de terebintina “Diamond G Forest 100% Pure Gum Spirits of Turpentine” no tratamento da Síndrome de Angelman, após terem sido observadas melhorias neurológicas numa paciente posteriormente ao uso deste óleo. Adicionalmente, existe um óleo alternativo, o “Creekwood Naturals 100% Pure Gum Spirits of Turpentine”, que não revelou qualquer efeito de melhoria nos pacientes. Este projeto teve como objetivo desenvolver e validar um método de cromatografia gasosa acoplada à espectrometria de massa para caracterizar os terpenóides dos OEs de terebintina utilizados no estudo da Síndrome de Angelman e de outros disponíveis no mercado, e verificar a autenticidade destes OEs através da sua rotulagem, da legislação e da Farmacopeia.
Os resultados mostram que os 8 OEs de terebintina analisados são compostos principalmente por monoterpenos, sendo que em 6 deles não existe uma diferença significativa na percentagem de α- e β-pineno (≈75%). Contudo, foram observadas variações no perfil terpénico de 2 OEs, sendo que um apresentava um perfil mais complexo, uma percentagem relativamente inferior de α-pineno (≈30%) e ainda a presença de eucaliptol, enquanto o outro possuía uma percentagem muito inferior de β-pineno (≈3%). A análise quiral dos óleos revelou que 7 OEs possuíam uma maior percentagem de (–)-α-pineno e (–)-β-pineno, enquanto o óleo Creekwood possuía uma maior percentagem de (+)-α-pineno e (–)-β-pineno. Na validação do método foram avaliados os limites de deteção (1,5 a 5,0 mg/L) e quantificação (5,0 a 16,7 mg/L), a linearidade (r2 > 0,991 e Ftab > Fcalc), a precisão (<15%) e a justeza (<15%), cujos resultados demonstraram que o método analítico em estudo é adequado para a quantificação dos terpenóides. Quanto à autenticidade dos OEs, verificou-se que, no geral, os rótulos estavam em conformidade com a legislação europeia, sob diferentes enquadramentos legais.
Essential oils (EOs) are complex mixtures of volatile compounds extracted from plants, composed mainly of terpenoids (monoterpenes and sesquiterpenes), and recognised for their bioactive properties. An observational study is testing “Diamond G Forest 100% Pure Gum Spirits of Turpentine” oil in the treatment of Angelman Syndrome, after neurological improvements were observed in a patient following the use of this oil. Additionally, there is an alternative oil, the “Creekwood Naturals 100% Pure Gum Spirits of Turpentine”, which has not shown any improvement in patients. This project aimed to develop and validate a gas chromatography-mass spectrometry method to characterise the terpenoids of the turpentine EOs used in the study of Angelman Syndrome and others available on the market, and to verify the authenticity of these EOs through their labelling, legislation and the Pharmacopoeia. The results show that all 8 turpentine EOs analysed are composed mainly of monoterpenes, with no significant difference in the percentage of α- and β-pinene (≈75%) in 6 of them. However, variations were observed in the terpene profile of 2 EOs, one of which had a more complex profile, a relatively low percentage of α-pinene (≈30%) and the presence of eucalyptol, while the other had a much inferior percentage of β-pinene (≈3%). Chiral analysis of the oils revealed that 7 EOs had a higher percentage of (–)-α-pinene and (–)-β-pinene, while the Creekwood oil had a higher percentage of (+)-α-pinene and (–)-β-pinene. For the method validation, the limits of detection (1,5 to 5,0 mg/L) and quantification (5,0 to 16,7 mg/L), linearity (r2 > 0,991 and Ftab > Fcalc), precision (<15%) and accuracy (<15%) were evaluated, and the results demonstrated that the analytical method under study is suitable for the quantification of terpenoids. As for the authenticity of the EOs, it was found that, in general, the labels complied with the European legislation, under different legal frameworks.
Essential oils (EOs) are complex mixtures of volatile compounds extracted from plants, composed mainly of terpenoids (monoterpenes and sesquiterpenes), and recognised for their bioactive properties. An observational study is testing “Diamond G Forest 100% Pure Gum Spirits of Turpentine” oil in the treatment of Angelman Syndrome, after neurological improvements were observed in a patient following the use of this oil. Additionally, there is an alternative oil, the “Creekwood Naturals 100% Pure Gum Spirits of Turpentine”, which has not shown any improvement in patients. This project aimed to develop and validate a gas chromatography-mass spectrometry method to characterise the terpenoids of the turpentine EOs used in the study of Angelman Syndrome and others available on the market, and to verify the authenticity of these EOs through their labelling, legislation and the Pharmacopoeia. The results show that all 8 turpentine EOs analysed are composed mainly of monoterpenes, with no significant difference in the percentage of α- and β-pinene (≈75%) in 6 of them. However, variations were observed in the terpene profile of 2 EOs, one of which had a more complex profile, a relatively low percentage of α-pinene (≈30%) and the presence of eucalyptol, while the other had a much inferior percentage of β-pinene (≈3%). Chiral analysis of the oils revealed that 7 EOs had a higher percentage of (–)-α-pinene and (–)-β-pinene, while the Creekwood oil had a higher percentage of (+)-α-pinene and (–)-β-pinene. For the method validation, the limits of detection (1,5 to 5,0 mg/L) and quantification (5,0 to 16,7 mg/L), linearity (r2 > 0,991 and Ftab > Fcalc), precision (<15%) and accuracy (<15%) were evaluated, and the results demonstrated that the analytical method under study is suitable for the quantification of terpenoids. As for the authenticity of the EOs, it was found that, in general, the labels complied with the European legislation, under different legal frameworks.
Descrição
Dissertação para obtenção do grau de Mestre no Instituto Universitário Egas Moniz
Palavras-chave
Adulteração Compostos orgânicos voláteis Cromatografia gasosa Óleos essenciais Terebintina Síndrome de Angelman