Xavier-Junior Francisco Humberto, Maciuk Alexandre, Rochelle do Vale Morais Andreza, Alencar Everton do Nascimento, Garcia Vera Lucia, Tabosa do Egito Eryvaldo Sócrates, Vauthier Christine
Institut Galien Paris Sud, CNRS UMR 8612, Faculté de Pharmacie, University Paris-Sud, Université Paris-Saclay, Five Rue J.B. Clément, 92296 Chatenay-Malabry Cedex, France.
Centro de Ciências da Saúde, Departamento de Farmácia, Laboratório de Sistemas Dispersos (LaSiD), Universidade Federal do Rio Grande do Norte, Av. Gal. Gustavo Cordeiro de Farias, S/N, Petrópolis 59010-180, Natal, RN, Brazil.
J Chromatogr Sci. 2017 Nov 1;55(10):969-978. doi: 10.1093/chromsci/bmx065.
A rapid, simple, precise and economic method for the quantification of main compounds of copaiba resin and essential oils (Copaifera langsdorffii Desf.) by gas chromatography (GC) has been developed and validated. Copaiba essential oil was extracted by hydrodistillation from the copaiba resin. Resin derivatization allowed the identification of diterpenes compounds. A gas chromatography-mass spectroscopy (GC/MS) method was developed to identify compounds composing the copaiba resin and essential oil. Then the GC/MS method was transposed to be used with a flame ionization detector (FID) and validated as a quantitative method. A good correlation between GC/MS and GC/FID was obtained favoring method transposition. The method showed satisfactory sensitivity, specificity, linearity, precision, accuracy, limit of detection and limit of quantitation for β-caryophyllene, α-humulene and caryophyllene oxide analyses in copaiba resin and essential oils. The main compounds identified in copaiba essential oil were β-bisabolene (23.6%), β-caryophyllene (21.7%) and α-bergamotene (20.5%). Copalic acid methyl ester (15.6%), β-bisabolene (12.3%), β-caryophyllene (7.9%), α-bergamotene (7.1%) and labd-8(20)-ene-15,18-dioic acid methyl ester (6.7%) were diterpenes identified from the derivatized copaiba resin. The proposed method is suitable for a reliable separation, identification and quantification of compounds present in copaiba resin and essential oil. It could be proposed as an analytical method for the analysis of copaiba oil fraction in raw and essential oil parent extracts and after they have been incorporate in pharmaceutical formulations.
已开发并验证了一种通过气相色谱法（GC）对苦配巴树脂和精油（南美苦配巴）主要成分进行快速、简单、精确且经济的定量方法。苦配巴精油通过水蒸馏法从苦配巴树脂中提取。树脂衍生化可鉴定二萜类化合物。开发了一种气相色谱 - 质谱联用（GC/MS）方法来鉴定构成苦配巴树脂和精油的化合物。然后将该GC/MS方法转换为与火焰离子化检测器（FID）联用，并作为定量方法进行验证。GC/MS和GC/FID之间获得了良好的相关性，有利于方法转换。该方法在苦配巴树脂和精油中β-石竹烯、α-葎草烯和氧化石竹烯分析方面显示出令人满意的灵敏度、特异性、线性、精密度、准确度、检测限和定量限。苦配巴精油中鉴定出的主要化合物为β-红没药烯（23.6%）、β-石竹烯（21.7%）和α-佛手柑油烯（20.5%）。从衍生化的苦配巴树脂中鉴定出的二萜类化合物有柯帕酸甲酯（15.6%）、β-红没药烯（12.3%）、β-石竹烯（7.9%）、α-佛手柑油烯（7.1%）和labd-8(20)-ene-15,18-二酸甲酯（6.7%）。所提出的方法适用于可靠地分离、鉴定和定量苦配巴树脂和精油中存在的化合物。它可作为一种分析方法，用于分析生苦配巴油馏分、精油母提取物以及它们被纳入药物制剂后的情况。
