Copaifera L. genus (Leguminoseae) is native from tropical America, the producer of a valuable oilresin, named copaíba oil. This genus has 72 species, 16 of them endemic in Brazil. Copaíba oils are clear viscous liquids whose colour varies from yellow to brown, obtained by the direct exudation from trunk trees. The oilresin has many applications in the industries such as paints and varnishes, cosmetics, perfumery as odour fixative and is widely used in folk medicine. Many biological activities have been noticed to these oilresins, which are anthelmintic, analgesic, anti-inflammatory, gastroprotective, antitumor and trypanosomicidal, several therapeutic properties of copaíba oil were already confirmed by pharmacological studies. Chemically, Copaiba oilresins consist in a mixture of volatile sesquiterpenes and resinous diterpenic acids. Kaurans, clerodans and labdans are the main structural diterpene skeletons, some of them with biological properties already described, such as colavenol and the acids kaurenoic, hardwickiic, copalic and hydroxi-copalic. From a bioassay-guided fractionation, antitumor activity was verified for both hardwickiic acid and copalic acid. Our research groups, Amazonian Biomolecules Chemistry (Q-Bioma), in Manaus, Amazonas; and Advanced Bioprocesses on Chemistry of Natural Products (ABC-NP), in Rio de Janeiro, have been studying the upscaling process to isolate biomarkers and useful substances from Amazonian oilresins to allow formulations, in vivo studies and quality control establishment with reference substances. At the present project, the isolation of biomarkers of copaíba oils for their use in quality control is described. The compounds were fractionated using KOH impregnated silica, a technique used to be applied to obtain a better separation between the acidic compounds of the non-acids, without the usual emulsion formation problems. It is a more efficient and alternative technique, applied in laboratory scale and easily extended to larger quantities. In this technique, the sesquiterpenes are usually obtained with hexane, after a preparation of the KOH impregnated silica with isopropanol. Here, we describe, an alternative method, preparing the silica with an aqueous solution, and the first fraction obtained in dichloromethane (DCM) and diterpenic acids obtained as potassium salts, with methanol (MeOH). After column fractionation, the salt fraction is subjected to a liquid-liquid partition, collecting the fractions in DCM after being acidified to their respective pH values. Isolation of the acids was performed using a pH zone-refining gradient, followed by fast flash vacuum open-column chromatography to purify terpenes prior to crystallization. Mass spectrometry (MS) and nuclear magnetic resonance (NMR) were applied to identification. Hardwickiic, acetoxy-copalic, hydroxy-copalic and clorechinic acids were isolated using this methodology, that could be applied to several other matrices with varied amounts of terpenoid acids. In addition to the acids, a sesquiterpene was also isolated by the recrystallization technique. Its identification was performed by retention times comparison with linear hydrocarbons on gas chromatograph coupled to the flame ionization detector (GC-FID) and mass spectra (GC-MS) from literature, which related the substance as epi-α-bisabolol. As copalic acid was previously described as the only diterpene found in all copaiba oils, this acid can be used as a biomarker, a necessary substance to allow the authenticity of this oilresin at this quality control. The technique allowed an easier separation and upscaling purification of terpenic acids from copaíba oils.