Production of rice husk bio-oil and comprehensive characterization (qualitative and quantitative) by HPLC/PDA and GC GC/qMS

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Authors: Eliane Lazzari, Allan dos Santos Polidoro, Bruna Onorevoli, Tiago Schena, Aline Nunes Silva, Enelise Scapin, Rosangela Assis, Jacques, Elina Bastos Caramão


Pyrolysis of rice husk (RH) is an efficient process for the transformation of biomass to bio-oil (high-added value product). Bio-oil consists of two immiscible phases (organic and aqueous) both with potential for the generation of important chemicals for the industry. The aim of this study was to produce bio-oil by pyrolysis of RH and elucidate its chemical composition. Response surface methodology (RSM) was successfully used to determine the optimal pyrolysis conditions for the RH dry bio-oil production using central composite design (CCD). Temperature and flow rate significantly affected the bio-oil production and higher dry bio-oil yield was achieved at 650 °C and N2 flow rate of 100 mL min−1 (predicted values of 16.9%). High performance liquid chromatography with photodiode array detection (HPLC/PDA) and comprehensive two-dimensional gas chromatography with quadrupole mass spectrometry detection (GC × GC/qMS) were used to provide a comprehensive characterization (qualitative and quantitative) of both phases from RH bio-oil. Through GC × GC/qMS analysis a total number of 98 compounds were found in organic phase; from these, 62 were quantified using a developed quantitative method by relative response factors (RRFs). Phenols and ketones (cyclic ketones) were majority in the organic phase, 8.21 and 5.90 wt%, respectively, and the benzofuran (1.37 wt%) corresponds to the major identified compound. HPLC/PDA analysis evidenced a high concentration of benzenediols and furfurals in the aqueous phase. Catechol was the major compound (2063 mg L−1) followed by furfural (997 mg L−1) and hydroquinone (899 mg L−1). This is the first time that GC × GC/qMS and HPLC/PDA has been used to characterize (qualitatively and quantitatively) both phases from RH bio-oil which showed potential use as a source of high-added value chemicals.

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