Recent advances and comparisons of conventional and alternative extraction techniques of phenolic compounds.

Phenolic compounds are a group of secondary metabolites produced by plants under stressful conditions. Phenolic compounds play an important role in the prevention and treatment of certain illnesses and are exploited by the food and pharmaceutical industries. Conventional methods are commonly used as models to compare the efficiencies of alternative extraction methods. Among alternative extraction processes, microwave-assisted extraction (MAE), pressurized liquid extraction (PLE), supercritical fluid extraction (SFE) and ultrasonic-assisted extraction (UAE) are the most studied. These methods produce extracts rich in phenolic compounds using moderate temperatures, short extraction times, and solvents generally recognized as safe. The combination of extraction time and temperature plays a critical role in the stability of the compounds. Solvents of higher polarity enhance the extraction of phenolic compounds. The use of the ethanol-water mixture for MAE, PLE, and UAE is recommended. MAE and UAE involve shorter extraction times than do PLE and SFE. SFE requires a low average temperature (40 °C). MAE produces the highest total phenolic content [227.63 mg GAE/g dry basis (d.b.)], followed by PLE (173.65 mg GAE/g d.b.), UAE (92.99 mg GAE/g d.b.) and SFE (37 mg GAE/g d.b.). Extraction yields and recovery rates of the phenolic compounds can be enhanced by combining and integrating extraction methods.

Ultrasound-Assisted Extraction of Phenolic Compounds from Adenaria floribunda Stem: Economic Assessment.

Adenaria floribunda is a native species found in tropical regions of South America used as a traditional medicine. Ultrasound-assisted extraction (UAE) is an extraction process known to increase the extraction yield, reduce extraction times, and use low temperatures. This study aims to obtain water-based extracts from A. floribunda stems using UAE, hot water extraction (HWE), and Soxhlet extraction and perform an economic analysis. The global extraction yield (GEY) and total phenolic compounds (TPC) of extracts ranged from 5.24% to 10.48% and from 1.9 ± 0.44 mg GAE g-1 DW to 6.38 ± 0.28 mg GAE g-1, respectively. Gallic acid, catechin, and ferulic acid were identified in the extract using HPLC-UV. Results indicate that Soxhlet extraction has the best performance regarding GEY and TPC. However, after performing an economic assessment, the cost of manufacturing (COM) of Soxhlet extraction (US$ 5.8 flask-1) was higher than the UAE (US$ 3.86 flask-1) and HWE (US$ 3.92 flask-1). The sensitivity results showed that obtaining extracts from A. floribunda by UAE and HWE is economically feasible when the selling price is above US$ 4 flask-1. Soxhlet extraction is a feasible technique when the selling price is above US$ 7 flask-1.

A comparative and economic study of the extraction of oil from Baru (Dipteryx alata) seeds by supercritical CO2 with and without mechanical pressing.

The present study evaluated the effect of supercritical fluid extraction (SFE) assisted by cold pressing (SFEAP) on the overall yield, extraction kinetics, composition of baru seed oil and manufacturing cost (COM). The best extraction conditions were determined in extraction assays combining different pressures (150-350 bar) and temperatures (35 and 45 °C). The extraction yield by SFEAP (28.6 g oil/100 g baru seed) was approximately 31% higher than that obtained by SFE (21.9 g oil/100 g baru seed), according to the kinetic study with the best extraction conditions (350 bar and 45 °C). The extraction yield observed under this condition allowed us to obtain a lower COM for both techniques (SFE was US$ 118.32/kg baru oil and SFEAP was US$ 87.03/kg baru oil) compared to lower pressures and temperatures. The oil obtained under all extraction conditions was rich in unsaturated fatty acids and other bioactive compounds. The extraction of baru seed oil by SFEAP resulted in a higher yield and lower manufacturing cost than SFE.

Obtaining bixin from semi-defatted annatto seeds by a mechanical method and solvent extraction: Process integration and economic evaluation.

This work involves the application of physical separation methods to concentrate the pigment of semi-defatted annatto seeds, a noble vegetal biomass rich in bixin pigments. Semi-defatted annatto seeds are the residue produced after the extraction of the lipid fraction from annatto seeds using supercritical fluid extraction (SFE). Semi-defatted annatto seeds are use in this work due to three important reasons: i) previous lipid extraction is necessary to recovery the tocotrienol-rich oil present in the annatto seeds, ii) an initial removal of the oil via SFE process favors bixin separation and iii) the cost of raw material is null. Physical methods including i) the mechanical fractionation method and ii) an integrated process of mechanical fractionation method and low-pressure solvent extraction (LPSE) were studied. The integrated process was proposed for processing two different semi-defatted annatto materials denoted Batches 1 and 2. The cost of manufacture (COM) was calculated for two different production scales (5 and 50L) considering the integrated process vs. only the mechanical fractionation method. The integrated process showed a significantly higher COM than mechanical fractionation method. This work suggests that mechanical fractionation method is an adequate and low-cost process to obtain a rich-pigment product from semi-defatted annatto seeds.

Fast analysis of curcuminoids from turmeric (Curcuma longa L.) by high-performance liquid chromatography using a fused-core column.

The recent development of fused-core technology in HPLC columns is enabling faster and highly efficient separations. This technology was evaluated for the development of a fast method for the analysis of main curcuminoids (curcumin, demethoxycurcumin and bisdemethoxycurcumin) present in extracts of turmeric (Curcuma longa L.). A step-by-step strategy was used to optimize temperature (40-55 °C), flow rate (1.0-2.5 mL min(-1)), mobile phase composition and equilibration time (1-5 min). A gradient method was developed using acidified water and acetonitrile combined with high column temperature (55 °C) and flow rate (2.5 mL min(-1)). Optimized conditions provided a method for the separation of these three curcuminoids in approximately 1.3 min with a total analysis time (sample-to-sample) of 7 min, including the clean-up and the re-equilibration of the column. Evaluation of chromatographic performance revealed excellent intraday and interday reproducibility (>99%), resolution (>2.23), selectivity (>1.12), peak symmetry (1.24-1.42) while presenting low limits of detection (<0.40 mg L(-1)) and quantification (<1.34 mg L(-1)). The robustness of the method was calculated according to the concentration/dilution of the sample and the injection volume. Several combinations of methanol and ethanol with water as sample solvents were evaluated and the best chromatographic results and extraction rate were obtained using 100% methanol. Finally, the developed method was validated with different extracts of turmeric rhizome and products that use turmeric in their formulation.