Construction of a supercritical fluid extraction (SFE) equipment: validation using annatto and fennel and extract analysis by thin layer chromatography coupled to image

Abstract The present work describes setting up a laboratory unit for supercritical fluid extraction. In addition to its construction, a survey of cost was done to compare the cost of the homemade unit with that of commercial units. The equipment was validated using an extraction of annatto seeds’ oil, and the extraction and fractionation of fennel oil were used to validate the two separators; for both systems, the solvent was carbon dioxide. The chemical profiles of annatto and fennel extracts were assessed using thin layer chromatography; the images of the chromatographic plates were processed using the free ImageJ software. The cost survey showed that the homemade equipment has a very low cost (~US$ 16,000) compared to commercial equipment. The extraction curves of annatto were similar to those obtained in the literature (yield of 3.8% oil). The separators were validated, producing both a 2.5% fraction of fennel seed extract rich in essential oils and another extract fraction composed mainly of oleoresins. The ImageJ software proved to be a low-cost tool for obtaining an initial evaluation of the chemical profile of the extracts.

Supercritical fluid extraction from fennel (Foeniculum vulgare): global yield, composition and kinetic data

Supercritical fluid extraction (SFE) from solids has proven to be technically feasible for almost any system; nonetheless, its economical viability has been proven for a restricted number of systems. A common practice is to compare the cost of manufacturing of vegetable extracts by a variety of techniques without deeply considering the huge differences in composition and functional properties among the various types of extracts obtained; under this circumstance, the cost of manufacturing do not favor SFE. Additionally, the influence of external parameters such as the agronomic conditions and the SFE system geometry are not considered. In the present work, these factors were studied for the system fennel seeds + CO2. The effects of the harvesting season and the degree of maturation on the global yields for the system fennel seeds + CO2 were analyzed at 300 bar and 40 degrees C. The effects of the pressure on the global yields were determined for the temperatures of 30 and 40 degrees C. Kinetics experiments were done for various ratios of bed height to bed diameter. Fennel extracts were also obtained by hydrodistillation and low-pressure solvent extraction. The chemical composition of the fennel extracts were determined by gas chromatography. The SFE maximum global yield (12.5%, dry basis) was obtained with dry harvested fennel seeds. Anethole and fenchone were the major constituents of the extract; the following fat acids palmitic (C16H32O2), palmitoleic stearic (C18H36O2), oleic (C18H34O2), linoleic (C18H32O2) and linolenic (C18H30O2) were also detected in the extracts. A relation between amounts of feed and solvent, bed height and diameter, and solvent flow rate was proposed. The models of Sovova, Goto et al. and Tan and Lion were capable of describing the mass transfer kinetics. (c) 2005 Elsevier B.V. All rights reserved.

Content of essential oil of fennel seeds in two different stages of development

This experiment was carried out at Plant Production Sector, Agronomical Science College-Botucatu, S.P., Brazil, in March, 2000. The aim of this assay was to determine the yield of essential oil of fennel (Foeniculum vulgare Miller) in different stages of development. Essential oils were prepared by hydrodistillation from the seeds using of Clevenger apparatus. The water utilized for the extraction of essential oil was sufficient to cover 100 g of seeds and the mixture was distilled for three hours. The volume of essential oil in the graduated side -arm of Clevenger apparatus was observed. There were no significative difference statistic was observed (Tukey 5%) in percentage (v/m) of oil content, based on dry weight of green seeds compared with dry weight of mature seeds, when they were harvested in two different stages of development. There was significative difference statistic between data obtained of humidity content of green seeds when these were compared with mature seeds. These results shows that others specifics studies about adaptation of fennel in tropical conditions are necessary, because the obtained data were different of data described on literature.

The biology and thermal requirements of the fennel aphid Hyadaphis foeniculi (Passerini) (Hemiptera: Aphididae)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Temperature-dependent fecundity and life table of the fennel aphid hyadaphis foeniculi (passerini) (hemiptera: aphididae)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Estimating the development of the fennel aphid, Hyadaphis foeniculi (Passerini) (Hemiptera: Aphiididae), using non-linear models

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Cottage cheeses functionalized with fennel and chamomile extracts: comparative performance between free and microencapsulated forms

Globally, there is a trend for healthy food products, preferably incorporating natural bioactive ingredients, replacing synthetic additives. From previous screening studies, extracts of Foeniculum vulgare Mill. (fennel) and Matricaria recutita L. (chamomile) maintained nutritional properties and improved the antioxidant activity of cottage cheese. Nevertheless, this effect was limited to 7 days. Accordingly, aqueous extracts of these plants were microencapsulated in alginate and incorporated into cottage cheese to achieve an extended bioactivity. Plain cottage cheese, and cheese functionalized by direct addition of free decoctions, were prepared and compared. Independently of plant species, "functionalization type" factor did not show a significant effect on the nutritional parameters, as also confirmed in the linear discriminant analysis, where these parameters were not selected as discriminating variables. Furthermore, samples functionalized with microencapsulated extracts showed higher antioxidant activity after the 7th day, thereby demonstrating that the main purpose of this experimental work was achieved.

Antioxidant activity and phenolic composition of herbal infusions consumed in Brazil

Processed tea and herbal infusions were Studied for their phenol content, antioxidant activity and main flavonoids. Total phenolics were determined by Folin-Ciocalteu method and ranged from N.D. to 46.46 +/- 0.44 mg/g GAE. Flavonoids were investigated by HPLC, and myricetin, quercetin, kaempferol were identified in black, green, and chamomile tea. Antioxidant activity was evaluated using two methods: DPPH and beta-carotene bleaching test (BCB). Using the BCB, the highest activities were found for infusions of black tea, mate, lemongrass, chamomile, and fennel; whereas fresh herbal infusions presented the lowest activities. Using the DPPH method, fresh herbal infusions presented the highest activities. Processed leaves with the lowest IC50 values were green and black tea (147.63 and 288.60 mu g/mL, respectively). The results of this research show that the infusions studied are good Source of compounds presenting antioxidant activity in vitro.

Mathematical modelling of supercritical CO2 extraction of volatile oils from aromatic plants

The modelling of the experimental data of the extraction of the volatile oil from six aromatic plants (coriander, fennel, savoury, winter savoury, cotton lavender and thyme) was performed using five mathematical models, based on differential mass balances. In all cases the extraction was internal diffusion controlled and the internal mass transfer coefficienty (k(s)) have been found to change with pressure, temperature and particle size. For fennel, savoury and cotton lavender, the external mass transfer and the equilibrium phase also influenced the second extraction period, since k(s) changed with the tested flow rates. In general, the axial dispersion coefficient could be neglected for the conditions studied, since Peclet numbers were high. On the other hand, the solute-matrix interaction had to be considered in order to ensure a satisfactory description of the experimental data.

Extraction of volatile oil from aromatic plants with supercritical carbon dioxide: experiments and modeling

An overview of the studies carried out in our laboratories on supercritical fluid extraction (SFE) of volatile oils from seven aromatic plants: pennyroyal (Mentha pulegium L.), fennel seeds (Foeniculum vulgare Mill.), coriander (Coriandrum sativum L.), savory (Satureja fruticosa Beguinot), winter savory (Satureja montana L.), cotton lavender (Santolina chamaecyparisus) and thyme (Thymus vulgaris), is presented. A flow apparatus with a 1 L extractor and two 0.27 L separators was built to perform studies at temperatures ranging from 298 to 353 K and pressures up to 30.0 MPa. The best compromise between yield and composition compared with hydrodistillation (HD) was achieved selecting the optimum experimental conditions of extraction and fractionation. The major differences between HD and SFE oils is the presence of a small percentage of cuticular waxes and the relative amount of thymoquinone, an oxygenated monoterpene with important biological properties, which is present in the oils from thyme and winter savory. On the other hand, the modeling of our data on supercritical extraction of volatile oil from pennyroyal is discussed using Sovova's models. These models have been applied successfully to the other volatile oil extractions. Furthermore, other experimental studies involving supercritical CO2 carried out in our laboratories are also mentioned.

Extra̧ão de Macro e Micronutrientes Pela Parte Aérea de Erva-Doce EM Fuņão de Calagem e Aduba̧ão com Esterco de Cama de Frango

A greenhouse experiment was conducted in the Soil Science Department of the Botucatu College of Agricultural Sciences (UNESP), Brazil, using a Dark Red Latosol in 25 L pots. The soil was limed to 50 and 70% of base saturation; and doses 0, 10, 20, 30 and 40 t ha-1 of chicken manure were applied, in December of 1999. The experimental design was completely randomized blocks with a factorial arrangement 5x2, 10 treatments and three replications. This work was carried to evaluate leaf number, height plants, fresh and dry weight by aerial part of sweet fennel, and macronutrients and micronutrients removal. The organic fertilization affected the accumulation of N, P, K, S, B and Mn; liming affected the nutrient uptake, except for the Ca, Mg, S and Fe; the interaction of factors affected K, Mg and Mn.

Antimicrobial activity of the essential oils of some spice herbs

Essential oils were obtained from fennel seeds, dill, cumin and coriander. Their antimicrobial activity was tested on isolated clinical specimens of patients treated at the University Hospital of the School of Medicine of Botucatu, SP, UNESP. Microorganisms were grown in BHI (Brain Heart Infusion/Oxoid) at 37oC/18 hours and resuspended in 0,5 Mac Farland's Standard (1,5 x 108 CFU/mL). The diffusion method was performed, putting 10 μl of the essential oils on paper disks (6mm of diameter) (Blank Disks/CECON) at 37oC/24 hours. After this period, the disks were put on plates containing Mueller Hinton Agar (Oxoid) and inoculated with the microorganisms. After 48 hours at 37oC, inhibitory zones were measured (mm) for the respective oils and strains. The essential oil from Anethum graveolens showed antimicrobial activity against Staphylococcus aureus (inhibitory zone=18 mm), Salmonella sp. (=11 mm) and E. coli (10 mm). The Cuminum cyminum essential oil was effective against E. coli, P. aeruginosa and Salmonella sp. and their inhibitory zones were 18, 10 and 23 mm, respectively. Coriandrum sativum oil was active only against Salmonella sp. (18 mm) and Foeniculum vulgare inhibited only E. coli (9 mm).

Extratos vegetais e produtos naturais com potencial de uso no controle de Tetranychus urticae Koch (Acari: Tetranychidae) na cultura da videira

Pós-graduação em Agronomia - FEIS

Associação de variedades de goiaba, bioinseticidas e o parasitóide Diachasmimorpha longicaudata no controle de Anastrepha fraterculus

Pós-graduação em Agronomia (Produção Vegetal) - FCAV