OFF-LINE SUPERCRITICAL-FLUID EXTRACTION - HIGH-RESOLUTION GAS-CHROMATOGRAPHY APPLIED TO THE STUDY OF MORACEAE SPECIES

Supercritical fluid extraction with CO2, Performed in a home-made system, of rhizomes of Dorstenia bryoniifolia Mart. ex Miq. (Moraceae) and of bark roots of Brosimum gaudichaudii Trecul (Moraceae) afforded crude extracts that were analysed by high resolution gas chromatography (HRGC). The D. bryoniifolia extract contained, besides the previously reported pimpinelin and isobergapten, the furocoumarins psoralen, bergapten, isopimpinelin and the triterpenes alpha- and beta-amyrin and the acetate of the latter. The B. gaudichaudii extract contained a number of terpenoids as well as the previously reported psoralen and bergapten. Supercritical fluid extraction gave extracts qualitatively similar to those obtained by Soxhlet extraction with hexane and, together with off-line HRGC, was shown to be a fast and accurate technique to be used in rapid phytochemical examination.

Extraction and exchange behavior of metal species in therapeutically applied peat

The binding and availability of metals (Al, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Zn) in therapeutically applied peat (GroBes Gifhorner Moor, Sassenburg/North Germany) was characterized by means of a versatile extraction approach. Aqueous extracts of peat were obtained by a standardized batch equilibrium procedure using high-purity water (pH 4.5 and 5.0), 0.01 mol l(-1) calcium chloride solution, 0.0 1 mol l(-1) ethylenediaminetetraacetic acid (EDTA) and 0.01 mol l(-1) diethylenetriarnine pentaacetic acid (DTPA) solution as metal extractants. In addition, the availability of peat-bound metal species was kinetically studied by collecting aliquots of extracts after different periods of extraction time (5, 10, 15, 30, 60 and 120 min). Metal determinations were performed by atomic spectrometry methods (AAS, ICP-OES) and dissolved organic matter (DOM) was characterized by UV/Vis measurements at 254 and 436 nm, respectively. of the extractants studied Ca, Mg and Mn were the most available metals, in contrast to peat-bound Fe and Al. The relative standard deviation s(r) of the developed extraction procedures was mostly in the range of 4 to 20%, depending on the metal and its concentration in peat. A pH increase favored the extraction of metals and DOM from peat revealing complex extraction kinetics. Moreover, a competitive exchange between peat-bound metal species and added Cu(II) ions showed that > 100 mg of Cu(II) per 50 g wet peat was necessary to exchange the maximum of bound metals (e.g. 21.8% of Al, 3.9% of Fe, 79.0% of Mn, 81.9% of Sr, related to their total content). (C) 2002 Elsevier B.V. B.V. All rights reserved.

Lignin from sugar cane bagasse: Extraction, fabrication of nanostructured films, and application

Four lignin samples were extracted from sugar cane bagasse using four different alcohols (methanol, ethanol, n-propanol, and 1-butanol) via the organosolv-CO2 supercritical pulping process. Langmuir films were characterized by surface pressure vs mean molecular area (Pi-A) isotherms to exploit information at the molecular level carrying out stability tests, cycles of compression/expansion (hysteresis), subphase temperature variations, and metallic ions dissolved into the water subphase at different concentrations. Briefly, it was observed that these lignins are relatively stable on the water surface when compared to those obtained via different extraction processes. Besides, the Pi-A isotherms are shifted to smaller molecular areas at higher subphase temperatures and to larger molecular areas when the metallic ions are dissolved into the subphase. The results are related to the formation of stable aggregates (domains) onto the water subphase by these lignins, as shown in the Pi-A isotherms. It was found as well that the most stable lignin monolayer onto the water subphase is that extracted with 1-butanol. Homogeneous Langmuir-Blodgett (LB) films of this lignin could be produced as confirmed by UV-vis absorption spectroscopy and the cumulative transfer parameter. In addition, FTIR analysis showed that this lignin LB film is structured in a way that the phenyl groups are organized preferentially parallel to the substrate surface. Further, these LB films were deposited onto gold interdigitated electrodes and ITO and applied in studies involving the detection of Cd+2 ions in aqueous solutions at low concentration levels throughimpedance spectroscopy and electrochemical measurements. FTIR spectroscopy was carried out before and after soaking the thin films into Cd+2 aqueous solutions, revealing a possible physical interaction between the lignin phenyl groups and the heavy metal ions. The importance of using nanostructured systems is demonstrated as well by comparing both LB and cast films.

Solid-phase extraction of sugar cane soot extract for analysis by gas chromatography with flame ionisation and mass spectrometric detection

The incomplete combustion of biomass is one of the most important sources of emissions of organic compounds into the atmosphere, like polycyclic aromatic hydrocarbons (PAHs) which show genotoxic activity. Since environmental samples generally contain interferents and trace amounts of PAHs of interest, concentration and clean-up procedures are usually required prior to the final chromatographic analysis. This paper discusses the performance of Sep-Pak cartridges (silica gel and RP18) on clean-up of sugar cane soot extract. The best results were obtained with a silica Sep-Pak cartridge. The recoveries ranged from 79% (benzo[b]fluoranthene) to 113% (benzo[e]pyrene). (C) 2000 Elsevier B.V. B.V. All rights reserved.

Optimisation of conditions for the extraction of casearins from Casearia sylvestris using response surface methodology

Optimal conditions for the extraction of casearins from Casearia sylvestris were determined using response surface methodology. The maceration and sonication extraction techniques were performed using a 3 x 3 x 3 full factorial design including three acidity conditions, three solvents of different polarities and three extraction times. The yields and selectivities of the extraction of casearins were significantly influenced by acidity conditions. Taking into account all variables tested, the optimal conditions for maceration extraction were estimated to involve treatment with dichloromethane saturated with ammonium hydroxide for 26 h. Similar yields and selectivities for casearins were determined for sonication extraction using the same solvent but for the much shorter time of I h. The best results for stabilisation of the fresh plant material were obtained using leaves that had been oven dried at 40 degrees C for 48 h. Copyright (c) 2006 John Wiley & Sons, Ltd.

Panoramic evaluation of mesiodistal axial inclinations of maxillary anterior teeth in orthodontically treated subjects

The objectives of this study were to evaluate, through panoramic radiographs, the mesiodistal axial inclinations of the maxillary anterior teeth at the beginning and end of nonextraction orthodontic treatment, and to compare the results with the mesiodistal axial inclinations of a control sample with normal (acceptable) occlusions. Methods: the experimental sample consisted of 40 white patients (20 male, 20 female; mean age, 14 years) with Class I maloccusions who were treated orthodontically with a standard edgewise (not preadjusted) technique without extractions. The mean treatment period was 1.6 years. The control sample comprised 42 white subjects (14 male, 28 female; age range, 12-17 years) with untreated normal (acceptable) occlusions. Panoramic radiographs were taken of the patients at the beginning (T1) and end (T2) of treatment. The mean values of the mesiodistal axial inclination at T1 were compared with the mean values at T2, and both were compared with the mesiodistal axial inclinations of the control sample. Results- the mesiodistal axial inclinations of the maxillary anterior teeth of the experimental group at T1 were different from those of the control group for 50% of the evaluated teeth. In contrast, the inclinations at T2 were consistent with the normal anatomical configuration of the controls. Conclusions: the panoramic radiograph is an effective tool for evaluating the mesiodistal axial inclinations of maxillary anterior teeth.

Evaluation of periapical repair following retrograde filling with different root-end filling materials in dog teeth with periapical lesions

Objective. The objective of this study was to evaluate periapical repair following retrograde filling using different root-end filling materials.Study design. After induction of periapical lesions, 48 root canals from do teeth were partially filled. Endodontic surgery was performed and 3 different materials were used for root-end filling: Sealer 26, Sealapex plus zinc oxide, or mineral trioxide aggregate (NITA). No additional procedures were performed in the control group after partial filling of the root canal. After 180 days, the animals were killed, the rnaxillas and mandibles were removed, and specimens were submitted for histologic processing.Results. Histopathologic analysis revealed similar periapical repair for the groups in which Sealer 26, Sealapex plus zinc oxide, and MTA were used (P >.05). The control group showed unsatisfactory periapical repair W <.05).Conclusion. There was no difference in periapical tissue healing alter retrograde filling with the tested materials, which indicates that these 3 root-end filling materials are equally useful.

Comparative ablation rate from a Er : YAG laser on enamel and dentin of primary and permanent teeth

This study was conducted to analyze the ablation rate and micromorphological aspects of microcavities in enamel and dentin of primary and permanent teeth using a Er:YAG laser system. Micromorphological evaluation has been performed in terms of permanent teeth; however, little information about Er: YAG laser interaction with primary teeth can be found in the literature. Because children have been the most beneficiary patients with laser therapy in our offices, it is extremely necessary to compare the effects of this kind of laser system on the enamel and dentin of permanent and primary teeth. In this study, we used eleven intact primary anterior exfoliated teeth and six extracted permanent molar teeth. We used a commercial laser system: a Er: YAG Twin Light laser system (Fotona Medical Lasers, Slovenia) at 2940 nm, changing average energy levels per pulse ( 100, 200, 300, and 400 mJ) producing 48 microcavities in enamel and dentin of primary and permanent teeth. Primary teeth are more easily ablated than are permanent teeth, when related to enamel or dentin. However, while this laser system is capable of slowly revealing the enamel's microstructure, in dentin only the lowest laser energies permit this kind of observation, more easily decomposing the original tissue aspect, when related to primary or permanent teeth. Statistically, the only different factor at the 5% level was an energy per pulse of 400 mJ, confirming the results found in SEM. Our results showed that dentin in both primary and permanent teeth is less resistant to Er: YAG laser ablation; this fact is easily observed under SEM observation and through the ablation rate evaluation.

Anatomoradiographic description of the teeth of pacas bred in captivity (Agouti paca, Linnaeus, 1766)

Two newborn males, two adult males 9 and 72 months old, one newborn female and two adult females of 30 and 54 months old pacas were used. Animals were radiographed on lateral recumbency, teeth were extracted and the vestibulolingual and mesiodistal lengths were achieved at the occlusal surface, besides the longitudinal length. The lower incisors presented greater length in relation to the other ones and sinuous shape; the upper incisors, relatively smaller, are practically straight. There is no canine tooth, and after a great diastema there is one premolar and three molars in each hemiarcade. In adult pacas, the enamel of incisors presents yellowish colour, mainly in the labial surface; in the premolars and molars, the enamel is present as internal sheets disposed nearly in a parallel way and in vestibulolingual direction, through practically all the dental length, which provides several joined teeth aspect.