Brazil has great energy potential for the production of biodiesel, due to its great size and variety of climates with many regions of pastures and because it is one of the greatest exporters of bovine meat of the world. Beef tallow is a potential raw material for the production of biodiesel, presenting an efficient transesterification and easy separation of phases. In this work, the transesterification of the tallow by homogeneous catalysis with a solution of methanolic of KOH was carried out by means of heating and preliminary formation of a microemulsion. In this study, the biodiesel obtained was characterized by physicochemical means of the Norms of the ANP 07/2008. Fatty acids from beef tallow were characterized by gas chromatography−mass spectrometry (GC−MS) and quantified by thermogravimetric analyses (TGA). Similar quantities of saturated and unsaturated fatty acids were observed by correlation GC−TGA. The beef tallow biodiesel obtained using a simple methodology presented a high yield (96.26%), even though the raw material had high quantities of FFA (3.6 ± 0.02%).
Rationale
Electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (ESI FT‐ICR MS) is an important analytical technique used for the elucidation of crude oil polar compounds at the molecular level, providing thousands of heteroatom compounds in a single analysis. Due to the high resolution, the complexity of data produced, and steps involved in spectra acquisition and processing, it is necessary to estimate its intermediate precision.
Methods
Intermediate precision was estimated for positive‐ and negative‐ion ionization modes (ESI(±)) using Composer® software for two Brazilian crude oil samples. The analytical parameters evaluated were the class distribution histogram, the double bond equivalent (DBE) distribution, and the DBE versus carbon number. The statistical parameters used to study the intermediate precision were calculated from the average, standard deviation, confidence interval (significance level at 5%), coefficient of variation (CV), intermediate precision limit (ISO 5725), and principal component analysis (PCA).
Results
Two crude oil samples (A and B) were analyzed, in triplicate, for seven consecutive days by ESI(±) FT‐ICR MS. The assigned class limit by ESI(+) for crude oil A was 0.42% (O2S[H] class) and for crude oil B was 0.04% (N2O2S[H] class). The assigned DBE intensity limits for the two crude oils were 0.04% for ESI(+) and 0.013% for ESI(−). The PCA for ESI(−) and ESI(+) modes presented better precision for crude oils B and A, respectively.
Conclusions
The most abundant classes and DBE of the majority class (i.e., with the highest intensity) are the parameters produced from the Composer® software that had the highest precision and can be used to estimate crude oil properties. The DBE values presented lower intermediate precision limit values (0.04%) than the assigned class values (0.4%). According to CV and PCA, ESI(+) was more precise for crude oil A (83% precision) and ESI(−) for crude oil B (84% precision).
Mimosa caesalpiniifolia is a native plant of the Brazilian northeast, and few studies have investigated its chemical composition and biological significance. This work describes the identification of the first chemical constituents in the ethanolic extract and fractions of M. caesalpiniifolia stem bark based on NMR, GC-qMS and HRMS analyses, as well as an assessment of their cytotoxic activity. GC-qMS analysis showed fatty acid derivatives, triterpenes and steroid substances and confirmed the identity of the chemical compounds isolated from the hexane fraction. Metabolite biodiversity in M. caesalpiniifolia stem bark revealed the differentiated accumulation of pentacyclic triterpenic acids, with a high content of betulinic acid and minor amounts of 3-oxo and 3β-acetoxy derivatives.
OPEN ACCESSMolecules 2015, 20
4205Bioactive analysis based on total phenolic and flavonoid content showed a high amount of these compounds in the ethanolic extract, and ESI-(−)-LTQ-Orbitrap-MS identified caffeoyl hexose at high intensity, as well as the presence of phenolic acids and flavonoids. Furthermore, the evaluation of the ethanolic extract and fractions, including betulinic acid, against colon (HCT-116), ovarian (OVCAR-8) and glioblastoma (SF-295) tumour cell lines showed that the crude extract, hexane and dichloromethane fractions possessed moderate to high inhibitory activity, which may be related to the abundance of betulinic acid. The phytochemical and biological study of M. caesalpiniifolia stem bark thus revealed a new alternative source of antitumour compounds, possibly made effective by the presence of betulinic acid and by chemical co-synergism with other compounds.
Context: 'Carnauba' wax is a natural product obtained from the processing of the powder exuded from Copernicia prunifera (Miller) H. E. Moore (Arecaceae). This material is widely used in the Brazilian folk medicine, including the treatment of rheumatism and syphilis. Objective: To investigate the antiprotozoal activity of hexane and EtOH extracts from the 'carnauba' wax as well as from the isolated compounds from the bioactive extracts. Material and methods: Two different samples of 'carnauba' (C. prunifera) waxes -types 1 and 4 -were individually extracted using hexane (EH) and EtOH (EE). Aliquots of hexane (type 1 -EH-1 and EH-4) and EtOH (type 4 -EE-1 and EE-4) extracts were tested against promastigote (2-200 lg/mL in DMSO during 48 h at 24 C) and amastigote (3-150 lg/mL in DMSO during 120 h at 37 C) forms of Leishmania infantum as well as against trypomastigote (3-150 lg/mL in DMSO during 24 h at 37 C) forms of Trypanosoma cruzi. Bioactive extracts EH-1 and EE-4 were subjected to a bioactivity-guided fractionation to afford three dammarane-type triterpenoids (1-3). The in vitro antiprotozoal activities of the obtained compounds were evaluated as described above. Additionally, the cytotoxicity activity of compounds 1-3 against mammalian conjunctive cells (NCTC -2-200 lg/mL in DMSO during 48 h at 37 C) was determined. Results: From the bioactive hexane and EtOH extracts from the 'carnauba' (C. prunifera) wax, were isolated three dammarane-type triterpenoids: (24R Ã )-methyldammar-25-ene-3b,20-diol (carnaubadiol, 1), (24R Ã )-methyldammara-20,25-dien-3-one (2) and (24R Ã )-methyldammara-20,25-dien-3a-ol (3). These compounds were identified based on the analysis of NMR and MS spectroscopic data. Compounds 1-3 were effective against the intracellular amastigotes of L. infantum, with IC 50 values ranging from 8 to 52 lM, while compounds 1 and 3 displayed activity against trypomastigote forms of T. cruzi with IC 50 values of 15 and 35 lM, respectively. The mammalian cytotoxicity assay demonstrated no damage to NCTC conjunctive cells up to 200 lM, except for compound 1, which demonstrated a CC 50 value of 34 lM. Conclusion: Based on the results, it was possible to conclude that the detected antiprotozoal bioactivity of 'carnauba' (C. prunifera) wax extracts could be related to the presence of the natural dammarane triterpenoid derivatives. The results suggested that these compounds could be used as promising scaffolds for drug design studies for leishmaniasis and Chagas disease.
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