Temperature High Resolution Gas Chromatography Research Articles

Activity of Brazilian and Bulgarian propolis against different species of Leishmania

Extracts of propolis samples collected in Brazil and Bulgaria were assayed against four Leishmania species--Leishmania amazonensis, L. braziliensis, L. chagasi from the New World, and L. major from the Old World--associated to different clinical forms of leishmaniasis. The composition of the extracts has been previously characterized by high temperature high resolution gas chromatography coupled to mass spectrometry. Considering the chemical differences among the extracts and the behavior of the parasites, it was observed significant differences in the leishmanicidal activities with IC50/1 day values in the range of 2.8 to 229.3 microg/ml . An overall analysis showed that for all the species evaluated, Bulgarian extracts were more active than the ethanol Brazilian extract. As the assayed propolis extracts have their chemical composition determined it merits further investigation the effect of individual components or their combinations on each Leishmania species.

Two decades of high temperature gas chromatography (1983–2003): what's next?

The evolution of the concept of High Temperature High Resolution Gas Chromatography (HT-HRGC) is presented together with examples highlighting its potentialities. The range of molecular weight and number of functional groups present in the molecules eluting at higher temperature, far exceeds (Kovats Indices of 120) the usual HRGC range for analytes (Kovats Indices of 40–45). With usual column lengths and film thickness, this will already extend the range of analytes by 400 Da. Short, thin film columns would acme another 500 Da to the molecular weight window traditionally dealt with by HRGC. This range (∼700–1500 Da) can be surpassed by molecules presenting peculiar structures, the ceiling being ∼5000 Da. It is currently tackled only for peptides, oligosaccharides and a few polymers, by conventional analytical techniques. However, higher molecular weight analogues of all other organic species and yet unknown carbon skeletons have been neglected because this range was only poorly accessible to usual analytical techniques dealing with complex mistures.

Chemical composition and microbicidal activity of extracts from Brazilian and Bulgarian propolis.

The chemical composition of ethanol extracts from a Brazilian (Et-Bra) and a Bulgarian (Et-Blg) propolis, and their activity against the protozoan Trypanosoma cruzi, several fungi and bacteria species were determined. The chemical composition was determined by high temperature high resolution gas chromatography coupled to mass spectrometry. Microbiological activity was assayed in vitro against T. cruzi, Candida albicans, Sporothrix schenckii, Paracoccidioides brasiliensis, Neisseria meningitidis, Streptococcus pneumoniae and Staphylococcus aureus. Et-Bra and Et-Blg, although with totally distinct compositions, were active against T. cruzi and the three species of fungi. Et-Blg was more effective than Et-Bra against bacteria, particularly N. meningitidis and Strep. pneumoniae. Although with different classes of components, both propolis extracts showed microbicidal activity. For the bactericidal activity it was possible to establish a positive correlation with the high content of flavonoids of the Bulgarian extract.

Flavonoids and trypanocidal activity of Bulgarian propolis

Acetone and ethanol extracts of two Bulgarian propolis samples ( Bur and Lov) were investigated by high temperature high resolution gas chromatography coupled to mass spectrometry (HT-HRGC-MS), and their activity against Trypanosoma cruzi was evaluated. The ethanol extracts— Et- Bur and Et- Lov—showed similar composition, with a high content of flavonoids, and strong inhibitory activity against T. cruzi proliferative epimastigotes, which were more susceptible than trypomastigotes. In the presence of blood, the activity of Et- Bur or Et- Lov against trypomastigotes was similar to that of the standard drug, crystal violet. Both extracts also showed similar and significant activity against Staphylococcus aureus and Candida albicans, while being inactive against Escherichia coli. The acetone extract, Ket- Bur, was more active than Et- Bur against both forms of T. cruzi.

Chemical composition of Tipuana tipu, a source for tropical honey bee products.

Tipuana tipu (Benth.) Kuntze is a tree from the leguminosae family (Papilionoideae) indigenous in Argentina and extensively used in urbanism, mainly in Southern Brazil. The epicuticular waxes of leaves and branch, and flower surface were studied by high temperature high resolution gas chromatography. Several compounds were characterized, among which the aliphatic alcohols were predominant in branch, leaves and receptacle. Alkanes were predominant only in the petals and the aliphatic acids were predominant in stamen. In branches and leaf epicuticular surfaces, six long chain wax esters series were characterized, as well as lupeol and b-amyrin hexadecanoates.

Three series of high molecular weight alkanoates found in Amazonian plants

Electron impact mass spectra were measured by high temperature high resolution gas chromatography–mass spectrometry (HT-HRGC–MS) for three homologous series of high molecular weight compounds present in the Amazonian plants Marupá ( Simaruba amara) and Brazil nut ( Bertholettia excelsa). Based on their mass spectra, the compounds were identified as three wax ester series of α-tocopherol (vitamin E), β-tocopherol and phytol (2,6,10,14-tetramethylhexadec-14-en-16-ol). The interpretations are supported by high resolution mass spectrometry and GC retention indices of authentic standards.

Lupeol alkanoates in Brazilian propolis.

High temperature high resolution gas chromatography coupled to mass spectrometry (HT-HRGC-MS) isa powerful analytical tool. In this work we applied this technique to the study of crude extracts of propolis collected near the city of Uberlândia-Minas Gerais State. Eucalyptus trees and native plants from "cerrado" (savannah) were the material sources disposable for the Apis mellifera bees. A lot of known propolis constituents were identified, however, several high molecular weight compounds including lupeol alkanoates were identified for first time in propolis.

Further lipophilic flavonols in Vellozia graminifolia (Velloziaceae) by high temperature gas chromatography: quick detection of new compounds.

Further lipophilic flavonols present in Vellozia graminifolia have been determined by high temperature high resolution gas chromatography (HTHRGC) and by HTHRGC coupled to mass spectrometry (MS). These methods resulted in the detection, isolation and characterisation of a monoisoprenylated flavonol 3,5,4'-trimethoxy-3'-hydroxy-6,7-(2"-isopropenyldihydrofurano)flavone from the ethyl acetate extract of the whole plant. The structural elucidation was accomplished using spectral data, including two-dimensional NMR, and on chemical transformations. Both HTHRGC and HTHRGC-MS were shown to be alternative and extremely valuable methods for the quick screening of flavonoid aglycones and other chemical metabolites of the Velloziaceae.

Estado da arte da cromatografia gasosa de alta resolução e alta temperatura

The developments in stationary phase synthesis and capillary column technology, have opened new perspectives in analysis of high molecular mass compounds (³600 daltons) and thermolabile organic compounds by High Temperature High Resolution Gas Chromatography (HT-HRGC). HT-HRGC is a new analytical borderline and its application to the analysis of high molecular mass compounds is still in its infancy. The apolar and medium polar gum phases can now be operated at temperatures up to 400-480oC, being used for the analysis of n-alcanes up to C-100, lipids, oligosaccharides, industrial resins, polyglycerols, cyclodextrins, porphyrins, etc. This technique should play a leading role as a powerful tool, for many different analysis types, in multidisciplinary fields of Science.

Systematic study of high molecular weight compounds in Amazonian plants by high temperature gas chromatography-mass spectrometry.

The fractions of hexane and dichloromethane extraction from marupá (Simaruba amara) and (Bertholletia excelsa) leaves were analyzed by HT-HRGC (high temperature high resolution gas chromatography) and HT-HRGC coupled to mass spectrometry (HT-HRGC-MS). Several compounds can be characterized including unusual high molecular weight compounds.

Pentacyclic Triterpenoid Alkanoates in Propolis

A series of high molecular mass pentacyclic terpenoid wax esters (TTFAE) were characterized for the first time in hexane extracts of Brazilian propolis (Carangola, Minas Gerais State). Identification was by HT-HRGC (High Temperature High Resolution Gas Chromatography) and HT-HRGC coupled to mass spectrometry (HT-HRGC-MS).

Application of High Temperature High Resolution Gas Chromatography to Crude Extracts of Propolis

The underivatized acetone and hexane fractions from propolis samples (predominant flora Citrus spp. and Vernonia polyanthes) were analyzed by HT-HRGC (high temperature high resolution gas chromatography) and HT-HRGC coupled to mass spectrometry (HT-HRGC-MS). Several compounds, including flavonoid aglycones, phenolic acids, and high molecular weight compounds were characterized in crude extracts by HT-HRGC-MS. HT-HRGC and HT-HRGC-MS were shown to be quick and informative tools for rapid analysis of crude extracts without need for prior derivatization and purification.

Application of High Temperature High Resolution Gas Chromatography to Crude Extracts of Propolis

The underivatized acetone and hexane fractions from propolis samples (predominant flora Citrus spp. and Vernonia polyanthes) were analyzed by HT-HRGC (high temperature high resolution gas chromatography) and HT-HRGC coupled to mass spectrometry (HT-HRGC-MS). Several compounds, including flavonoid aglycones, phenolic acids, and high molecular weight compounds were characterized in crude extracts by HT-HRGC-MS. HT-HRGC and HT-HRGC-MS were shown to be quick and informative tools for rapid analysis of crude extracts without need for prior derivatization and purification.

Application of high temperature high resolution gas chromatography to paraffinic deposits in petroleum production pipelines

AbstractHTHRGC was found essential for optimizing representative preparation of high molecular weight samples and enabling fingerprinting of heavy fractions of crude oils and associated paraffinic deposits in production pipelines. Laboratory experiments aimed at simulating the process of paraffin deposition could also be easily evaluated. A comparative investigation of the performance of cold on‐column and SPI (PTV type) injectors, in conjunction with high temperature capillary columns, for analysis of high molecular weight fractions, was also conducted during the course of this work.