Electrospray Ionization Mass Spectrometry Fingerprinting Of Propolis.

Crude ethanolic extracts of propolis, a natural resin, have been directly analysed using electrospray ionization mass (ESI-MS) and tandem mass spectrometry (ESI-MS/MS) in the negative ion mode. European, North American and African samples have been analyzed, but emphasis has been given to Brazilian propolis which displays diverse and region-dependent chemical composition. ESI-MS provides characteristic fingerprint mass spectra, with propolis samples being divided into well-defined groups directly related to their geographical origins. Chemometric multivariate analysis statistically demonstrates the reliability of the ESI-MS fingerprinting method for propolis. On-line ESI-MS/MS tandem mass spectrometry of characteristic [M - H](-) ion markers provides an additional dimension of fingerprinting selectivity, while structurally characterizing the ESI-MS marker components of propolis. By comparison with standards, eight such markers have been identified: para-coumaric acid, 3-methoxy-4-hydroxycinnamaldehyde, 2,2-dimethyl-6-carboxyethenyl-2H-1-benzopyran, 3-prenyl-4-hydroxycinnamic acid, chrysin, pinocembrin, 3,5-diprenyl-4-hydroxycinnamic acid and dicaffeoylquinic acid. The negative mode ESI-MS fingerprinting method is capable of discerning distinct composition patterns to typify, to screen the sample origin and to reveal characteristic details of the more polar and acidic chemical components of propolis samples from different regions of the world.129739-4

Tentativas de obtenção de precursores do acido crisantemico

Orientador : Concetta KascheresDissertação (mestrado) - Universidade Estadual de Campinas, Instituto de QuimicaMestrad

Manipulação gravimetrica automatica de soluções

Orientador : Celio PasquiniTese (doutorado) - Universidade Estadual de Campinas, Instituto de QuimicaDoutorad

Instantaneous Characterization Of Vegetable Oils Via Tag And Ffa Profiles By Easy Ambient Sonic-spray Ionization Mass Spectrometry.

A fast and reliable method is presented for the analysis of vegetable oils. Easy ambient sonic-spray ionization mass spectrometry (EASI-MS) is shown to efficiently desorb and ionize the main oil constituents from an inert surface under ambient conditions and to provide comprehensive triacylglyceride (TAG) and free fatty acid (FFA) profiles detected mainly as either [TAG + Na](+) or [FFA-H](-) ions. EASI(+/-)-MS analysis is simple, easily implemented, requires just a tiny droplet of the oil and is performed without any pre-separation or chemical manipulation. It also causes no fragmentation of TAG ions hence diacylglyceride (DAG) and monoacylglyceride (MAG) profiles and contents can also be measured. The EASI(+/-)-MS profiles of TAG and FFA permit authentication and quality control and can be used, for instance, to access levels of adulteration, acidity, oxidation or hydrolysis of vegetable oils in general.135738-4

Characterization Of Vegetable Oils By Electrospray Ionization Mass Spectrometry Fingerprinting: Classification, Quality, Adulteration, And Aging.

An improved approach for the direct infusion electrospray ionization mass spectrometry (ESI-MS) analysis of vegetable oils is described. The more polar components of the oils, including the fatty acids, are simply extracted with methanol/water (1:1) solution and analyzed by direct infusion ESI-MS in both the negative and positive ion modes. This fingerprinting analysis was applied to genuine samples of olive, soybean, corn, canola, sunflower, and cottonseed oil, to admixtures of these oils, and samples of aged soybean oil. ESI-MS fingerprints in the positive ion mode of the extracts divide the oils into well-defined groups, as confirmed by principal component analysis, whereas ESI-MS fingerprints in the negative ion mode clearly differentiate olive oil from the five other refined oils. The method is also shown to detect aging and adulteration of vegetable oils.777429-3

Ambient Mass Spectrometry: Bringing Ms Into The Real World"."

Mass spectrometry has recently undergone a second contemporary revolution with the introduction of a new group of desorption/ionization (DI) techniques known collectively as ambient mass spectrometry. Performed in an open atmosphere directly on samples in their natural environments or matrices, or by using auxiliary surfaces, ambient mass spectrometry (MS) has greatly simplified and increased the speed of MS analysis. Since its debut in 2004 there has been explosive growth in the applications and variants of ambient MS, and a very comprehensive set of techniques based on different desorption and ionization mechanisms is now available. Most types of molecules with a large range of masses and polarities can be ionized with great ease and simplicity with the outstanding combination of the speed, selectivity, and sensitivity of MS detection. This review describes and compares the basis of ionization and the concepts of the most promising ambient MS techniques known to date and illustrates, via typical analytical and bioanalytical applications, how ambient MS is helping to bring MS analysis deeper than ever into the real world open atmosphere environment--to wherever MS is needed.398265-9

Instantaneous characterization of vegetable oils via TAG and FFA profiles by easy ambient sonic-spray ionization mass spectrometry

A fast and reliable method is presented for the analysis of vegetable oils. Easy ambient sonic-spray ionization mass spectrometry (EASI-MS) is shown to efficiently desorb and ionize the main oil constituents from an inert surface under ambient conditions and to provide comprehensive triacylglyceride (TAG) and free fatty acid (FFA) profiles detected mainly as either [TAG + Na]+ or [FFA − H]− ions. EASI(±)-MS analysis is simple, easily implemented, requires just a tiny droplet of the oil and is performed without any pre-separation or chemical manipulation. It also causes no fragmentation of TAG ions hence diacylglyceride (DAG) and monoacylglyceride (MAG) profiles and contents can also be measured. The EASI(±)-MS profiles of TAG and FFA permit authentication and quality control and can be used, for instance, to access levels of adulteration, acidity, oxidation or hydrolysis of vegetable oils in general1354738744CONSELHO NACIONAL DE DESENVOLVIMENTO CIENTÍFICO E TECNOLÓGICO - CNPQCOORDENAÇÃO DE APERFEIÇOAMENTO DE PESSOAL DE NÍVEL SUPERIOR - CAPESFINANCIADORA DE ESTUDOS E PROJETOS - FINEPFUNDAÇÃO DE AMPARO À PESQUISA DO ESTADO DE SÃO PAULO - FAPESPSem informaçãoSem informaçãoSem informaçãoSem informaçã

Factors that influence the yield and composition of Brazilian propolis extracts

During the extraction of propolis several factors were varied in order to determine how they affected the yield and phenolic composition of the obtained extracts. Six samples of green propolis from the Southeastern region of Brazil were tested. The results indicate that the highest yield of propolis extracts obtained by maceration, which also had the greatest number of components, were those using 70% (v/v) ethanol or more as a solvent. The Soxhlet extraction procedure resulted in even higher yields. No differences were observed between extracts macerated in the presence or absence of light. An increase in yield was observed between extracts macerated for 10 and 30 days although the phenolic content did not vary significantly. The total phenolic content of all extracts varied from 6.41 to 15.24 % but no direct correlation could be found between any of the factors tested

Characterization Of Must And Wine Of Six Varieties Of Grapes By Direct Infusion Electrospray Ionization Mass Spectrometry.

Samples of must derived from six different varieties of grapes taken during the fermentation process, as well as the respective wine samples directly after the end of the malolactic fermentation, were analyzed by direct infusion negative ion mode electrospray ionization mass spectrometry (ESI-MS). Diagnostic ions for must were different from those of wine samples, although small variations for each of the grape varieties were also detected. The addition of unfermented must or sugar to wine could also be clearly detected. The spectra were acquired in a few minutes per sample, indicating that ESI-MS can be used for high-throughput analysis of samples and should prove useful for quality control during and after the fermentation process.41185-9