Comparison of GC and HPLC for quantification of organic acids in two jaboticaba (Myrciaria) fruit varieties

Gas chromatography (GC) with trimethylsilyl derivative formation was compared to high-performance liquid chromatography (HPLC) for quantification of organic acids (OAs) in two jaboticaba (Myrciaria) fruit (pulp and pericarp) varieties (Sabará and Açu Paulista). Succinic and citric acids were the major OAs found in all the samples analyzed. Besides being much more tedious, the results obtained with GC were significantly lower than HPLC (p<0.05) when the data (acids, variety, two parts and flowering days) were considered together. The presence of both acids was confirmed by gas chromatography-mass spectrometry (GC-MS).

Investigation of the occurrence of pesticide residues in rural wells and surface water following application to tobacco

In this work the exposure of wells and surface water to pesticides, commonly used for tobacco cropping, was assessed. Water consumption wells and surface water flows were sampled at different times. After a preconcentration step with solid phase extraction (SPE), the selected pesticides were determined by gas chromatography with electron capture detection (GC-ECD) or high performance liquid chromatography with diode array detection (HPLC-DAD). No pesticides were detected in the well water samples and surface water flow in the winter season. However, in the spring and summer higher concentrations of chlorpyrifos and imidacloprid were found in the water source samples. Atrazine, simazine and clomazone were also found. The occurrence of pesticides in collected water samples was related with the application to tobacco.

Chemical composition and antimicrobial activity of the essential oil from Aeolanthus suaveolens Mart. ex Spreng

The essential oils from leaves (sample A) and flowers (sample B) of Aeolanthus suaveolens Mart. ex Spreng were obtained by hydrodistillation and analyzed by GC, GC-MS, and chiral phase gas chromatography (CPGC). Six compounds have been identified from the essential oils, representing ca 94.3 and 93% of the oils corresponding to samples A and B, respectively. The major constituents of samples A and B essential oils were respectively, linalool (34.2%/34.9%), (-)-massoialactone (25.9%/17.0%) and (E)-beta-farnesene (25.4%/29.1%). The enantiomeric distribution of the monoterpene linalool was established by analysis on heptakis- (6-O-methyl-2,3-di-O-pentyl)-beta-cyclodextrin capillary column. The antimicrobial activity of the essential oil from leaves and isolated compounds was also evaluated.

Utilização do índice de retenção linear para caracterização de compostos voláteis em café solúvel utilizando GC-MS e coluna HP-Innowax

Gas chromatography coupled with mass spectrometry (GC-MS) is widely used for the characterization of volatile compounds. However, due to the complexity of the soluble coffee matrix, a complete identification of the components should not be based on mass spectra interpretation only. The linear index of retention (LRI) is frequently used to give support to mass spectra. The aim of this work is to investigate the characterization of the volatile compounds in soluble coffee samples by GC-MS using LRI values found with a HP-INNOWAX column. The method used allows a significant increase of the reliability of identifying compounds.

Desenvolvimento e validação de método de análise de glifosato em grãos de soja

The main objective of this work is to develop an efficient procedure to determine glyphosate in soybean grains. The cleanup of the aqueous extracts was done in two steps, beginning with liquid-liquid partitioning and then solid-phase extraction with anion exchange resin. After derivatization with a mixture of trifluoroacetic anhydride (TFAA) and trifluoroethanol (TFE), quantification was done by gas chromatography coupled to mass spectrometry. The mean recovery and RSD of the spiked samples were, respectively, 80.5% and 3.1% at level 0.200 mg kg-1, 93.3% and 18.7% at level 0.500 mg kg-1 and 92% and 3.5% at level 1.000 mg kg-1. The method was linear in the working range (correlation coefficient = 0.9965).

Otimização de metodologia para derivação de desoxinivalenol através de planejamento experimental

The objective of this work was to optimize the derivatization reaction for determining deoxynivalenol (DON) by gas chromatography employing an experimental planning procedure. The factors were: temperature, reaction time, catalyst and trifluoroacetic anhydride concentration. The relative peak areas were used to evaluated the effects. The best conditions for DON derivatization were 200 µL TFAA and 18 mg sodium bicarbonate for 6 min at 74 ºC for 7 to 21 µg of DON. Under these conditions, the detection limit was 1.4 µg of DON.

Análise por cromatografia gasosa de BTEX nas emissões de motor de combustão interna alimentado com diesel e mistura diesel-biodiesel (B10)

This paper describes the procedures for analysing pollutant gases emitted by engines, such as volatile organic compounds (benzene, toluene, ethylbenzene, o-xylene, m-xylene and p-xylene) by using high resolution gas chromatography (HRGC). For IC engine burning, in a broad sense, the use of the B10 mixture reduces drastically the emissions of aromatic compounds. Especially for benzene the reduction of concentrations occurs at the level of about 24.5%. Although a concentration value below 1 µg mL-1 has been obtained, this reduction is extremely significant since benzene is a carcinogenic compound.

Perfil de ácidos graxos e avaliação da alteração em óleos de fritura

The present study had the purpose of evaluating the profile of fatty acids and the total alteration of cottonseed, sunflower and palm oils brought about during discontinued frying processes of cassava frozen chips. An increase in the percentage of saturated fatty acids and a decrease in polyunsaturated fatty acids was observed, regardless of the type of oil used. With regard to the oil's global alteration, the results showed that palm oil, the most saturated one, underwent less alteration. However, none of the oils presented total polar compound values above the limits prescribed.

Determinação da matéria-prima utilizada na produção do biodiesel adicionado ao diesel mineral através de monitoramento seletivo de íons

The selective ion monitoring acquisition mode in mass spectrometry was applied to identify, in the diesel complex matrix, the raw materials (vegetable oil and alcohol) that originate biodiesel. Biodiesel samples obtained from babassu, castor, palm and soybean vegetable oils and pure fatty acid methyl and ethyl esters were used to develop this method, using specific fragments in mass spectrometry and the "window system" in gas chromatography. The commercial Brazilian B2 samples were found to be produced with soybean oil, transesterified with methanol.

Métodos de amostragem e análise para compostos reduzidos de enxofre atmosférico

This work presents a review of sampling and analytical methods that can be applied to atmospheric traces of reduced sulphur compounds (RSC) in the atmosphere. Sampling methodology involving discontinuous methods with preconcentration is mostly used. For the most part, adsorption on solids and cryogenic capture are applied as a procedure. The analysis of these compounds has been done mainly by gas chromatography with FPD, fluorescence and spectrophotometry. Advantages and disadvantages of the methodologies are also mentioned in this paper, aiming to guide the reader towards the most appropriate choice of a sampling and analytical method for RSCs.

Efeito do 1-metilciclopropeno sobre a emissão dos ésteres voláteis de bananas ao longo do amadurecimento

Fresh green bananas (Musa sp., subgroup Prata) were treated with a dose of only 90 ηg g-1 of 1-MCP for 13 hours and the evolution of the volatile compounds along the ripeness was studied. A method to quantify the emission of esters was developed by cryogenic headspace and gas chromatography. Esters of acetate, butyrate, isobutyrate and isovalerate were found as major compounds. The application of the 1-MCP for 13 hours delayed the appearance of the coloration 8 of the peel for 3 days and decreased quantitatively in about 46% the total production of esters in the banana until the 15° day of harvested.

Desenvolvimento de metodologia analítica para determinação de colesterol em ração para ruminantes através de planejamento experimental fatorial

A chromatographic method was developed for cholesterol determination in feed for ruminants using response surface methodology. Among the five approaches of sample preparation methods tested, the saponification of the sample without heating presented less interference in the gas chromatography. The method presented a relative standard deviation (RSD) of 4.3%, recoveries between 84 and 87% and detection limit of 0.001 mg of cholesterol per g of feed.

Determinação de isotiocianato de benzila em Carica papaya utilizando cromatografia gasosa com detectores seletivos

In the present work, a method was developed and validated for the quantification of benzyl isothiocyanate (BITC) in the fruits of Carica papaya. The quantification of this compound was carried out by gas chromatography (GC) with selective detectors - nitrogen phosphorus detector (NPD) and flame photometric detector (FPD). The performance of these detectors showed a higher sensitivity of the NPD with a broader linear range of detection. The LOD/LOQ were 0.038/0.100 µg/mL for NPD and 5.78/19.29 µg/mL for FPD. The recovery of the method for BITC was 90,64%. An average value of BITC concentration in all the analyzed samples was 16,23 µg BITC/g.

Volatile compounds in the thermoplastic extrusion of bovine rumen

The volatile compounds of raw and extruded bovine rumen, extracted by dynamic headspace, were separated by gas chromatography and analyzed by GC-MS. Raw and extruded materials presented thirty-two volatile compounds. The following compounds were identified in raw bovine rumen: heptane, 1-heptene, 4-methyl-2-pentanone, toluene, hexanal, ethyl butyrate, o-xylene, m-xylene, p-xylene, heptanal, limonene, nonanal, dodecane, tridecane, tetradecane, pentadecane, hexadecane, heptadecane and octadecane. The following compounds were identified in the extruded material: 1-heptene, 2,4-dimethylhexane, toluene, limonene, undecane, tetradecane, pentadecane, hexadecane, heptadecane, octadecane and nonadecane. Mass spectra of some unidentified compounds indicated the presence of hydrocarbons with branched chains or cyclic structure.

Determinação da relação siringila/guaiacila da lignina em madeiras de eucalipto por pirólise acoplada à cromatografia gasosa e espectrometria de massas (PI CG/EM)

The use of analytical pyrolysis combined with gas chromatography/mass spectrometry (Py-GC/MS) to determine the syringyl/guaiacyl ratio (S/G) in lignins from Eucalyptus spp woods was investigated. Sample of E. grandis and "E. urograndis" wood, with and without extractives, were subjected to pyrolysis from 300 ºC to 600 ºC. The products that results from pyrolysis were identified by mass spectrometry and the S/G ratio was determined based on the areas of the peaks corresponding to the guaiacyl and syringyl derivatives. The best S/G estimation is achieved when pyrolysis is carried out at 550 ºC. Extractives and carbohydrate present in the woods do not interfere with the results.