Search results for: SPME%20methods
Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 8

Search results for: SPME%20methods

8 Evaluation of Solid Phase Micro-extraction with Standard Testing Method for Formaldehyde Determination

Authors: Y. L. Yung, Kong Mun Lo

Abstract:

In this study, solid phase micro-extraction (SPME) was optimized to improve the sensitivity and accuracy in formaldehyde determination for plywood panels. Further work has been carried out to compare the newly developed technique with existing method which reacts formaldehyde collected in desiccators with acetyl acetone reagent (DC-AA). In SPME, formaldehyde was first derivatized with O-(2,3,4,5,6 pentafluorobenzyl)-hydroxylamine hydrochloride (PFBHA) and analysis was then performed by gas chromatography in combination with mass spectrometry (GC-MS). SPME data subjected to various wood species gave satisfactory results, with relative standard deviations (RSDs) obtained in the range of 3.1-10.3%. It was also well correlated with DC values, giving a correlation coefficient, RSQ, of 0.959. The quantitative analysis of formaldehyde by SPME was an alternative in wood industry with great potential

Keywords: Formaldehyde, GCMS, Plywood and SPME

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7 Speciation Analysis by Solid-Phase Microextraction and Application to Atrazine

Authors: K. Benhabib, X. Pierens, V-D Nguyen, G. Mimanne

Abstract:

The main hypothesis of the dynamics of solid phase microextraction (SPME) is that steady-state mass transfer is respected throughout the SPME extraction process. It considers steady-state diffusion is established in the two phases and fast exchange of the analyte at the solid phase film/water interface. An improved model is proposed in this paper to handle with the situation when the analyte (atrazine) is in contact with colloid suspensions (carboxylate latex in aqueous solution). A mathematical solution is obtained by substituting the diffusion coefficient by the mean of diffusion coefficient between analyte and carboxylate latex, and also thickness layer by the mean thickness in aqueous solution. This solution provides an equation relating the extracted amount of the analyte to the extraction a little more complicated than previous models. It also gives a better description of experimental observations. Moreover, the rate constant of analyte obtained is in satisfactory agreement with that obtained from the initial curve fitting.

Keywords: Pesticide, SPME methods, polyacrylate, steady state.

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6 Optimization and Validation for Determination of VOCs from Lime Fruit Citrus aurantifolia (Christm.) with and without California Red Scale Aonidiella aurantii (Maskell) Infested by Using HS-SPME-GC-FID/MS

Authors: K. Mohammed, M. Agarwal, J. Mewman, Y. Ren

Abstract:

An optimum technic has been developed for extracting volatile organic compounds which contribute to the aroma of lime fruit (Citrus aurantifolia). The volatile organic compounds of healthy and infested lime fruit with California red scale Aonidiella aurantii were characterized using headspace solid phase microextraction (HS-SPME) combined with gas chromatography (GC) coupled flame ionization detection (FID) and gas chromatography with mass spectrometry (GC-MS) as a very simple, efficient and nondestructive extraction method. A three-phase 50/30 μm PDV/DVB/CAR fibre was used for the extraction process. The optimal sealing and fibre exposure time for volatiles reaching equilibrium from whole lime fruit in the headspace of the chamber was 16 and 4 hours respectively. 5 min was selected as desorption time of the three-phase fibre. Herbivorous activity induces indirect plant defenses, as the emission of herbivorous-induced plant volatiles (HIPVs), which could be used by natural enemies for host location. GC-MS analysis showed qualitative differences among volatiles emitted by infested and healthy lime fruit. The GC-MS analysis allowed the initial identification of 18 compounds, with similarities higher than 85%, in accordance with the NIST mass spectral library. One of these were increased by A. aurantii infestation, D-limonene, and three were decreased, Undecane, α-Farnesene and 7-epi-α-selinene. From an applied point of view, the application of the above-mentioned VOCs may help boost the efficiency of biocontrol programs and natural enemies’ production techniques.

Keywords: Lime fruit, Citrus aurantifolia, California red scale, Aonidiella aurantii, VOCs, HS-SPME/GC-FID-MS.

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5 Optimization of the Headspace Solid-Phase Microextraction Gas Chromatography for Volatile Compounds Determination in Phytophthora Cinnamomi Rands

Authors: Rui Qiu, Giles Hardy, Dong Qu, Robert Trengove, Manjree Agarwal, YongLin Ren

Abstract:

Phytophthora cinnamomi (P. c) is a plant pathogenic oomycete that is capable of damaging plants in commercial production systems and natural ecosystems worldwide. The most common methods for the detection and diagnosis of P. c infection are expensive, elaborate and time consuming. This study was carried out to examine whether species specific and life cycle specific volatile organic compounds (VOCs) can be absorbed by solid-phase microextraction fibers and detected by gas chromatography that are produced by P. c and another oomycete Pythium dissotocum. A headspace solid-phase microextraction (HS-SPME) together with gas chromatography (GC) method was developed and optimized for the identification of the VOCs released by P. c. The optimized parameters included type of fiber, exposure time, desorption temperature and desorption time. Optimization was achieved with the analytes of P. c+V8A and V8A alone. To perform the HS-SPME, six types of fiber were assayed and compared: 7μm Polydimethylsiloxane (PDMS), 100μm Polydimethylsiloxane (PDMS), 50/30μm Divinylbenzene/CarboxenTM/Polydimethylsiloxane DVB/CAR/PDMS), 65μm Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), 85μm Polyacrylate (PA) fibre and 85μm CarboxenTM/ Polydimethylsiloxane (Carboxen™/PDMS). In a comparison of the efficacy of the fibers, the bipolar fiber DVB/CAR/PDMS had a higher extraction efficiency than the other fibers. An exposure time of 16h with DVB/CAR/PDMS fiber in the sample headspace was enough to reach the maximum extraction efficiency. A desorption time of 3min in the GC injector with the desorption temperature of 250°C was enough for the fiber to desorb the compounds of interest. The chromatograms and morphology study confirmed that the VOCs from P. c+V8A had distinct differences from V8A alone, as did different life cycle stages of P. c and different taxa such as Pythium dissotocum. The study proved that P. c has species and life cycle specific VOCs, which in turn demonstrated the feasibility of this method as means of

Keywords: Gas chromatography, headspace solid-phase microextraction, optimization, volatile compounds.

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4 The Effect of Drying Conditions on the Presence of Volatile Compounds in Cranberries

Authors: Karina Ruse, Martins Sabovics, Tatjana Rakcejeva, Lija Dukalska, Ruta Galoburda, Laima Berzina

Abstract:

the research was accomplished on fresh in Latvia wild growing cranberries and cranberry cultivars. The aim of the study was to evaluate effect of pretreatment method and drying conditions on the volatile compounds composition in cranberries. Berries pre-treatment methods were: perforation, halving and steam-blanching. The berries before drying in a cabinet drier were pre-treated using all three methods, in microwave vacuum drier – using a steam-blanching and halving. Volatile compounds in cranberries were analysed using GC-MS of extracts obtained by SPME. During present research 21 various volatile compounds were detected in fresh cranberries: the cultivar 'Steven' - 15, 'Bergman' and 'Early black' – 13, 'Ben Lear' and 'Pilgrim' – 11 and wild cranberries – 14 volatile compounds. In dried cranberries 20 volatile compounds were detected. Mathematical data processing allows drawing a conclusion that there exists the significant influence of cranberry cultivar, pre-treatment method and drying condition on volatile compounds in berries and new volatile compound formation.

Keywords: volatile compounds, cranberries, convective drier, microwave-vacuum drier

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3 Headspace Solid-phase Microextraction of Volatile and Furanic Compounds in Coated Fish Sticks: Effect of the Extraction Temperature

Authors: M. Trinidad Pérez-Palacios, Catarina Petisca, Olívia Pinho, Isabel M.P.L.V.O. Ferreira

Abstract:

This work evaluated the effect of temperature on headspace solid-phase microextraction of volatile and furanic compounds in coated fish sticks. The major goal was the analysis of the samples as consumed, to reproduce volatile compounds people feel when consuming those products. Extraction at 37 ºC (the human body temperature) throughout the HS-SPME analysis of volatile and furanic compounds in coated fish was compared with higher extraction temperatures, which are frequently used for this kind of determinations. The profile of volatile compounds found in deepfried (F) and non-fried (NF) coated fish at 37 and 50 ºC was different from that obtained at 80 ºC. Concerning furan and its derivatives, an extra formation of these compounds was observed at higher extraction temperatures. The analysis of volatile and furanic compounds in fish coated sticks simulating the cooking and eating conditions can be reliably carried out setting the headspace absorption temperature at 37 ºC.

Keywords: Analysis of samples as consumed, fish coated sticks, furans, headspace extraction temperature, volatiles.

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2 The Relations of Volatile Compounds, Some Parameters and Consumer Preference of Commercial Fermented Milks in Thailand

Authors: Suttipong Phosuksirikul, Rawichar Chaipojjana, Arunsri Leejeerajumnean

Abstract:

The aim of research was to define the relations between volatile compounds, some parameters (pH, titratable acidity (TA), total soluble solid (TSS), lactic acid bacteria count) and consumer preference of commercial fermented milks. These relations tend to be used for controlling and developing new fermented milk product. Three leading commercial brands of fermented milks in Thailand were evaluated by consumers (n=71) using hedonic scale for four attributes (sweetness, sourness, flavour, and overall liking), volatile compounds using headspace-solid phase microextraction (HS-SPME) GC-MS, pH, TA, TSS and LAB count. Then the relations were analyzed by principal component analysis (PCA). The PCA data showed that all of four attributes liking scores were related to each other. They were also related to TA, TSS and volatile compounds. The related volatile compounds were mainly on fermented produced compounds including acetic acid, furanmethanol, furfural, octanoic acid and the volatiles known as artificial fruit flavour (beta pinene, limonene, vanillin, and ethyl vanillin). These compounds were provided the information about flavour addition in commercial fermented milk in Thailand.

Keywords: Fermented milk, volatile compounds, preference, PCA.

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1 Volatile Profile of Monofloral Honeys Produced by Stingless Bees from the Brazilian Semiarid Region

Authors: Ana Caroliny Vieira da Costa, Marta Suely Madruga

Abstract:

In Brazil, there is a diverse fauna of social bees, known by Meliponinae or native stingless bees. These bees are important for providing a differentiated product, especially regarding unique sweetness, flavor, and aroma. However, information about the volatile fraction in honey produced by stingless native bees is still lacking. The aim of this work was to characterize the volatile compound profile of monofloral honey produced by jandaíra bees (Melipona subnitida Ducke) which used chanana (Turnera ulmifolia L.), malícia (Mimosa quadrivalvis) and algaroba (Prosopis juliflora (Sw.) DC) as their floral sources; and by uruçu bees (Melipona scutellaris Latrelle), which used chanana (Turnera ulmifolia L.), malícia (Mimosa quadrivalvis) and angico (Anadenanthera colubrina) as their floral sources. The volatiles were extracted using HS-SPME-GC-MS technique. The condition for the extraction was: equilibration time of 15 minutes, extraction time of 45 min and extraction temperature of 45°C. Through the results obtained, it was observed that the floral source had a strong influence on the aroma profile of the honey under evaluation, since the chemical profiles were marked primarily by the classes of terpenes, norisoprenoids, and benzene derivatives. Furthermore, the results obtained suggest the existence of differentiator compounds and potential markers for the botanical sources evaluated, such as linalool, D-sylvestrene, rose oxide and benzenethanol. These reports represent a valuable contribution to certifying the authenticity of those honey and provides for the first time, information intended for the construction of chemical knowledge of the aroma and flavor that characterize these honey produced in Brazil.

Keywords: Aroma, honey, semiarid, stingless, volatiles.

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