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Sample records for carbowax

  1. Determination of solubility parameters and thermodynamic properties in hydrocarbon-solvent systems by gas chromatography

    Directory of Open Access Journals (Sweden)

    E. Díaz

    2007-06-01

    Full Text Available Gas chromatography used to calculate the specific retention volume of several hydrocarbons in different chromatographic liquid phases (Squalane, Carbowax-400, Carbowax-1500, Carbowax-4000, Amine-220, Dinonyl phthalate, Tributyl phosphate and Trixylenyl phosphate. Some thermodynamic parameters, such as enthalpy of sorption and Flory-Huggins parameters relating the interaction between liquid phases and solutes, were also calculated from the determined retention volumes. Liquid phase solubility parameters of Squalane, Carbowax-400, Carbowax-1500 and Carbowax-4000 at 80 ºC as well as the polar and apolar components were calculated too. A new model was proposed to correlate polar contribution to the solubility parameter of a liquid phase with the specific retention volume of a solute in this liquid phase.

  2. EFFECT OF EMBEDDING METHODS VERSUS FIXATIVE TYPE ON KARYOMETRIC MEASURES

    NARCIS (Netherlands)

    BOON, ME; VANDERPOEL, HG; TAN, CJA; KOK, LP

    1994-01-01

    The influence of fixation and embedding methods in seven urologic tumor samples was studied karyometrically for 12 preparatory techniques. Routine histologic formalin fixation was compared with Carbowax and Kryofix fixatives. Also, histologic material was studied embedded in paraffin and plastic (GM

  3. DNA Extraction from Bronchial Aspirates for Molecular Cytology: Which Method to Take?

    OpenAIRE

    Grote, Hans Jürgen; Schmiemann, Viola; Sarbia, Mario; Böcking, Alfred

    2003-01-01

    Objective: To date, there are only few systematic reports on the quality of DNA extracted from routine diagnostic cytologic specimens. It was the aim of the present study to evaluate the ability of 50% ethanol/2% carbowax (Saccomanno fixative) to preserve bronchial secretions with high quality genomic DNA as well as to compare different DNA extraction methods. Methods: DNA was extracted from 45 bronchial aspirates by four different extraction protocols. Beside DNA yield, DNA quality with rega...

  4. Essential oils of camphor tree (cinnamomum camphora nees & eberm) cultivated in Southern Brazil

    OpenAIRE

    Caren D. Frizzo; Santos, Ana C; Natalia Paroul; Luciana A. Serafini; Eduardo Dellacassa; Daniel Lorenzo; Patrick Moyna

    2000-01-01

    The essential oils of two varieties of Camphor tree (Cinnamomum camphora Nees & Eberm, Lauraceae), known as Hon-Sho and Ho-Sho cultivated in experimental stands in Southern Brazil were studied. The essential oils were obtained from the leaves and twigs of young plants by hydrodistillation. The identification of the components was performed using GC, GC/MS and retention indexes on methyl silicone and carbowax phases. The main components identified were linalool in the Ho-Sho and camphor in the...

  5. Comparative study of different fabric phase sorptive extraction sorbents to determine emerging contaminants from environmental water using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Lakade, Sameer S; Borrull, Francesc; Furton, Kenneth G; Kabir, Abuzar; Fontanals, Núria; Marcé, Rosa Maria

    2015-11-01

    A new sorptive extraction technique, fabric phase sorptive extraction (FPSE), using different coating chemistries: non-polar sol-gel poly(dimethyldiphenylsiloxane) (PDMDPS), medium polar sol-gel poly(tetrahydrofuran) (PTHF), and polar sol-gel poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (PEG-PPG-PEG triblock) and sol-gel Carbowax 20 M were evaluated to extract a group of pharmaceuticals and personal care products (PPCPs) with wide range of polarity from environmental aqueous samples. Different parameters affecting FPSE such as sample pH, stirring speed, addition of salt, extraction time, sample volume, elution solvent and desorption time were optimized for each sorbent coated FPSE media. Under optimum conditions, FPSE media coated with sol-gel Carbowax 20 M provided the highest absolute recoveries (77-85%) for majority of the analytes with the exception of the most polar ones. Nevertheless, all four sorbents offered better recovery compared to the commercially available coating for stir-bar sorptive extraction based on Ethylene Glycol/Silicone (EG/Silicone). The method based on FPSE with sol-gel Carbowax 20 M media and liquid chromatography-(electrospray ionization) tandem mass spectrometry (LC-(ESI) MS/MS) was developed and validated for environmental water samples. Good apparent recoveries (41-80%), detection limits (1-50 ng L(-1)), repeatability (%RSD<15%, n=5) and reproducibility (%RSD<18%, n=5) were achieved. PMID:26452968

  6. Strength Loss in MA-MOX Green Pellets from Radiation Damage to Binders

    Energy Technology Data Exchange (ETDEWEB)

    Paul A. Lessing; W.R. Cannon; Gerald W. Egeland; Larry D. Zuck; James K. Jewell; Douglas W. Akers; Gary S. Groenewold

    2013-06-01

    The fracture strength of green Minor Actinides (MA)-MOX pellets containing 75 wt.% DUO2, 20 wt. % PuO2, 3 wt. % AmO2 and 2 wt. % NpO2 was studied as a function of storage time, after mixing in the binder and before sintering, to test the effect of radiation damage on binders. Fracture strength degraded continuously over the 10 days of the study for all three binders studied: PEG binder (Carbowax 8000), microcrystalline wax (Mobilcer X) and Styrene-acrylic copolymer (Duramax B1022) but the fracture strength of Duramax B1022 degraded the least. For instance, for several hours after mixing Carbowax 8000 with MA MOX, the fracture strength of a pellet was reasonably high and pellets were easily handled without breaking but the pellets were too weak to handle after 10 days. Strength measured using diametral compression test showed strength degradation was more rapid in pellets containing 1.0 wt. % Carbowax PEG 8000 compared to those containing only 0.2 wt. %, suggesting that irradiation not only left the binder less effective but also reduced the pellet strength. In contrast the strength of pellets containing Duramax B1022 degraded very little over the 10 day period. It was suggested that the styrene portion of the Duramax B1022 copolymer provided the radiation resistance.

  7. Strength loss in MA-MOX green pellets from radiation damage to binders

    Energy Technology Data Exchange (ETDEWEB)

    Lessing, Paul A. [Idaho National Laboratory, Idaho Falls, ID 83415 (United States); Cannon, W. Roger, E-mail: wrogercannon@gmail.com [Idaho National Laboratory, Idaho Falls, ID 83415 (United States); Egeland, Gerald W.; Zuck, Larry D.; Jewell, James K.; Akers, Douglas W.; Groenewold, Gary S. [Idaho National Laboratory, Idaho Falls, ID 83415 (United States)

    2013-06-15

    The fracture strength of green Minor Actinides (MA)-MOX pellets containing 75 wt.% DUO{sub 2}, 20 wt.% PuO{sub 2}, 3 wt.% AmO{sub 2} and 2 wt.% NpO{sub 2} was studied as a function of storage time, after mixing with the binder and before sintering, to test the effect of radiation damage on binders. Fracture strength degraded continuously over the 10 days of the study for all three binders studied: PEG binder (Carbowax 8000), microcrystalline wax (Mobilcer X) and styrene–acrylic copolymer (Duramax B1022) but the fracture strength of Duramax B1022 degraded the least. For instance, for several hours after mixing Carbowax 8000 with MA-MOX, the fracture strength of a pellet was reasonably high and pellets were easily handled without breaking but the pellets were too weak to handle after 10 days. Strength measured using diametral compression test showed that strength degradation was more rapid in pellets containing 1.0 wt.% Carbowax PEG 8000 compared to those containing only 0.2 wt.%, suggesting that irradiation not only left the binder less effective but also reduced the pellet strength. In contrast the strength of pellets containing Duramax B1022 degraded very little over the 10 days period. It was suggested that the styrene portion present in the Duramax B1022 copolymer provided the radiation resistance.

  8. Strength loss in MA-MOX green pellets from radiation damage to binders

    Science.gov (United States)

    Lessing, Paul A.; Cannon, W. Roger; Egeland, Gerald W.; Zuck, Larry D.; Jewell, James K.; Akers, Douglas W.; Groenewold, Gary S.

    2013-06-01

    The fracture strength of green Minor Actinides (MA)-MOX pellets containing 75 wt.% DUO2, 20 wt.% PuO2, 3 wt.% AmO2 and 2 wt.% NpO2 was studied as a function of storage time, after mixing with the binder and before sintering, to test the effect of radiation damage on binders. Fracture strength degraded continuously over the 10 days of the study for all three binders studied: PEG binder (Carbowax 8000), microcrystalline wax (Mobilcer X) and styrene-acrylic copolymer (Duramax B1022) but the fracture strength of Duramax B1022 degraded the least. For instance, for several hours after mixing Carbowax 8000 with MA-MOX, the fracture strength of a pellet was reasonably high and pellets were easily handled without breaking but the pellets were too weak to handle after 10 days. Strength measured using diametral compression test showed that strength degradation was more rapid in pellets containing 1.0 wt.% Carbowax PEG 8000 compared to those containing only 0.2 wt.%, suggesting that irradiation not only left the binder less effective but also reduced the pellet strength. In contrast the strength of pellets containing Duramax B1022 degraded very little over the 10 days period. It was suggested that the styrene portion present in the Duramax B1022 copolymer provided the radiation resistance.

  9. An Electronic Nose Based on Coated Piezoelectric Quartz Crystals to Certify Ewes’ Cheese and to Discriminate between Cheese Varieties

    Directory of Open Access Journals (Sweden)

    Maria Teresa S. R. Gomes

    2012-02-01

    Full Text Available An electronic nose based on coated piezoelectric quartz crystals was used to distinguish cheese made from ewes’ milk, and to distinguish cheese varieties. Two sensors coated with Nafion and Carbowax could certify half the ewes’ cheese samples, exclude 32 cheeses made from cow’s milk and to classify half of the ewes’ cheese samples as possibly authentic. Two other sensors, coated with polyvinylpyrrolidone and triethanolamine clearly distinguished between Flamengo, Brie, Gruyère and Mozzarella cheeses. Brie cheeses were further separated according to their origin, and Mozzarella grated cheese also appeared clearly separated from non-grated Mozzarella.

  10. Radioimpurity identification by retention index in tritium labeling

    International Nuclear Information System (INIS)

    Retention indexes (RI's) on SE-30 and Carbowax 20M columns are characteristic and can be used for identification purposes. A method for predicting RI on the basis of the number of atoms and contributions from substituents and functional groups is discussed. This method establishes a structure retention index relationship, capable of relating structure to RI and is useful for suggesting structures to match with radioactive peaks. Examples of labelled side products tentatively identified in this manner are given. (author) 13 refs.; 2 tabs

  11. Investigation of plant water relations with divided root systems of soybean.

    Science.gov (United States)

    Michel, B E; Elsharkawi, H M

    1970-11-01

    Soybean (Glycine max) was grown with root systems divided between adjacent cartons containing nutrient solution or soil. By adding polyethylene glycol (Carbowax 6000) to reduce solute potential or withholding water to reduce soil matric potential until water absorption from that side stopped, the root xylem water potential could be ascertained. Carbowax appeared to increase root resistance. An imbalance technique is described with which soil moisture contents of adjacent containers were followed individually. The patterns of water absorption obtained following repeated additions of water or addition of CaCl(2) solutions to one side indicated soil hydraulic conductivity became limiting at a soil water potential of -2 bars. A high concentration of CaCl(2) added to one side greatly reduced transpiration and produced severe plant injury. With part of the root system developing in nutrient solution, growth of roots into and water absorption from soil were slow; however, reduction of solute potential in the solution side greatly increased water absorption from the soil side. PMID:16657537

  12. Chemical analysis and fuel properties of oils from oilseed by supercritical fluid extraction

    Energy Technology Data Exchange (ETDEWEB)

    Yilmaz, N.; Sari, H.; Demirbas, A.

    2002-04-01

    In this work, the composition and the proportions of fatty acids in selected oilseeds growing in Turkey were determined. The dried and crushed samples were extracted in a standard Soxhlet extractor with acetone. During supercritical fluid extraction (SFE) the samples were carried out in a 100 mL cylindrical autoclave for 60 min at 515 K and 6.6 MPa at above critical temperature and critical pressure of acetone. After saponification, acidulation, and methylation procedures, methyl esters of the fatty acids from the Soxhlet and SFE were analyzed by a Hewlett-Packard 5790 GC on a 12 m 0.2 mm capillary column coated with Carbowax PEG 20. While the yield of saturated fatty acids from SFE of the samples increased, the yield of linoleic acid decreased. The increases and decreases in the fatty acids were irregular. (author)

  13. Determination of microquantities of methanol and ethanol in toluene by gas chromatography

    International Nuclear Information System (INIS)

    A study is made of the detection of methanol and ethanol in toluene by means of gas chromatography, using Porapak Q columns, 1 m long at 189 degree centigree, employing a flame ionization detector, with propanol as an internal standard. The variation od the detector absolute and relative response was found to be linear within the range of concentration studied, that is, from 5 to 1000 ppm. The limit of sensitivity for the detection of ethanol in a column of 2% Ucon, over Chromosorob G deactivated with 0,1% Carbowax 400, was 20 ppm, which was four times higher than the limit of sensitivity of the Porapak Q column. Also in this case, the absolute and relative response of the detector was linear. (Author) 3 refs

  14. Determination of phthalates in wine by headspace solid-phase microextraction followed by gas chromatography-mass spectrometry: fibre comparison and selection.

    Science.gov (United States)

    Carrillo, J D; Salazar, C; Moreta, C; Tena, M T

    2007-09-14

    This paper describes the development of a headspace solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC-MS) method for determining phthalates in wine. The HS-SPME conditions were thoroughly studied: first, the performance of six fibres at three temperature values and two sample volumes was surveyed by means of a 6 x 3 x 2 multi-factor categorical experimental design. From this study, three fibres - carbowax-divinylbenzene (CW-DVB), polyacrylate (PA) and polydimethylsiloxane-divinylbenzene (PDMS-DVB) - were selected. Then, temperature, sample volume and sodium chloride concentration were optimised using a central composite design and the overall desirability function for each fibre. The optimal values were 70 degrees C, a NaCl concentration of 2.6, 3.6 and 5.5M for PA, CW-DVB and PDMS-DVB fibres, respectively, and sample volumes of 4.0, 3.5 and 3.0 mL. Next, the performance characteristics of the three fibres were obtained and compared. PDMS-DVB fibre showed the best repeatability values followed by CW-DVB. PA fibre was not suitable for diethylhexylphthalate extraction and showed poor repeatability for the heavier phthalates, and was therefore discarded. Finally, the performance of CW-DVB and PDMS-DVB fibres was checked for red, white and rosé wines. PMID:17644103

  15. Modified HS-SPME for determination of quantitative relations between low-molecular oxygen compounds in various matrices.

    Science.gov (United States)

    Dawidowicz, Andrzej L; Szewczyk, Joanna; Dybowski, Michal P

    2016-09-01

    Similar quantitative relations between individual constituents of the liquid sample established by its direct injection can be obtained applying Polydimethylsiloxane (PDMS) fiber in the headspace solid phase microextraction (HS-SPME) system containing the examined sample suspended in methyl silica oil. This paper proves that the analogous system composed of sample suspension/emulsion in polyethylene glycol (PEG) and Carbowax fiber allows to get similar quantitative relations between components of the mixture as those established by its direct analysis, but only for polar constituents. It is demonstrated for essential oil (EO) components of savory, sage, mint and thyme, and of artificial liquid mixture of polar constituents. The observed differences in quantitative relations between polar constituents estimated by both applied procedures are insignificant (Fexp < Fcrit). The presented results indicates that wider applicability of the system composed of a sample suspended in the oil of the same physicochemical character as that of used SPME fiber coating strongly depends on the character of interactions between analytes-suspending liquid and analytes-fiber coating. PMID:27543021

  16. TREATMENT BY ALTERNATIVE METHODS OF REGRESSION GAS CHROMATOGRAPHIC RETENTION INDICES OF 35 PYRAZINES

    Directory of Open Access Journals (Sweden)

    Fatiha Mebarki

    2016-02-01

    Full Text Available The study treated two closer alternative methods of which the principal characteristic: a non-parametric method (the least absolute deviation (LAD and a traditional method of diagnosis OLS.This was applied to model, separately, the indices of retention of the same whole of 35 pyrazines (27 pyrazines with 8 other pyrazines in the same unit eluted to the columns OV-101 and Carbowax-20M, by using theoretical molecular descriptors calculated using the software DRAGON. The detection of influential observations for non-parametric method (LAD is a problem which has been extensively studied and offers alternative dicapproaches whose main feature is the robustness.here is presented and compared with the standard least squares regression .The comparison between methods LAD and OLS is based on the equation of the hyperplane, in order to confirm the robustness thus to detect by the meaningless statements and the points of lever and validated results in the state approached by the tests statistics: Test of Anderson-Darling, shapiro-wilk, Agostino, Jarque-Bera, graphic test (histogram of frequency and the confidence interval thanks to the concept of robustness to check if the distribution of the errors is really approximate.

  17. Determination of diphenylether herbicides in water samples by solid-phase microextraction coupled to liquid chromatography.

    Science.gov (United States)

    Sheu, Hong-Li; Sung, Yu-Hsiang; Melwanki, Mahaveer B; Huang, Shang-Da

    2006-11-01

    Solid-phase microextraction (SPME) coupled to LC for the analysis of five diphenylether herbicides (aclonifen, bifenox, fluoroglycofen-ethyl, oxyfluorfen, and lactofen) is described. Various parameters of extraction of analytes onto the fiber (such as type of fiber, extraction time and temperature, pH, impact of salt and organic solute) and desorption from the fiber in the desorption chamber prior to separation (such as type and composition of desorption solvent, desorption mode, soaking time, and flush-out time) were studied and optimized. Four commercially available SPME fibers were studied. PDMS/divinylbenzene (PDMS/DVB, 60 microm) and carbowax/ templated resin (CW/TPR, 50 microm) fibers were selected due to better extraction efficiencies. Repeatability (RSD, 0.994), and detection limit (0.33-1.74 and 0.22-1.94 ng/mL, respectively, for PDMS/DVB and CW/TPR) were investigated. Relative recovery (81-104% for PDMS/DVB and 83-100% for CW/TPR fiber) values have also been calculated. The developed method was successfully applied to the analysis of river water and water collected from a vegetable garden. PMID:17313105

  18. Detection of Landmine Signature using SAW-based Polymer-coated Chemical Sensor

    Directory of Open Access Journals (Sweden)

    O. K. Kannan

    2004-07-01

    Full Text Available The explosive charge within a landmine is the source for a mixture of chemical vapours that form a distinctive chemical signature indicative of a landmine. The concentrations of these compounds in the air over landmines is extremely low (parts-per-trillion or lower, well below the minimum detection limits of most field-portable chemical sensors. This paper describes a portable  surface acoustic wave-based polymer-coated sensor for the detection of hidden explosives. The sensitivity and selectivity of polymer-based sensors depend on several factors including the chemo-selective coating used, the physical properties of the vapour(s of interest, the selected transducers, and the operating conditions. The polymer-based sensor was calibrated in the  laboratory using the explosive vapour generator. The preliminary results indicated that the carbowax 1000 could be a very good chemical interface to sense low levels of chemical signature of explosive material. Response for 50 ppb of TNT vapours was observed to be 400 Hz for an exposure of 2 min.

  19. Applying Convolution-Based Processing Methods To A Dual-Channel, Large Array Artificial Olfactory Mucosa

    Science.gov (United States)

    Taylor, J. E.; Che Harun, F. K.; Covington, J. A.; Gardner, J. W.

    2009-05-01

    Our understanding of the human olfactory system, particularly with respect to the phenomenon of nasal chromatography, has led us to develop a new generation of novel odour-sensitive instruments (or electronic noses). This novel instrument is in need of new approaches to data processing so that the information rich signals can be fully exploited; here, we apply a novel time-series based technique for processing such data. The dual-channel, large array artificial olfactory mucosa consists of 3 arrays of 300 sensors each. The sensors are divided into 24 groups, with each group made from a particular type of polymer. The first array is connected to the other two arrays by a pair of retentive columns. One channel is coated with Carbowax 20 M, and the other with OV-1. This configuration partly mimics the nasal chromatography effect, and partly augments it by utilizing not only polar (mucus layer) but also non-polar (artificial) coatings. Such a device presents several challenges to multi-variate data processing: a large, redundant dataset, spatio-temporal output, and small sample space. By applying a novel convolution approach to this problem, it has been demonstrated that these problems can be overcome. The artificial mucosa signals have been classified using a probabilistic neural network and gave an accuracy of 85%. Even better results should be possible through the selection of other sensors with lower correlation.

  20. Comparative study of the whisky aroma profile based on headspace solid phase microextraction using different fibre coatings.

    Science.gov (United States)

    Câmara, J S; Marques, J C; Perestrelo, R M; Rodrigues, F; Oliveira, L; Andrade, P; Caldeira, M

    2007-05-25

    A dynamic headspace solid-phase microextraction (HS-SPME) and gas chromatography coupled to ion trap mass spectrometry (GC-(IT)MS) method was developed and applied for the qualitative determination of the volatile compounds present in commercial whisky samples which alcoholic content was previously adjusted to 13% (v/v). Headspace SPME experimental conditions, such as fibre coating, extraction temperature and extraction time, were optimized in order to improve the extraction process. Five different SPME fibres were used in this study, namely, poly(dimethylsiloxane) (PDMS), poly(acrylate) (PA), Carboxen-poly(dimethylsiloxane) (CAR/PDMS), Carbowax-divinylbenzene (CW/DVB) and Carboxen-poly(dimethylsiloxane)-divinylbenzene (CAR/PDMS/DVB). The best results were obtained using a 75 microm CAR/PDMS fibre during headspace extraction at 40 degrees C with stirring at 750 rpm for 60 min, after saturating the samples with salt. The optimised methodology was then applied to investigate the volatile composition profile of three Scotch whisky samples--Black Label, Ballantines and Highland Clan. Approximately seventy volatile compounds were identified in the these samples, pertaining at several chemical groups, mainly fatty acids ethyl esters, higher alcohols, fatty acids, carbonyl compounds, monoterpenols, C13 norisoprenoids and some volatile phenols. The ethyl esters form an essential group of aroma components in whisky, to which they confer a pleasant aroma, with "fruity" odours. Qualitatively, the isoamyl acetate, with "banana" aroma, was the most interesting. Quantitatively, significant components are ethyl esters of caprilic, capric and lauric acids. The highest concentration of fatty acids, were observed for caprilic and capric acids. From the higher alcohols the fusel oils (3-methylbutan-1-ol and 2.phenyletanol) are the most important ones.

  1. Partitioning behavior of aromatic components in jet fuel into diverse membrane-coated fibers.

    Science.gov (United States)

    Baynes, Ronald E; Xia, Xin-Rui; Barlow, Beth M; Riviere, Jim E

    2007-11-01

    Jet fuel components are known to partition into skin and produce occupational irritant contact dermatitis (OICD) and potentially adverse systemic effects. The purpose of this study was to determine how jet fuel components partition (1) from solvent mixtures into diverse membrane-coated fibers (MCFs) and (2) from biological media into MCFs to predict tissue distribution. Three diverse MCFs, polydimethylsiloxane (PDMS, lipophilic), polyacrylate (PA, polarizable), and carbowax (CAR, polar), were selected to simulate the physicochemical properties of skin in vivo. Following an appropriate equilibrium time between the MCF and dosing solutions, the MCF was injected directly into a gas chromatograph/mass spectrometer (GC-MS) to quantify the amount that partitioned into the membrane. Three vehicles (water, 50% ethanol-water, and albumin-containing media solution) were studied for selected jet fuel components. The more hydrophobic the component, the greater was the partitioning into the membranes across all MCF types, especially from water. The presence of ethanol as a surrogate solvent resulted in significantly reduced partitioning into the MCFs with discernible differences across the three fibers based on their chemistries. The presence of a plasma substitute (media) also reduced partitioning into the MCF, with the CAR MCF system being better correlated to the predicted partitioning of aromatic components into skin. This study demonstrated that a single or multiple set of MCF fibers may be used as a surrogate for octanol/water systems and skin to assess partitioning behavior of nine aromatic components frequently formulated with jet fuels. These diverse inert fibers were able to assess solute partitioning from a blood substitute such as media into a membrane possessing physicochemical properties similar to human skin. This information may be incorporated into physiologically based pharmacokinetic (PBPK) models to provide a more accurate assessment of tissue dosimetry of

  2. Optimization of an analytical methodology for the determination of alkyl- and methoxy-phenolic compounds by HS-SPME in biomass smoke

    Energy Technology Data Exchange (ETDEWEB)

    Conde, Francisco J.; Afonso, Ana M.; Gonzalez, Venerando; Ayala, Juan H. [University of La Laguna, Campus de Anchieta, Department of Analytical Chemistry, Nutrition and Food Science, La Laguna (Spain)

    2006-08-15

    A sampling and analysis method for the determination of 21 phenolic compounds in smoke samples from biomass combustion has been developed. The smoke is used to make smoked foods, following an artisanal procedure used in some parts of the Canary Islands. The sampling system consists of a Bravo H air sampler, two impingers, each one containing an aqueous solution of sodium hydroxide 0.1 mol L{sup -1}, followed by a silica gel trap. The variables optimized to reach the best sampling conditions were volume of absorbent solution and sampling flow. Under the optimum conditions, 100 mL of absorbent solution of NaOH 0.10 mol L{sup -1} and 2 L min{sup -1} for the sampling flow, sampling efficiencies are higher than 80%. Analysis of phenolic compounds was carried out by headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). Five different fiber coatings were employed in this study. By means of a central composite design, extraction time, salt concentration, and pH of the solution were optimized: 65-{mu}m carbowax-divinylbenzene, extraction time 90 min, concentration in NaCl of 35% (m/v), and pH 2 yielded the highest response. Detection limits of phenol and their alkyl derivatives, guaiacol and eugenol, are between 1.13 and 4.60 ng mL{sup -1}. 3-Methoxyphenol, 2,6-dimethoxyphenol, and vanillin have detection limits considerably higher. Good linearity (R {sup 2}{>=}0.98) was observed for all calibration curves in the established ranges. The reproducibility of the method (RSD, relative standard deviation) was found to oscillate between 7 and 18% (generally close or lower than 10%). (orig.)

  3. Optimization of headspace solid-phase microextraction for the analysis of specific flavors in enzyme modified and natural Cheddar cheese using factorial design and response surface methodology.

    Science.gov (United States)

    Januszkiewicz, Julien; Sabik, Hassan; Azarnia, Sorayya; Lee, Byong

    2008-06-27

    A headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC/MS) method was developed using experimental designs to quantify the flavor of commercial Cheddar cheese and enzyme-modified Cheddar cheese (EMCC). Seven target compounds (dimethyl disulfide, hexanal, hexanol, 2-heptanone, ethyl hexanoate, heptanoic acid, delta-decalactone) representative of different chemical families frequently present in Cheddar cheese were selected for this study. Three types of SPME fibres were tested: Carboxen/polydimethylsiloxane (CAR/PDMS), polyacrylate (PA) and Carbowax/divinylbenzene (CW/DVB). NaCl concentration and temperature, as well as extraction time were tested for their effect on the HS-SPME process. Two series of two-level full factorial designs were carried out for each fibre to determine the factors which best support the extraction of target flavors. Therefore, central composite designs (CCDs) were performed and response surface models were derived. Optimal extraction conditions for all selected compounds, including internal standards, were: 50 min at 55 degrees C in 3M NaCl for CAR/PDMS, 64 min at 62 degrees C in 6M NaCl for PA, and 37 min at 67 degrees C in 6M NaCl for CW/DVB. Given its superior sensitivity, CAR/PDMS fibre was selected to evaluate the target analytes in commercial Cheddar cheese and EMCC. With this fibre, calibration curves were linear for all targeted compounds (from 0.5 to 6 microg g(-1)), except for heptanoic acid which only showed a linear response with PA fibres. Detection limits ranged from 0.3 to 1.6 microg g(-1) and quantification limits from 0.8 to 3.6 microg g(-1). The mean repeatability value for all flavor compounds was 8.8%. The method accuracy is satisfactory with recoveries ranging from 97 to 109%. Six of the targeted flavors were detected in commercial Cheddar cheese and EMCC. PMID:18495140