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Sample records for headspace sorptive extraction

  1. Quantitative analysis of perfumes in talcum powder by using headspace sorptive extraction.

    Science.gov (United States)

    Ng, Khim Hui; Heng, Audrey; Osborne, Murray

    2012-03-01

    Quantitative analysis of perfume dosage in talcum powder has been a challenge due to interference of the matrix and has so far not been widely reported. In this study, headspace sorptive extraction (HSSE) was validated as a solventless sample preparation method for the extraction and enrichment of perfume raw materials from talcum powder. Sample enrichment is performed on a thick film of poly(dimethylsiloxane) (PDMS) coated onto a magnetic stir bar incorporated in a glass jacket. Sampling is done by placing the PDMS stir bar in the headspace vial by using a holder. The stir bar is then thermally desorbed online with capillary gas chromatography-mass spectrometry. The HSSE method is based on the same principles as headspace solid-phase microextraction (HS-SPME). Nevertheless, a relatively larger amount of extracting phase is coated on the stir bar as compared to SPME. Sample amount and extraction time were optimized in this study. The method has shown good repeatability (with relative standard deviation no higher than 12.5%) and excellent linearity with correlation coefficients above 0.99 for all analytes. The method was also successfully applied in the quantitative analysis of talcum powder spiked with perfume at different dosages. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Time since discharge of 9mm cartridges by headspace analysis, part 1: Comprehensive optimisation and validation of a headspace sorptive extraction (HSSE) method.

    Science.gov (United States)

    Gallidabino, M; Romolo, F S; Weyermann, C

    2017-03-01

    Estimating the time since discharge of spent cartridges can be a valuable tool in the forensic investigation of firearm-related crimes. To reach this aim, it was previously proposed that the decrease of volatile organic compounds released during discharge is monitored over time using non-destructive headspace extraction techniques. While promising results were obtained for large-calibre cartridges (e.g., shotgun shells), handgun calibres yielded unsatisfying results. In addition to the natural complexity of the specimen itself, these can also be attributed to some selective choices in the methods development. Thus, the present series of paper aimed to more systematically evaluate the potential of headspace analysis to estimate the time since discharge of cartridges through the use of more comprehensive analytical and interpretative techniques. Specifically, in this first part, a method based on headspace sorptive extraction (HSSE) was comprehensively optimised and validated, as the latter recently proved to be a more efficient alternative than previous approaches. For this purpose, 29 volatile organic compounds were preliminary selected on the basis of previous works. A multivariate statistical approach based on design of experiments (DOE) was used to optimise variables potentially involved in interaction effects. Introduction of deuterated analogues in sampling vials was also investigated as strategy to account for analytical variations. Analysis was carried out by selected ion mode, gas chromatography coupled to mass spectrometry (GC-MS). Results showed good chromatographic resolution as well as detection limits and peak area repeatability. Application to 9mm spent cartridges confirmed that the use of co-extracted internal standards allowed for improved reproducibility of the measured signals. The validated method will be applied in the second part of this work to estimate the time since discharge of 9mm spent cartridges using multivariate models.

  3. Application of headspace sorptive extraction and gas chromatographic/mass spectrometric and chemometric methods to the quantification of pine nuts and pecorino in Pesto Genovese.

    Science.gov (United States)

    Zunin, Paola; Leardi, Riccardo; Boggia, Raffaella

    2009-01-01

    Headspace sorptive extraction and GC/MS, coupled with chemometric tools, were used to predict the amounts of pine nuts and Pecorino in Pesto Genovese, a typical Italian basil-based pasta sauce. Two groups of samples were prepared at different times and with ingredients from different batches for building the predicting models and testing their performances. Principal component analysis and partial least-squares regression (PLS) were applied to the chromatographic data. The 24 most-predictive variables were selected, and the application of PLS to the training set samples led to two models that explained approximately 70% of the variance in cross-validation, with prediction errors of 0.1 g for Pecorino and 0.6 g for pine nuts, thus confirming the reliability of the analytical method and the predicting ability of the models. The results obtained for the test set samples were not completely satisfactory, with a prediction error and a bias of 5.0 and -4.1 g, respectively, for Pecorino and corresponding values of 4.1 and 2.0 g for pine nuts. This preliminary study shows that the analytical methods used can allow construction of models with high predictive ability only if the great variability of the headspace composition of the ingredients and the effect of Twister are considered.

  4. Determination of E,E-farnesol in Makgeolli (rice wine) using dynamic headspace sampling and stir bar sorptive extraction coupled with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Ha, Jaeho; Wang, Yiru; Jang, Hyejin; Seog, Homoon; Chen, Xi

    2014-01-01

    In this paper, we analysed the volatile and semi-volatile compounds, including E,E-farnesol in Makgeolli which is a traditional type of Korean fermented rice wines. Forty-one compounds including alcohols, 1-butanol-3-methyl acetate, E,E-farnesol, stearol, and phytane, were separated and quantified by dynamic headspace sampling (DHS) and stir bar sorptive extraction (SBSE) coupled with gas chromatography-mass spectrometry. SBSE has been found to be an effective method for analysing E,E-farnesol levels in Makgeolli. The experimental parameters related to the extraction efficiency of the SBSE method, such as ethanol concentration and filtration, were studied and optimised. The linear dynamic range of the SBSE method for E,E-farnesol ranged from 0.02 to 200ngml(-1) with R(2)=0.9974. The limit of detection and limit of quantification of the SBSE method were 0.02 and 0.05ngml(-1), respectively. The relative standard deviation of intra- and inter-day reproducibility was less than 6.2% and 9.9%, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

  5. Evaluation of three headspace sorptive extraction coatings for the determination of volatile terpenes in honey using gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

    2015-06-19

    Headspace sorptive extraction (HSSE) was used to preconcentrate seven monoterpenes (eucalyptol, linalool, menthol, geraniol, carvacrol, thymol and eugenol) for separation by gas chromatography and mass spectrometry (GC-MS). Three commercially available coatings for the stir bars, namely Polydimethylsiloxane (PDMS), polyacrilate (PA) and Ethylene glycol-silicone (EG-Silicone), were tested, and the influential parameters both in the adsorption and the thermal desorption steps were optimized. PDMS provided the best sensitivity for linalool, geraniol, menthol and eucalyptol, whereas EG-Silicone was best for extracting the phenolic monoterpenes studied. Considering the average obtained slopes from all compounds, PDMS pointed as the best option, and the analytical characteristics for the HSSE-TD-GC-MS method using this coating were obtained. Quantification of the samples was carried out by matrix-matched calibration using a synthetic honey. Detection limits ranged between 0.007 and 0.032 ng g(-1), depending on the compound. Twelve honey samples of different floral origins were analyzed using the HSSE-GC-MS method, the analytes being detected at concentrations up to 64 ng g(-1).

  6. Non-Destructive Assessment of Aroma Volatiles from a Climacteric Near-Isogenic Line of Melon Obtained by Headspace Stir-Bar Sorptive Extraction

    Science.gov (United States)

    Fernández-Trujillo, Juan Pablo; Dos-Santos, Noelia; Martínez-Alcaraz, Rocío; Le Bleis, Inés

    2013-01-01

    A climacteric aromatic near-isogenic line (NIL) of melon (Cucumis melo L.) SC3-5-1 contained an introgression of the non-climacteric Korean cultivar “Shongwan Charmi” accession PI 161375 (SC) in the genetic background of the non-climacteric cultivar “Piel de Sapo” (PS). The aroma production was monitored during ripening at 21 °C in intact fruit using headspace sorptive bar extraction (HSSE). Bars were composed of polydimethylsiloxane (PDMS) and aromas were desorbed and analyzed by gas-chromatography mass-spectrometry. The aromatic profile was composed of 70 aromatic compounds plus 21 alkanes with a predominance of esters, particularly acetate (2-methylbutyl acetate, 2-methylpropyl acetate, hexyl acetate, and phenylmethyl acetate). Some compounds were severely affected by postharvest time. The acetate esters (3-methylbutyl acetate, butan-2-yl acetate and phenylmethyl acetate) decreased with ripening and sulfur-derived compounds (S-methyl butanethioate and S-methyl 3-methylbutanethioate) increased gradually with ripening. A few compounds increased at the senescence phase (propyl ethanoate). Other compounds such as hexadecanoic acid showed a marked decrease after harvest, some decreasing from a relative maximum at harvest (2-methylpropyl hexanoate; n-hexanoic acid; nonanoic acid).

  7. Integrated sampling and analysis unit for the determination of sexual pheromones in environmental air using fabric phase sorptive extraction and headspace-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Alcudia-León, M Carmen; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel; Kabir, Abuzar; Furton, Kenneth G

    2017-03-10

    This article presents a novel unit that integrates for the first time air sampling and preconcentration based on the use of fabric phase sorptive extraction principles. The determination of Tuta absoluta sexual pheromone traces in environmental air has been selected as analytical problem. For this aim, a novel laboratory-built unit made up of commercial brass elements as holder of the sol-gel coated fabric extracting phase has been designed and optimized. The performance of the integrated unit was evaluated analyzing environmental air sampled in tomato crops. The unit can work under sampling and analysis mode which eliminates any need for sorptive phase manipulation prior to instrumental analysis. In the sampling mode, the unit can be connected to a sampling pump to pass the air through the sorptive phase at a controlled flow-rate. In the analysis mode, it is placed in the gas chromatograph autosampler without any instrumental modification. It also diminishes the risk of cross contamination between sampling and analysis. The performance of the new unit has been evaluated using the main components of the sexual pheromone of Tuta absoluta [(3E,8Z,11Z)-tetradecatrien-1-yl acetate and (3E,8Z)-tetradecadien-1-yl acetate] as model analytes. The limits of detection for both compounds resulted to be 1.6μg and 0.8μg, respectively, while the precision (expressed as relative standard deviation) was better than 3.7%. Finally, the unit has been deployed in the field to analyze a number of real life samples, some of them were found positive. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Analysis of volatiles of malt whisky by solid-phase microextraction and stir bar sorptive extraction.

    Science.gov (United States)

    Demyttenaere, Jan C R; Martínez, Jorge I Sánchez; Verhé, Roland; Sandra, Pat; De Kimpe, Norbert

    2003-01-24

    Blended Scotch whisky was analysed by solid-phase microextraction (SPME) and stir bar sorptive extraction (SBSE) to study the composition of the volatiles. For SPME analysis, three different fibres were compared, poly(dimethylsiloxane) (PDMS) (100 microm). poly(acrylate) (PA) (85 microm) and divinylbenzene-Carboxen on poly(dimethylsiloxane) (DVB-CAR-(PDMS) (50/30 microm). It was found that the PDMS and DVB-CAR-PDMS fibres showed a higher enrichment capacity than PA as well as a better reproducibility. The influence of sampling time, temperature and salt addition on the enrichment of volatiles as well as the difference between liquid and headspace SPME were studied. An optimum SPME method was developed. Finally a more recent sample preparation technique, namely SBSE was evaluated to extract whisky volatiles.

  9. The use of stir bar sorptive extraction-A potential alternative method for the determination of furan, evaluated using two example food matrices

    Energy Technology Data Exchange (ETDEWEB)

    Ridgway, Kathy, E-mail: Kathy.Ridgway@Unilever.com [Safety and Environmental Assurance Centre, Unilever Colworth, Bedfordshire, MK44 1LQ (United Kingdom); Lalljie, Sam P.D. [Safety and Environmental Assurance Centre, Unilever Colworth, Bedfordshire, MK44 1LQ (United Kingdom); Smith, Roger M. [Department of Chemistry, Loughborough University, Loughborough, Leics, LE11 3TU (United Kingdom)

    2010-01-11

    A comparison is made between static headspace analysis and stir bar sorptive extraction (SBSE) for the quantitative determination of furan. The SBSE technique was optimised and evaluated using two example food matrices (coffee and jarred baby food). The use of the SBSE technique in most cases, gave comparable results to the static headspace method, using the method of standard additions with d{sub 4}-labelled furan as an internal standard. Using the SBSE method, limits of detection down to 2 ng g{sup -1} were achieved, with only a 1 h extraction. The method was performed at ambient temperatures, thus eliminating the possibility of formation of furan during extraction.

  10. Direct Contact Sorptive Extraction: A Robust Method for Sampling Plant Volatiles in the Field.

    Science.gov (United States)

    Kfoury, Nicole; Scott, Eric; Orians, Colin; Robbat, Albert

    2017-09-27

    Plants produce volatile organic compounds (VOCs) with diverse structures and functions, which change in response to environmental stimuli and have important consequences for interactions with other organisms. To understand these changes, in situ sampling is necessary. In contrast to dynamic headspace (DHS), which is the most often employed method, direct contact sampling employing a magnetic stir bar held in place by a magnet eliminates artifacts produced by enclosing plant materials in glass or plastic chambers. Direct-contact sorptive extraction (DCSE) using polydimethylsiloxane coated stir bars (Twisters) coated stir bars is more sensitive than DHS, captures a wider range of compounds, minimizes VOC collection from neighboring plants, and distinguishes the effects of herbivory in controlled and field conditions. Because DCSE is relatively inexpensive and simple to employ, scalability of field trials can be expanded concomitant with increased sample replication. The sensitivity of DCSE combined with the spectral deconvolution data analysis software makes the two ideal for comprehensive, in situ profiling of plant volatiles.

  11. Alternative sorptive extraction method for gas chromatography determination of halogenated anisoles in water and wine samples

    Energy Technology Data Exchange (ETDEWEB)

    Montes, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain); Rodriguez, I. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)], E-mail: qnisaac@usc.es; Rubi, E.; Bollain, M.H.; Cela, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)

    2007-09-05

    An alternative sorptive microextraction method for the determination of five halogenated anisoles in water and wine matrices is proposed. Analytes were concentrated in an inexpensive and disposable piece of bulk polydimethylsiloxane (PDMS), desorbed with a small volume of organic solvent, and determined by gas chromatography with electron-capture detection (GC-ECD) or tandem mass spectrometry (GC-MS/MS). The influence of several factors on the efficiency of extraction and desorption steps was investigated in detail and the observed behaviour justified on the basis of thermodynamics and kinetics of the solid-phase microextraction technique. Under optimised conditions, analytes were first extracted in the headspace (HS) mode, at room temperature, for 2.5 h and then desorbed with 1 mL of n-pentane. This extract was further evaporated to 50 {mu}L. The overall extraction yield of the procedure ranged from 40 to 55% and the limits of quantification remained between 0.5 and 20 ng L{sup -1}, depending on the compound considered and the detection technique. Precision and linearity of the method were excellent for all species with both GC-ECD and GC-MS/MS detection. Matrix effects were evaluated with different water and wine samples; moreover, the suitability of the PDMS sorbent for storage of analytes, under different conditions, was demonstrated.

  12. Characterisation, quantity and sorptive properties of microplastics extracted from cosmetics.

    Science.gov (United States)

    Napper, Imogen E; Bakir, Adil; Rowland, Steven J; Thompson, Richard C

    2015-10-15

    Cosmetic products, such as facial scrubs, have been identified as potentially important primary sources of microplastics to the marine environment. This study characterises, quantifies and then investigates the sorptive properties of plastic microbeads that are used as exfoliants in cosmetics. Polyethylene microbeads were extracted from several products, and shown to have a wide size range (mean diameters between 164 and 327 μm). We estimated that between 4594 and 94,500 microbeads could be released in a single use. To examine the potential for microbeads to accumulate and transport chemicals they were exposed to a binary mixture of (3)H-phenanthrene and (14)C-DDT in seawater. The potential for transport of sorbed chemicals by microbeads was broadly similar to that of polythene (PE) particles used in previous sorption studies. In conclusion, cosmetic exfoliants are a potentially important, yet preventable source of microplastic contamination in the marine environment. Copyright © 2015 Elsevier Ltd. All rights reserved.

  13. Analysis of volatiles in Pinotage wines by stir bar sorptive extraction and chemometric profiling.

    Science.gov (United States)

    Weldegergis, Berhane T; Crouch, Andrew M

    2008-11-12

    A fast, simple, cost-effective, and reliable method based on stir bar sorptive extraction (SBSE) in the headspace mode was used for the analysis of 39 volatile components in Pinotage wines. The method was sensitive, with LODs ranging from 50.0 pg/L to 281 ng/L and LOQs between 180 pg/L and 938 ng/L. Precision was between 6 and 20%. The intermediate precision was within the acceptable range. Moreover, good calibration curves with R(2) > 0.99 for all compounds were achieved. The method was successfully applied for the analysis of 87 young Pinotage wines of vintages 2005 and 2006 collected from various South African regions. To characterize the results based on vintage and origin, the obtained concentrations of the compounds were subjected to chemometric analysis. Exploratory factor analysis (FA), principal component analysis (PCA), and analysis of variance (one-way ANOVA) were consecutively done. The chemometrics approach revealed a reasonable correlation among the volatile components of these wines, as well as with respect to their year of production.

  14. Multiple headspace extraction for gas detection in ionic liquids.

    Science.gov (United States)

    Müller, D; Fühl, M; Pinkwart, K; Baltes, N

    2014-10-16

    In this study multiple headspace extraction was used for the first time to measure the saturation concentration of carbon monoxide and oxygen in various ionic liquids (ILs). Many processes in ILs involve the reaction of gases so that the reactant solubility is not a mere characteristical parameter, but understanding the solubility of gases in ILs is required for assessing the feasibility of possible applications. Multiple headspace extraction has proofed to be a powerful tool to obtain solubilities in good accordance with literature data. The measured saturation concentration for carbon monoxide and oxygen in ILs based on rarely researched tetracyanoborates and other anions was in the range of 1.5-6.5mmol/L. The great advantage of multiple headspace extraction is that it is a nonexpensive method that can be realised in most analytical laboratories by combination of a simple gas chromatograph and an eligible headspace injector.

  15. A short review of headspace extraction and ultrasonic solvent extraction for honey volatiles fingerprinting

    OpenAIRE

    Jerković, I.; Marijanović, Z.

    2009-01-01

    Honey volatiles exhibit a potential role in distinguishing honeys as a function of botanical origin, but heating of honey generates artefacts such as compounds of Strecker degradation and Maillard reaction products. This short review is focused on the most recently applied methods for honey volatiles fingerprinting (without generation of thermal artefacts): headspace extraction (dynamic headspace extraction (DHE), headspace solid-phase microextraction (HS-SPME)) and ultrasonic solvent extract...

  16. A comparison of sorptive extraction techniques coupled to a new quantitative, sensitive, high throughput GC-MS/MS method for methoxypyrazine analysis in wine.

    Science.gov (United States)

    Hjelmeland, Anna K; Wylie, Philip L; Ebeler, Susan E

    2016-02-01

    Methoxypyrazines are volatile compounds found in plants, microbes, and insects that have potent vegetal and earthy aromas. With sensory detection thresholds in the low ng L(-1) range, modest concentrations of these compounds can profoundly impact the aroma quality of foods and beverages, and high levels can lead to consumer rejection. The wine industry routinely analyzes the most prevalent methoxypyrazine, 2-isobutyl-3-methoxypyrazine (IBMP), to aid in harvest decisions, since concentrations decrease during berry ripening. In addition to IBMP, three other methoxypyrazines IPMP (2-isopropyl-3-methoxypyrazine), SBMP (2-sec-butyl-3-methoxypyrazine), and EMP (2-ethyl-3-methoxypyrazine) have been identified in grapes and/or wine and can impact aroma quality. Despite their routine analysis in the wine industry (mostly IBMP), accurate methoxypyrazine quantitation is hindered by two major challenges: sensitivity and resolution. With extremely low sensory detection thresholds (~8-15 ng L(-1) in wine for IBMP), highly sensitive analytical methods to quantify methoxypyrazines at trace levels are necessary. Here we were able to achieve resolution of IBMP as well as IPMP, EMP, and SBMP from co-eluting compounds using one-dimensional chromatography coupled to positive chemical ionization tandem mass spectrometry. Three extraction techniques HS-SPME (headspace-solid phase microextraction), SBSE (stirbar sorptive extraction), and HSSE (headspace sorptive extraction) were validated and compared. A 30 min extraction time was used for HS-SPME and SBSE extraction techniques, while 120 min was necessary to achieve sufficient sensitivity for HSSE extractions. All extraction methods have limits of quantitation (LOQ) at or below 1 ng L(-1) for all four methoxypyrazines analyzed, i.e., LOQ's at or below reported sensory detection limits in wine. The method is high throughput, with resolution of all compounds possible with a relatively rapid 27 min GC oven program.

  17. Determination of free medium-chain fatty acids in beer by stir bar sorptive extraction.

    Science.gov (United States)

    Horák, Tomás; Culík, Jirí; Jurková, Marie; Cejka, Pavel; Kellner, Vladimír

    2008-07-04

    Free medium-chain fatty acids in beer originate from raw materials, mainly from the fermentation activity of yeasts, and can influence beer taste, vitality of yeasts and also the foam stability of beer. This study presents the development of the method for the determination of free fatty medium-chain acids including caproic acid, caprylic acid, capric acid and lauric acid in beer or wort using stir bar sorptive extraction (SBSE). The combination of this extraction technique with solvent back extraction of the extracted analytes and subsequent gas chromatographic analysis with flame ionization detection was used for the determination of these compounds. The influences of different solvent back solutions, sampling time, solvent back extraction times and different contents of ethanol were studied. The method had high repeatability (RSD <6.7%), good linearity (the correlation coefficients were higher than 0.9963 for quadratic curves over the concentration range 0.5-8.0mg/l) and recoveries 57-89%.

  18. Fabric phase sorptive extraction: Two practical sample pretreatment techniques for brominated flame retardants in water.

    Science.gov (United States)

    Huang, Guiqi; Dong, Sheying; Zhang, Mengfei; Zhang, Haihan; Huang, Tinglin

    2016-09-15

    Sample pretreatment is the critical section for residue monitoring of hazardous pollutants. In this paper, using the cellulose fabric as host matrix, three extraction sorbents such as poly (tetrahydrofuran) (PTHF), poly (ethylene glycol) (PEG) and poly (dimethyldiphenylsiloxane) (PDMDPS), were prepared on the surface of the cellulose fabric. Two practical extraction techniques including stir bar fabric phase sorptive extraction (stir bar-FPSE) and magnetic stir fabric phase sorptive extraction (magnetic stir-FPSE) have been designed, which allow stirring of fabric phase sorbent during the whole extraction process. In the meantime, three brominated flame retardants (BFRs) [tetrabromobisphenol A (TBBPA), tetrabromobisphenol A bisallylether (TBBPA-BAE), tetrabromobisphenol A bis(2,3-dibromopropyl)ether (TBBPA-BDBPE)] in the water sample were selected as model analytes for the practical evaluation of the proposed two techniques using high-performance liquid chromatography (HPLC). Moreover, various experimental conditions affecting extraction process such as the type of fabric phase, extraction time, the amount of salt and elution conditions were also investigated. Due to the large sorbent loading capacity and unique stirring performance, both techniques possessed high extraction capability and fast extraction equilibrium. Under the optimized conditions, high recoveries (90-99%) and low limits of detection (LODs) (0.01-0.05 μg L(-1)) were achieved. In addition, the reproducibility was obtained by evaluating the intraday and interday precisions with relative standard deviations (RSDs) less than 5.1% and 6.8%, respectively. The results indicated that two pretreatment techniques were promising and practical for monitoring of hazardous pollutants in the water sample. Due to low solvent consumption and high repeated use performance, proposed techniques also could meet green analytical criteria.

  19. Multi-residue off-flavour profiling in wine using stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Franc, Céline; David, Frank; de Revel, Gilles

    2009-04-10

    A multi-residue method (MRM) for the detection and quantification of eight compounds responsible for off-flavours in wine using stir bar sorptive extraction (SBSE) followed by thermal desorption (TD) and gas chromatography-mass spectrometry (GC-MS) analysis is presented. The extraction and desorption conditions were optimised in order to get the best compromise for the simultaneous analysis of the eight target solutes, belonging to different chemical classes. The analytical conditions enable the quantification of the solutes below their respective organoleptic perception thresholds in wine. The method displayed good linearity over the concentration ranges explored in wine as well as excellent repeatability (RSD below 6%) and good reproducibility (RSD below 24%). The developed methodology was applied to the analysis of several wines and showed good agreement with the results collected with headspace solid-phase microextraction (HS-SPME) or liquid-liquid extraction (LLE) followed by GC-MS or electron capture detection (ECD). Good correlation was also found between the analytical and sensory results.

  20. Comparison of four extraction methods for analysis of volatile hop-derived aroma compounds in beer.

    Science.gov (United States)

    Richter, Tobias M; Eyres, Graham T; Silcock, Patrick; Bremer, Phil J

    2017-09-09

    The volatile organic compound profile in beer is derived from hops, malt, yeast, and interactions between the ingredients, making it very diverse and complex. Due to the range and diversity of the volatile organic compounds present, the choice of the extraction method is extremely important for optimal sensitivity and selectivity. This study compared four extraction methods for hop-derived compounds in beer late hopped with Nelson Sauvin. Extraction capacity and variation were compared for headspace solid phase micro extraction, stir bar sorptive extraction, headspace sorptive extraction, and solvent assisted flavour evaporation. Generally, stir bar sorptive extraction was better suited for acids, headspace sorptive extraction for esters and aldehydes, while headspace solid phase micro extraction was less sensitive overall, extracting 40% fewer compounds. Solvent assisted flavour evaporation with dichloromethane was not suitable for the extraction of hop-derived volatile organic compounds in beer, as the profile was strongly skewed towards alcohols and acids. Overall, headspace sorptive extraction found to be best suited, closely followed by stir bar sorptive extraction. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  1. Passive sampling and stir bar sorptive extraction for the determination of endocrine-disrupting compounds in water by GC-MS.

    Science.gov (United States)

    Magi, Emanuele; Di Carro, Marina; Liscio, Camilla

    2010-06-01

    A new method using the extraction and preconcentration capabilities of stir bar sorptive extraction, combined with high-resolution gas chromatography and mass spectrometry, was developed for the determination of five selected endocrine-disrupting compounds (4-n-nonylphenol, bisphenol A, estrone, 17beta-estradiol, and 17alpha-ethinylestradiol) in water. In situ derivatization to transform the phenolic compounds into lipophilic and volatile analytes was carried out with acetic anhydride. Two different methods of headspace derivatization to further improve the chromatographic properties of 17beta-estradiol and 17alpha-ethinylestradiol were developed and compared. The optimized method provided good sensitivity (limits of quantitation 1.2-2.6 ng), repeatability (relative standard deviation 2-9%), and reproducibility (relative standard deviation 10-17%). Passive sampling by means of polar organic chemical integrative samplers was applied to monitor river waters used as supply sources for drinking water treatment plants in the Liguria region of Italy. The analytes showed a different distribution at the three sites considered; bisphenol A proved to be the most abundant, ranging from 185 to 459 ng per sampler.

  2. Automated multisyringe stir bar sorptive extraction using robust montmorillonite/epoxy-coated stir bars.

    Science.gov (United States)

    Ghani, Milad; Saraji, Mohammad; Maya, Fernando; Cerdà, Víctor

    2016-05-01

    Herein we present a simple, rapid and low cost strategy for the preparation of robust stir bar coatings based on the combination of montmorillonite with epoxy resin. The composite stir bar was implemented in a novel automated multisyringe stir bar sorptive extraction system (MS-SBSE), and applied to the extraction of four chlorophenols (4-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol) as model compounds, followed by high performance liquid chromatography-diode array detection. The different experimental parameters of the MS-SBSE, such as sample volume, selection of the desorption solvent, desorption volume, desorption time, sample solution pH, salt effect and extraction time were studied. Under the optimum conditions, the detection limits were between 0.02 and 0.34μgL(-1). Relative standard deviations (RSD) of the method for the analytes at 10μgL(-1) concentration level ranged from 3.5% to 4.1% (as intra-day RSD) and from 3.9% to 4.3% (as inter-day RSD at 50μgL(-1) concentration level). Batch-to-batch reproducibility for three different stir bars was 4.6-5.1%. The enrichment factors were between 30 and 49. In order to investigate the capability of the developed technique for real sample analysis, well water, wastewater and leachates from a solid waste treatment plant were satisfactorily analyzed.

  3. Stir bar sorptive extraction approaches with a home-made portable electric stirrer for the analysis of polycyclic aromatic hydrocarbon compounds in environmental water.

    Science.gov (United States)

    Mao, Xiangju; Hu, Bin; He, Man; Fan, Wenying

    2012-10-19

    In this study, novel off/on-site stir bar sorptive extraction (SBSE) approaches with a home-made portable electric stirrer have been developed for the analysis of polycyclic aromatic hydrocarbon compounds (PAHs). In these approaches, a miniature battery-operated electric stirrer was employed to provide agitation of sample solutions instead of the commonly used large size magnetic stirrer powered by alternating current in conventional SBSE process, which could extend the SBSE technique from the conventional off-site analysis to the on-site sampling. The applicability of the designed off/on-site SBSE sampling approaches was evaluated by polydimethylsiloxane (PDMS) coating SBSE-high performance liquid chromatography-fluorescence detection (HPLC-FLD) analysis of six target PAHs in environmental water. The home-made portable electric stirrer is simple, easy-to-operate, user friendly, low cost, easy-to-be-commercialized, and can be processed in direct immersion SBSE, headspace sorptive extraction (HSSE) and continuous flow (CF)-SBSE modes. Since the stir bar was fixed onto the portable device by magnetic force, it is very convenient to install, remove and replace the stir bar, and the coating friction loss which occurred frequently in conventional SBSE process could be avoided. The parameters affecting the extraction of six target PAHs by the home-made portable SBSE sampling device with different sampling modes were studied. Under the optimum extraction conditions, good linearity was obtained by all of three SBSE extraction modes with correlation coefficient (R) higher than 0.9971. The limits of detection (LODs, S/N=3) were 0.05-3.41 ng L(-1) for direct immersion SBSE, 0.03-2.23 ng L(-1) for HSSE and 0.09-3.75 ng L(-1) for CF-SBSE, respectively. The proposed portable PDMS-SBSE-HPLC-FLD method was applied for the analysis of six target PAHs in East Lake water, and the analytical results obtained by on-site SBSE sampling were in good agreement with that obtained by off

  4. Determination of crystal violet in water by direct solid phase spectrophotometry after rotating disk sorptive extraction.

    Science.gov (United States)

    Manzo, Valentina; Navarro, Orielle; Honda, Luis; Sánchez, Karen; Inés Toral, M; Richter, Pablo

    2013-03-15

    The microextraction of crystal violet (CV) from water samples into polydimethylsiloxane (PDMS) using the rotating disk sorptive extraction (RDSE) technique was performed. The extracting device was a small Teflon disk that had an embedded miniature magnetic stirring bar and a PDMS (560 μL) film attached to one side of the disk using double-sided tape. The extraction involves a preconcentration of CV into the PDMS, where the analyte is then directly quantified using solid phase spectrophotometry at 600 nm. Different chemical and extraction device-related variables were studied to achieve the best sensitivity for the determination. The optimum extraction was performed at pH 14 because under this condition, CV is transformed to the neutral and colorless species carbinol, which can be quantitatively transferred to the PDMS phase. Although the colorless species is the chemical form extracted in the PDMS, an intense violet coloration appeared in the phase because the -OH bond in the carbinol molecule is weakened through the formation of hydrogen bonds with the oxygen atoms of the PDMS, allowing the resonance between the three benzene rings to compensate for the charge deficit on the central carbon atom of the molecule. The accuracy and precision of the method were evaluated in river water samples spiked with 10 and 30 μg L(-1) of CV, yielding a relative standard deviation of 6.2% and 8.4% and a recovery of 98.4% and 99.4%, respectively. The method detection limit was 1.8 μg L(-1) and the limit of quantification was 5.4 μg L(-1), which can be decreased if the sample volume is increased.

  5. Stir bar sorptive extraction for the analysis of short-chain chlorinated paraffins in water.

    Science.gov (United States)

    Llorca-Porcel, Julio; Martínez-Soriano, Esther; Valor, Ignacio

    2009-05-01

    An optimised method using stir bar sorptive extraction (SBSE) and a thermal desorption-GC-electron capture detector (GC-ECD) for the determination of short-chain chlorinated paraffins from water samples was developed. Recoveries near to 100% were obtained by using 20 mm x 0.5 mm (length x film thickness) PDMS commercial stir bars from 200 mL spiked water samples and 20% methanol addition with an extraction period of 24 h. Method sensitivity, linearity and precision were evaluated for surface water and wastewater spiked samples. A LOD of 0.03 and 0.04 microg/L was calculated for surface and wastewater, respectively. The precision of the method given as an RSD was below 20% for both matrices. The developed method was applied for the analysis of two real samples from a contaminated river and a wastewater treatment plant. Results were in accordance with those obtained using a previously developed method based on solid phase microextraction (SPME).

  6. Development and application of novel clonazepam molecularly imprinted coatings for stir bar sorptive extraction.

    Science.gov (United States)

    Li, Xiaoxu; Mei, Xiaoliang; Xu, Lei; Shen, Xin; Zhu, Wanying; Hong, Junli; Zhou, Xuemin

    2016-04-15

    The molecularly imprinted magnetic stir bar coatings were created based on graft-functional Fe3O4 nanoparticles with magnetic field-induced self-assembly. The magnetic complex including clonazepam as template, the graft-functional Fe3O4 nanoparticles and methacrylic acid as monomers was pre-assembled through π-π interaction and hydrogen bonding, then was directionally adsorbed on the surface of magnetic stir bar under the magnetic induction. The molecularly imprinted coating with well-ordered structure was generated by one-step copolymerization based on the cross linking of ethylene glycol dimethacrylate. The molecularly imprinted coating with multiple recognition sites could be manufactured and applied in polar solvents, and showed superior selectivity and fast binding kinetics for benzodiazepines. The analytes in herbal health foods, treated by stir bar sorptive extraction, were determined by HPLC-UV. Good linearity was observed in the range of 0.01-2 μg mL(-1). The content of clonazepam in the herbal health foods was found to be 44 ng g(-1), and the average recoveries were 89.8-103.3% with a relative standard deviation (RSD) <6.5%, demonstrating the successful application in real sample analysis.

  7. Dynamic fabric phase sorptive extraction for a group of pharmaceuticals and personal care products from environmental waters.

    Science.gov (United States)

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

    2016-07-22

    This paper describes for the first time the use of a new extraction technique, based on fabric phase sorptive extraction (FPSE). This new mode proposes the extraction of the analytes in dynamic mode in order to reduce the extraction time. Dynamic fabric phase sorptive extraction (DFPSE) followed by liquid chromatography-tandem mass spectrometry was evaluated for the extraction of a group of pharmaceuticals and personal care products (PPCPs) from environmental water samples. Different parameters affecting the extraction were optimized and best conditions were achieved when 50mL of sample at pH 3 was passed through 3 disks and analytes retained were eluted with 10mL of ethyl acetate. The recoveries were higher than 60% for most of compounds with the exception of the most polar ones (between 8% and 38%). The analytical method was validated with environmental samples such as river water and effluent and influent wastewater, and good performance was obtained. The analysis of samples revealed the presence of some PPCPs at low ngL(-1) concentrations. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Efficient analysis of selected estrogens using fabric phase sorptive extraction and high performance liquid chromatography-fluorescence detection.

    Science.gov (United States)

    Kumar, Rajesh; Gaurav; Heena; Malik, Ashok Kumar; Kabir, Abuzar; Furton, Kenneth G

    2014-09-12

    A simple, fast and sensitive analytical method using fabric phase sorptive extraction (FPSE) followed by high performance liquid chromatography with fluorescence detection (HPLC-FLD) has been developed for efficient quantification of biologically important molecules e.g., 17α-ethynylestradiol (EE2), β-estradiol (E2) and bisphenol A (BPA). FPSE is a new sorptive extraction technique that integrates the advantages of permeable sol-gel derived hybrid organic-inorganic sorbents with flexible and permeable fabric substrates, resulting in a highly efficient and sensitive extraction media that can be introduced directly into any kind of fluidic matrix. Various factors affecting the performance of FPSE technique were optimized. The chromatographic separation was carried using mobile phase acetonitrile/methanol/water (30:15:55; v/v) at a flow rate 1.0mL/min on C18 column with fluorescence detection (λex=280nm and λem=310nm). The calibration curves of the target analytes were prepared with good correlation coefficient values (R(2)>0.992). Limit of detection (LOD) values range from 20 to 42pg/mL. The developed method was applied successfully for the analysis of estrogen molecules in urine and various kinds of aqueous samples.

  9. Stir fabric phase sorptive extraction for the determination of triazine herbicides in environmental waters by liquid chromatography.

    Science.gov (United States)

    Roldán-Pijuán, Mercedes; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel; Kabir, Abuzar; Furton, Kenneth G

    2015-01-09

    Stir fabric phase sorptive extraction (SFPSE), which integrates sol-gel hybrid organic-inorganic coated fabric phase sorptive extraction media with a magnetic stirring mechanism, is presented for the first time. Two flexible fabric substrates, cellulose and polyester were used as the host matrix for three different sorbents e.g., sol-gel poly(tetrahydrofuran), sol-gel poly(ethylene glycol), and sol-gel poly(dimethyldiphenylsiloxane). The new microextraction device has been analytically evaluated using triazine herbicides as model compounds. The factors affecting the extraction efficiency of SFPSE have been investigated and the optimal extraction conditions have been determined. Under these optimum conditions, the limits of quantification (LOQs) for sol-gel poly(ethylene glycol) coated SFPSE device in combination with UPLC-DAD for the analysis of the seven triazine herbicides were in the range of 0. 26-1.50μg/L with precision (relative standard deviation) at 2μg/L concentration ranging from 1.4-4.8% (intra-day, n=5) and 6.8-11.8% (inter-day, n=3). Enrichment factors were found between 444 and 1411 (compared to 2000 theoretical maximum). Absolute extraction recoveries were in the range of 22.2-70.5%. The developed method was applied for the determination of selected triazine herbicides from three river water samples. Relative recoveries of the target analytes, in the range from 75 to 126%, were found to be satisfactory. The combination of SFPSE with LC-MS/MS allows the improvement of the method sensitivity to the range from 0.015μg/L to 0.026μg/L with precision better than 10.8% expressed as relative standard deviation (RSD).

  10. Preparation a new sorbent based on polymeric ionic liquid for stir cake sorptive extraction of organic compounds and inorganic anions.

    Science.gov (United States)

    Huang, Xiaojia; Wang, Yulei; Hong, Qiuyun; Liu, Yi; Yuan, Dongxing

    2013-11-01

    A new multi-interaction sorbent (MIS) based on polymeric ionic liquid was prepared and used as extractive medium of stir cake sorptive extraction (SCSE). In the presence of dimethyl sulfoxide, an ionic liquid, 1-vinylbenzyl-3-methylimidazolium chloride was used as monomer to copolymerize in situ with divinylbenzene to form the MIS. The influences of the content of monomer and the porogen solvent in the polymerization mixture on the extraction performance were investigated thoroughly. The MIS was characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. Parabens and aromatic amines were used to investigate the extraction performance of MIS-SCSE for apolar and strongly polar analytes, respectively. The extraction parameters for parabens and aromatic amines were optimized. At the same time, simple and sensitive analytical methods for parabens and aromatic amines in real samples were developed by the combination of MIS-SCSE and HPLC/DAD. Some inorganic anions, such as F(-), Br(-), NO3(-), PO4(3-) and SO4(2-), were used to test the extraction performance of MIS-SCSE for anions. Results indicated that mechanism involved in the extraction of MIS is the multi-interaction modes including π-π, hydrophobic, hydrogen-bonding, dipole-dipole and anion-exchange interactions.

  11. Determination of phthalate esters in polyvinyl chloride infusion bag by stir bar sorptive extraction combined with GC.

    Science.gov (United States)

    Sun, Meng; Dai, Jinna; Wang, Xiaofan; Zhao, Xu; Bi, Kaishun; Chen, Xiaohui

    2012-12-01

    A novel, efficient, and sensitive stir bar sorptive extraction method coupled with GC for the detection of four kinds of phthalate esters in plasticized polyvinyl chloride infusion bag has been developed and validated. Some experimental parameters including stirring speed, stirring time, pH value, salt concentration, desorption mode, desorption solvents, and desorption time were investigated and optimized. Under optimum condition, the validated assay was found to be linear (r > 0.9945) and LODs were between 1.07 and 2.67 ng for the four analytes. The method exhibited excellent precision with RSD varied from 4.5 to 6.1% (n = 5). The recoveries of the four phthalate esters at two different concentrations ranged from 80.5 to 93.4%. The results showed that the validated method could meet the need of determination of targets and was successfully applied to the analysis of phthalate esters in real samples.

  12. Development of a new stir bar sorptive extraction method for the determination of medium-level volatile thiols in wine.

    Science.gov (United States)

    Elpa, Decibel; Durán-Guerrero, Enrique; Castro, Remedios; Natera, Ramón; Barroso, Carmelo G

    2014-07-01

    A fast, simple, and reliable analytical method for the determination of medium-level volatile thiols in wines is presented. Stir bar sorptive extraction using ethylene glycol-silicone coated stir bars has been used in combination with thermal desorption gas chromatography with mass spectrometry for the analysis of 4-mercapto-4-methylpentan-2-one, 2-furanmethanethiol, 3-mercaptohexyl acetate, and 3-mercaptohexanol in wine. Optimization of the extraction technique was performed using a two-level fractional factorial design. For the extraction step, the optimum conditions were: Ethylene glycol and silicone coated stir bars, pH at 3.5, sample volume of 25 mL, extraction time of 90 min, NaCl content 4.0 g, and stirring speed at 500 rpm. The optimized method achieved good linearity for all studied compounds (r(2) > 0.995) and it provided detection limits of 21.52, 0.36, 0.73, and 2.55 μg/L for 4-mercapto-4-methylpentan-2-one, 2-furanmethanethiol, 3-mercaptohexyl acetate, and 3-mercaptohexanol, respectively. It was repeatable, with precisions lower than 18% relative standard deviation for both intraday and interday repeatability. The developed procedure is suitable for the determination of these kinds of compounds when they are present at medium concentration levels. It was finally applied to real wine samples with negative aroma derived from the high concentration levels of these compounds. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Headspace single drop microextraction coupled with microwave extraction of essential oil from plant materials.

    Science.gov (United States)

    Zhai, Yujuan; Sun, Shuo; Wang, Ziming; Zhang, Yupu; Liu, He; Sun, Ye; Zhang, Hanqi; Yu, Aimin

    2011-05-01

    Headspace single drop microextraction (HS-SDME) coupled with microwave extraction (ME) was developed and applied to the extraction of the essential oil from dried Syzygium aromaticum (L.) Merr. et Perry and Cuminum cyminum L. The operational parameters, such as microdrop volume, microwave absorption medium (MAM), extraction time, and microwave power were optimized. Ten microliters of decane was used as the microextraction solvent. Ionic liquid and carbonyl iron powder were used as MAM. The extraction time was less than 7 min at the microwave power of 440 W. The proposed method was compared with hydrodistillation (HD). There were no obvious differences in the constituents of essential oils obtained by the two methods.

  14. 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.

  15. Quantitative Analysis of Bioactive Compounds from Aromatic Plants by Means of Dynamic Headspace Extraction and Multiple Headspace Extraction-Gas Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Omar, Jone; Olivares, Maitane; Alonso, Ibone; Vallejo, Asier; Aizpurua-Olaizola, Oier; Etxebarria, Nestor

    2016-04-01

    Seven monoterpenes in 4 aromatic plants (sage, cardamom, lavender, and rosemary) were quantified in liquid extracts and directly in solid samples by means of dynamic headspace-gas chromatography-mass spectrometry (DHS-GC-MS) and multiple headspace extraction-gas chromatography-mass spectrometry (MHSE), respectively. The monoterpenes were 1st extracted by means of supercritical fluid extraction (SFE) and analyzed by an optimized DHS-GC-MS. The optimization of the dynamic extraction step and the desorption/cryo-focusing step were tackled independently by experimental design assays. The best working conditions were set at 30 °C for the incubation temperature, 5 min of incubation time, and 40 mL of purge volume for the dynamic extraction step of these bioactive molecules. The conditions of the desorption/cryo-trapping step from the Tenax TA trap were set at follows: the temperature was increased from 30 to 300 °C at 150 °C/min, although the cryo-trapping was maintained at -70 °C. In order to estimate the efficiency of the SFE process, the analysis of monoterpenes in the 4 aromatic plants was directly carried out by means of MHSE because it did not require any sample preparation. Good linearity (r2) > 0.99) and reproducibility (relative standard deviation % <12) was obtained for solid and liquid quantification approaches, in the ranges of 0.5 to 200 ng and 10 to 500 ng/mL, respectively. The developed methods were applied to analyze the concentration of 7 monoterpenes in aromatic plants obtaining concentrations in the range of 2 to 6000 ng/g and 0.25 to 110 μg/mg, respectively.

  16. Highly selective and sensitive analysis of dopamine by molecularly imprinted stir bar sorptive extraction technique coupled with complementary molecularly imprinted polymer sensor.

    Science.gov (United States)

    Prasad, Bhim Bali; Srivastava, Amrita; Tiwari, Mahavir Prasad

    2013-04-15

    This paper reports a combination of molecularly imprinted stir bar sorptive extraction and complementary molecularly imprinted polymer-sensor for the analysis of dopamine as a biomarker of several neurodegenerative diseases occurred at ultra trace level. This exploited iniferter initiated polymerization via "surface grafting-from" approach onto magnetic stir bar (for sorptive extraction) and multiwalled carbon nanotubes-ceramic electrode (for detection). Such hyphenation helped dual pre-concentration of dopamine in aqueous, biological and pharmaceutical samples. This enabled high sensitivity to achieve the stringent limit [limit of detection: 4.9ngL(-1), RSD=2.4%, S/N=3, cerebrospinal fluid] of clinical detection, without any problems of non-specific contributions and cross-reactivity.

  17. Optimization of extraction of apple aroma by dynamic headspace and influence of saliva on extraction of volatiles.

    Science.gov (United States)

    Mehinagic, Emira; Prost, Carole; Demaimay, Michel

    2004-08-11

    The dynamic headspace procedure of aroma extraction was optimized on Gala apples (Malus domestica). Two parameters affecting the extractability of compounds were studied: temperature and purge time. The influence of artificial saliva was also included. An increase in purge time and temperature caused an increase in the extraction of volatiles from the apple matrix. The optimum point of extraction was 40 degrees C and 70 min of purge. The study also showed that the addition of saliva influenced the extraction of volatile compounds, but this effect was different from one compound to another. To verify that the headspace extracts presented a global odor representativeness of fresh apple under these conditions of extraction, eight assessors compared the odor of extracts with fresh fruit odor for three different cultivars. With regard to the sensory profiles of extracts, the optimal conditions of extraction were suitable for extraction of volatile compounds, even if cooked apple odor appeared in some extracts. The similarity marks of extracts were low but acceptable.

  18. Surface modification of Poly(tetrafluorethylene) magnetic stirring bars with plasma of hexamethyldisiloxane and its applications in the stir bar sorptive extraction technique

    OpenAIRE

    R. Baeza-Marrufo; P. Acereto-Escoffié; C. Carrera-Figueiras; D. Muñoz-Rodriguez; A. Ávila-Ortega; J. A. López-Barrera; J. Morales-Corona; Olayo-González, R.

    2012-01-01

    This paper explores the potential of plasma polymerization to modify the surface of stir bars for its use in Stir Bar Sorptive Extraction (SBSE). The modification of the poly(tetrafluoroethylene) surface of stir bars was done through plasma polymerization of hexamethyldisiloxane (30 min, 110 W and 1.4×10-1 Torr). The coating was characterized by contact angle, Fourier transform infrared spectroscopy, energy dispersive x-ray analysis and scanning electron microscopy. The modified stir bars wer...

  19. A fast stir bar sorptive extraction method for the analysis of geosmin and 2-methylisoborneol in source and drinking water.

    Science.gov (United States)

    Bauld, T; Teasdale, P; Stratton, H; Uwins, H

    2007-01-01

    The presence of unpleasant taste and odour in drinking water is an ongoing aesthetic concern for water providers worldwide. The need for a sensitive and robust method capable of analysis in both natural and treated waters is essential for early detection of taste and odour events. The purpose of this study was to develop and optimise a fast stir bar sorptive extraction (SBSE) method for the analysis of geosmin and 2-methylisoborneol (MIB) in both natural water and drinking water. Limits of detection with the optimised fast method (45 min extraction time at 60 degrees C using 24 microL stir bars) were 1.1 ng/L for geosmin and 4.2 ng/L for MIB. Relative standard deviations at the detection limits were under 17% for both compounds. Use of multiple stir bars can be used to decrease the detection limits further. The use of 25% NaCl and 5% methanol sample modifiers decreased the experimental recoveries. Likewise, addition of 1 mg/L and 1.5 mg/L NaOCI decreased the recoveries and this effect was not reversed by addition of 10% thiosulphate. The optimised method was used to measure geosmin concentrations in treated and untreated drinking water. MIB concentrations were below the detection limits in these waters.

  20. Comparative studies of the static and dynamic headspace extraction of saturated short chain aldehydes from cellulose-based packaging materials.

    Science.gov (United States)

    Wenzl, T; Lankmayr, E P

    2002-03-01

    Aldehydes in cellulose-based materials such as cardboard are derived from lipid degradation. Depending on the production- and storage conditions of the cardboard, the aldehyde content changes. Owing to their sensorial properties, accurate control of their content is obligatory. The cardboard usually exhibits strong and even varying matrix effects and considerable inhomogeneity. The comparability of results of analysis after static and dynamic headspace extraction of short chained saturated aldehydes from cellulose-based matrices was studied. In the case of the static extraction technique, special attention was given to the establishment of the headspace equilibrium, which could be reached by the addition of water as a displacer. For dynamic headspace extraction, the volatiles were purged from the matrix by an inert gas and enriched on an adsorbent trap. In theory, the extraction yield should be 100%. Since there are no certified reference materials for verification of the extraction efficiency available, confirmation was achieved by determining the total amount of analytes in the sample by means of multiple headspace extraction.In comparison to the static operation mode, the major drawbacks of the dynamic technique were found to be based on a more complex parameter string and on limitations to the extractable sample quantities, which may result in enhanced uncertainty of the measurements. Nevertheless, the results of analysis pointed out that both headspace extraction techniques are suitable for the determination of volatile aldehydes from cellulose-based materials.

  1. Effect of Subcritical Fluid Extraction on the High Quality of Headspace Oil from Jasminum sambac (L.) Aiton.

    Science.gov (United States)

    Ye, Qiuping; Jin, Xinyi; Wei, Shiqin; Zheng, Gongyu; Li, Xinlei

    2016-05-01

    Subcritical fluid extraction (SFE), as a novel method, was applied to investigate the yield, quality, and sensory evaluation of headspace oil from Jasminum sambac (L.) Aiton in comparison with petroleum ether extraction (PEE). The results indicated that the yield of the headspace oil using SFE was significantly higher (P < 0.05) than when using PEE. SFE contributed to obtaining alcohols and ethers, prevented the thermal reaction of terpenes, and reduced α-caryophyllene and β-caryophyllene in the headspace oil. The contents of linalool (21.90%) and benzyl acetate (16.31%) were higher via SFE than PEE. In addition, the sensory evaluation of SFE was superior to PEE, indicating a fresh, jasmine-like odor and green-yellow color. Thus, SFE is an improved method for obtaining natural headspace oil from jasmine flowers.

  2. Effect of Subcritical Fluid Extraction on the High Quality of Headspace Oil from Jasminum sambac (L.) Aiton.

    Science.gov (United States)

    2016-04-22

    Subcritical fluid extraction (SFE), as a novel method, was applied to investigate the yield, quality, and sensory evaluation of headspace oil from Jasminum sambac (L.) Aiton in comparison with petroleum ether extraction (PEE). The results indicated that the yield of the headspace oil using SFE was significantly higher (P < 0.05) than when using PEE. SFE contributed to obtaining alcohols and ethers, prevented the thermal reaction of terpenes, and reduced α-caryophyllene and β-caryophyllene in the headspace oil. The contents of linalool (21.90%) and benzyl acetate (16.31%) were higher via SFE than PEE. In addition, the sensory evaluation of SFE was superior to PEE, indicating a fresh, jasmine-like odor and green-yellow color. Thus, SFE is an improved method for obtaining natural headspace oil from jasmine flowers.

  3. Sorptive capacities of lipids determined by passive dosing of non-polar organic chemicals

    DEFF Research Database (Denmark)

    Jahnke, Annika; Kierkegaard, Amelie; Bolinius, Damien

    VMS), chlorobenzenes and polychlorinated biphenyls via a common headspace over an olive oil donor phase to transfer the same chemical activity into the samples; iii) sampling of EOM and olive oil controls at different time points; iv) purge-and-trap extraction of the model chemicals onto ENV+ SPE cartridges, elution...... and GC/MS analysis; v) characterization of the lipid composition in all samples via NMR. Our experiments demonstrate that the sorptive capacities of the EOM samples do not differ significantly from the olive oil controls if the EOM consists of neutral lipids only. However, the EOM samples show small...

  4. Graphene oxide/polyethyleneglycol composite coated stir bar for sorptive extraction of fluoroquinolones from chicken muscle and liver.

    Science.gov (United States)

    Fan, Wenying; He, Man; Wu, Xiaoran; Chen, Beibei; Hu, Bin

    2015-10-30

    Graphene oxide (GO) is an ideal adsorbent for polar and less polar compounds due to its hexagonal carbon network structure with oxygen-containing groups, while its strong hydrophilicity and water solubility limited its application in sample pretreatment techniques. Herein, GO was composited with polyethyleneglycol (PEG) or polyaniline (PAN) through intermolecular interactions to improve its stability, and the GO/PEG and GO/PAN composite coated stir bars were prepared by sol-gel technique. Compared with GO/PAN composite and polydimethylsiloxane (PDMS) coated stir bar, the prepared GO/PEG composite coated stir bar exhibited higher extraction efficiency for five fluoroquinolones (FQs). Based on it, a method of GO/PEG composite coated stir bar sorptive extraction (SBSE) combined with high-performance liquid chromatography-fluorescence detector (HPLC-FLD) was proposed. The factors influencing SBSE, such as sample pH, salt effect, stirring rate, extraction time, desorption solvent and desorption time, were optimized, and the analytical performance of the developed SBSE-HPLC-FLD method was evaluated. The limits of detection (LODs) for five FQs were in the range of 0.0045-0.0079μgL(-1), and the enrichment factors (EFs) were in the range of 41.5-65.5-fold (theoretical enrichment factor was 100-fold). The reproducibility was also investigated at concentrations of 0.05μgL(-1) and the relative standard deviations (RSDs, n=6) were found to be in the range of 4.6-12.1%. The proposed method was successfully applied for the determination of FQs in chicken muscle and chicken liver samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Determination of parabens in house dust by pressurised hot water extraction followed by stir bar sorptive extraction and thermal desorption-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Ramírez, Noelia; Marcé, Rosa Maria; Borrull, Francesc

    2011-09-16

    This study describes the development of a new method for determining p-hydroxybenzoic esters (parabens) in house dust. This optimised method was based on the pressurised hot water extraction (PHWE) of house dust, followed by the acetylation of the extracted parabens, stir bar sorptive extraction (SBSE) with a polydimethylsiloxane stir bar, and finally analysis using thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). The combination of SBSE and PHWE allows the analytes to be preconcentrated and extracted from the aqueous extract in a single step with minimal manipulation of the sample. Furthermore the in situ acetylation of parabens prior to SBSE improved their extraction efficiency and their GC-MS signal. The method showed recoveries of between 40 and 80%, good linearity, repeatability and reproducibility (paraben to 2.1 ng g(-1) for methyl paraben) and quantification (from 3.3 ng g(-1) for propyl paraben to 8.5 ng g(-1) for methyl paraben). The proposed method was applied to the analysis of house dust samples. All the target parabens were found in the samples. Methyl and propyl parabens were the most abundant, with concentrations up to 2440 ng g(-1) and 910 ng g(-1), respectively. The high levels of parabens found in the samples confirm the importance of determining organic contaminants in indoor environments.

  6. Analysis of Volatile Compounds from Solanumbetaceum Cav. Fruits from Panama by Head-Space Micro Extraction

    Directory of Open Access Journals (Sweden)

    Armando A. Durant

    2013-01-01

    Full Text Available The characterization of the volatile compounds of two varieties of Solanum betaceum Cav. by means of headspace solid-phase microextraction (HS-SPME coupled with gas chromatography-mass spectrometry ( GC-MS i s presented. The HS-SPME method for extraction of the volatiles compounds was optimized by using a 2 3 central composite design. Maximum extraction of volatile compounds was achieved by using a divinylbenzene-carboxen-polydimethylsiloxane (DVB/CAR/PDMS fiber, extraction temperature 76° C, incubation time 44 min, and extraction time of 46 min. The main types of compounds detected in both varieties are terpenoids, followed by aromatics, esters, and aldehydes. Golden-yellow cultivars contained higher levels of esters and terpenes, while the reddish-purple variety contained a significant amount of aromatic compounds. The data structure of the chemical information obtained as well as the relationship between variables was evaluated by means of principal component analysis and cluster analysis.

  7. SIMPLE EXTRACTION OF GAMMA-HYDROXYBUTYRATE IN HUMAN WHOLE BLOOD BY HEADSPACE SOLID-PHASE MICROEXTRACTION

    OpenAIRE

    2001-01-01

    We have developed a simple method for the extraction of gamma-hydroxybutyrate (GHB) in human whole blood using headspace solid-phase microextraction (SPME). The procedure involves the conversion of GHB to gamma-butyrolactone (GBL) with acid catalysis; gamma-valerolactone (GVL) was used as internal standard (IS). After heating a vial containing a whole blood sample with GHB and IS at 80℃ for 5 min in the presence of H3PO4 solution, a Carboxen/polydimethylsiloxane -coated fiber was exposed to t...

  8. Metsulfuron-methyl Molecularly Imprinted Stir Bar Sorptive Extraction Coupled with High Performance Liquid Chromatography for Trace Sulfonylurea Herbicides Analysis in Complex Samples

    Institute of Scientific and Technical Information of China (English)

    XU Zhi-gang; DU Zhuo; LIAN Hai-xian; HU Yu-ling; LI Gong-ke

    2012-01-01

    Metsulfuron-methyl molecularly imprinted polymer(MIP)-coated stir bar was prepared for sorptive extraction of sulfonylurea herbicides in complex samples.The MIP-coating was about 21.3 μm thickness with the relative standard deviation(RSD) of 4.4%(n=10).It was homogeneous and porous with good thermal stability and chemical stability.The extraction capability of the MIP-coating was 2.8 timcs over that of the non-imprinted polymer (NIP)-coating in hexane.The MIP-coating exhibited selective adsorption ability to the template and its analogues.The extraction conditions,including extraction solvent,desorption solvent,extraction time,desorption time and stirring speed,were optimized.A method for the determination of six sulfonylurea herbicides by MIP-coated stir bar sorptive extraction coupled with high performance liquid chromatography(HPLC) was developed.The linear range was 10-200 μg/L and the detection limits were within a range of 2.0-3.3 μg/L.It was also applied to the analysis of sulfonylurea herbicides in spiked river water,soil and rice samples.

  9. Simultaneous determination of preservatives in beverages, vinegar, aqueous sauces, and quasi-drug drinks by stir-bar sorptive extraction (SBSE) and thermal desorption GC-MS.

    Science.gov (United States)

    Ochiai, Nobuo; Sasamoto, Kikuo; Takino, Masahiko; Yamashita, Satoru; Daishima, Shigeki; Heiden, Arnd C; Hoffmann, Andreas

    2002-05-01

    A method for the simultaneous determination of seven preservatives - sorbic acid, benzoic acid, and p-hydroxybenzoic acid ethyl, isopropyl, propyl, isobutyl, and butyl esters - in beverages, vinegar, aqueous sauces, and quasi-drug drinks has been developed using the stir-bar sorptive extraction technique then thermal desorption GC-MS analysis. The extraction conditions - pH, sample volume, extraction temperature, salt addition, and extraction time - were examined. d5-Benzoic acid and p-hydroxybenzoic acid sec-butyl ester were added as surrogate internal standards to compensate for the effect of sample matrix and coexisting analytes on the sorptive extraction. The linearity of the method was good over the concentration range from 1 to 1000 microg mL(-1) for sorbic acid, 10-1000 microg mL(-1) for benzoic acid, and 0.1-100 microg mL(-1) for p-hydroxybenzoic acid ethyl, isopropyl, propyl, isobutyl, and butyl esters, and the correlation coefficients were higher than 0.9984. The limit of detection ranged from 0.015 to 3.3 microg mL(-1). The recoveries (95-105%) and precision (RSD: 0.86-6.0%) of the method were examined by analyzing a sparkling soft drink, white wine, red wine, balsamic vinegar, soy sauce, and quasi-drug drink samples fortified at the 5 to 50 microg mL(-1) level.

  10. Rapid determination of methanol content in paper materials by alkaline extraction, coupled with headspace analysis.

    Science.gov (United States)

    Zhang, Chun-Yun; Li, Ling-Ling; Chai, Xin-Sheng; Barnes, Donald G

    2014-07-11

    This study reports on a rapid method for the determination of methanol in paper-based materials by alkaline extraction, coupled with headspace analysis. Methanol partition equilibria between solid-liquid phases and vapor-liquid phases were conducted in two separate containers, from which an equation for calculating the total methanol content in the original paper sample was derived. It was found that the extraction equilibrium of methanol from solid sample could be achieved within 5min at room temperature using a high-speed disintegrator, and a subsequent neutralization step is an effective way to prevent methanol from being regenerated at high temperature during headspace equilibration. The results showed that the relative standard deviations for reproducibility tests were in the range of 1.86-6.03%, and the recoveries were in the range of 92.3-107%. The present method is simple and practical; it can be an efficient tool for quantifying the methanol content in paper-based materials and thus play an important role in the investigation of methanol migration behavior in food and beverage packaging.

  11. Sensitive determination of estrogens in environmental waters treated with polymeric ionic liquid-based stir cake sorptive extraction and liquid chromatographic analysis.

    Science.gov (United States)

    Chen, Lei; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

    2016-05-15

    A simple, sensitive and environmentally friendly method using polymeric ionic liquid-based stir cake sorptive extraction followed by high performance liquid chromatography with diode array detection (HPLC/DAD) has been developed for efficient quantification of six selected estrogens in environmental waters. To extract trace estrogens effectively, a poly (1-ally-3-vinylimidazolium chloride-co-ethylene dimethacrylate) monolithic cake was prepared and used as the sorbent of stir cake sorptive extraction (SCSE). The effects of preparation conditions of sorbent and extraction parameters of SCSE for estrogens were investigated and optimized. Under optimal conditions, the developed method showed satisfactory analytical performance for targeted analytes. Low limits of detection (S/N=3) and quantification limits (S/N=10) were achieved within the range of 0.024-0.057 µg/L and 0.08-0.19 µg/L, respectively. Good linearity of method was obtained for analytes with the correlation coefficients (R(2)) above 0.99. At the same time, satisfactory method repeatability and reproducibility was achieved in terms of intra- and inter-day precisions, respectively. Finally, the established SCSE-HPLC/DAD method was successfully applied for the determination of estrogens in different environmental water samples. Recoveries obtained for the determination of estrogens in spiked samples ranged from 71.2% to 108%, with RSDs below 10% in all cases.

  12. Determination of fluoroquinolones in environmental water and milk samples treated with stir cake sorptive extraction based on a boron-rich monolith.

    Science.gov (United States)

    Mei, Meng; Huang, Xiaojia

    2016-05-01

    In this study, a new stir cake sorptive extraction using a boron-rich monolith as the adsorbent was prepared by the in situ copolymerization of vinylboronic anhydride pyridine complex and divinylbenzene. The effect of preparation parameters, including the ratio of vinylboronic anhydride pyridine complex and divinylbenzene, monomer mixture, and porogen solvent, on extraction performance was investigated thoroughly. The physicochemical properties of the adsorbent were characterized by infrared spectroscopy, scanning electron microscopy, and mercury intrusion porosimetry. Several conditions affecting the extraction efficiency were investigated in detail. Under the optimized conditions, a convenient and sensitive method for the determination of trace fluoroquinolones residues in water and milk samples was established by coupling stir cake sorptive extraction with high-performance liquid chromatography and diode array detection. The limits of detection for the target compounds were 0.10-0.26 and 0.11-0.22 μg/L for water and milk samples, respectively. In addition, the developed method showed good linearity, repeatability, and precision. Finally, the proposed method was successfully applied for the detection of trace fluoroquinolones residues in environmental water and milk samples. Satisfactory recoveries were obtained for the determination of fluoroquinolones in spiking samples that ranged from 68.8 to 120%, with relative standard deviations below 10% in all cases.

  13. Preparation of PDMS-coated microspheres by sol-gel method for sorptive extraction of PAHs

    Institute of Scientific and Technical Information of China (English)

    Chang Guang Yang; Xiang Juan Ji; Xiao Zheng Lan

    2008-01-01

    In this paper, a novel SPME mode, PDMS-coated solid glass microspheres (SGMs), were prepared by sol-gel method. Using homemade thermal desorption unit coupled with CGC-FID, six PAHs as model analytes, the performance of the new mode was characterized. The new extractive phase exhibited high thermal stability and satisfactory extraction capability. The detection limits were 0.01-0.045 ng/mL, and the linearity was from 0.5 ng/mL to 96 ng/mL. The R.S.D.s of repeatability for retention time and peak area were all within 0.074% and 6.7%, respectively. The recoveries of the PAHs were 78-127% from the sarnples taken from river water.

  14. Preparation of a new polymeric ionic liquid-based monolith for stir cake sorptive extraction and its application in the extraction of inorganic anions.

    Science.gov (United States)

    Huang, Xiaojia; Chen, Linli; Yuan, Dongxing; Bi, Shangshang

    2012-07-27

    In this study, a novel stir cake sorptive extraction (SCSE) sorbent based on polymeric ionic liquid-based monolith (PILM) for the extraction of inorganic anions was prepared. In the presence of a porogen solvent containing 1-propanol and dimethylformamid, an ionic liquid, 1-ally-3-methylimidazolium chloride was used as monomer to copolymerize in situ with ethylene dimethacrylate to form PILM. The effect of preparation conditions such as ratio of functional monomer to cross-linker, content of porogenic solvent on the extraction efficiencies were investigated in detail. The PILM was characterized by elemental analysis, scanning electron microscopy, mercury intrusion porosimetry and infrared spectroscopy. In order to investigate the extraction capacity of PILM-SCSE for inorganic anions, the SCSE was combined with ion chromatography with conductivity detection, F(-), Cl(-), NO(2)(-), Br(-), NO(3)(-), PO(4)(3-) and SO(4)(2-) were selected as detected solutes. Several extractive parameters, including pH values in sample matrix, desorption solvent, extraction and desorption time were optimized. The results showed that under the optimum experimental conditions, low detection limits (S/N=3) and quantification limits (S/N=10) of the proposed method for the target anions were achieved within the range of 0.11-2.08 and 0.37-6.88 μg/L, respectively. The method also showed good linearity, simplicity, practicality and low cost for the extraction inorganic anions. Finally, the proposed method was successfully used to detect different water samples include commercial purified water, tab water and river water. Acceptable recoveries and satisfactory repeatability were obtained. To the best of our knowledge, this is the first to use polymeric ionic liquid to enrich inorganic anions.

  15. Miniscale Liquid-Liquid Extraction Coupled with Full Evaporation Dynamic Headspace Extraction for the Gas Chromatography/Mass Spectrometric Analysis of Polycyclic Aromatic Hydrocarbons with 4000-to-14 000-fold Enrichment.

    Science.gov (United States)

    Liew, Christina Shu Min; Li, Xiao; Lee, Hian Kee

    2016-09-20

    A new sample preparation approach of combining a miniscale version of liquid-liquid extraction (LLE), termed miniscale-LLE (msLLE), with automated full evaporation dynamic headspace extraction (FEDHS) was developed. Its applicability was demonstrated in the extraction of several polycyclic aromatic hydrocarbons (PAHs) (acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, and pyrene) from aqueous samples. In the first step, msLLE was conducted with 1.75 mL of n-hexane, and all of the extract was vaporized through a Tenax TA sorbent tube via a nitrogen gas flow, in the FEDHS step. Due to the stronger π-π interaction between the Tenax TA polymer and PAHs, only the latter, and not n-hexane, was adsorbed by the sorbent. This selectivity by the Tenax TA polymer allowed an effective concentration of PAHs while eliminating n-hexane by the FEDHS process. After that, thermal desorption was applied to the PAHs to channel them into a gas chromatography/mass spectrometric (GC/MS) system for analysis. Experimental parameters affecting msLLE (solvent volume and mixing duration) and FEDHS (temperature and duration) were optimized. The obtained results achieved low limits of detection (1.85-3.63 ng/L) with good linearity (r(2) > 0.9989) and high enrichment factors ranging from 4200 to 14 100. The optimized settings were applied to the analysis of canal water sampled from an industrial area and tap water, and this methodology was compared to stir-bar sorptive extraction (SBSE). This innovative combined extraction-concentration approach proved to be fast, effective, and efficient in determining low concentrations of PAHs in aqueous samples.

  16. Dynamic headspace: a single-step extraction for isotopic analysis of microg/L concentrations of dissolved chlorinated ethenes.

    Science.gov (United States)

    Morrill, Penny L; Lacrampe-Couloume, Georges; Lollar, Barbara Sherwood

    2004-01-01

    In this study a dynamic headspace method was developed to measure the carbon isotope values of dissolved chlorinated ethenes at microg/L concentrations. A gas chromatograph/combustion/isotope ratio mass spectrometer (GC/C/IRMS) was modified to include a headspace extraction system followed by a cryogenic trap. Extracting headspace from a 160 mL vial with 80 mL of aqueous solution and 40 g of NaCl for 8-12 min resulted in accurate and reproducible delta13C values for trichloroethene (TCE) and cis-1,2-dichloroethene (cDCE) at concentrations of 50-75 microg/L. Based on these results a conservative lower limit of quantitation of 38 microg/L can be calculated for these compounds. For more volatile compounds such as tetrachloroethene (PCE) and vinyl chloride (VC), field data analyzed using this method indicate a lower limit of quantitation in the tens of microg /L range.

  17. Water stable metal-organic framework packed microcolumn for online sorptive extraction and direct analysis of naproxen and its metabolite from urine sample.

    Science.gov (United States)

    Hu, Yuling; Song, Chaoyong; Liao, Jia; Huang, Zelin; Li, Gongke

    2013-06-14

    The metal-organic framework MIL-101 was fabricated in a polyetheretherketone (PEEK) tube as micro-trapping device, and applied to sorptive extraction of naproxen and its metabolite in urine samples. The remarkable water stability of the MIL-101 characterizes the material as being different from other moisture sensitive metal-organic framework. It is therefore suitable for extraction of pharmaceuticals from biological fluids. The adsorption isotherms in aqueous solution showed that the adsorption of naproxen on MIL-101 is endothermic. Additionally, MIL-101 exhibited higher extraction capacity to naproxen than that of C18-bonded silica and multi-walled nanotube. A specially designed in-tube sorptive extraction (ITSE) device endows the extraction process with the characteristic of rapidness, convenience, and easy of conjunction with high performance liquid chromatography (HPLC). Finally the MIL-101 based ITSE method coupled with HPLC and fluorescence detection was applied to analysis of naproxen and 6-O-desmethylnaproxen in urine samples. Parameters that influence the online extraction procedure, including pH of the sample solution, flow rate of extraction, sample volume, desorption solvents and time were investigated. The method is proved to be highly sensitive with the linear range of 0.05-6.0μgL(-1) and the limits of detection of 0.034 and 0.011μgL(-1) for naproxen and 6-O-desmethylnaproxen, respectively. The recoveries in urine samples were 85.3-98.3% for naproxen and 94.0-97.3% for 6-O-desmethylnaproxen with intra- and inter-day RSDs of 2.7-5.2% and 7.1-8.1%, respectively. Urine samples could be directly subjected to analysis without any additional sample pretreatment. The proposed method was demonstrated an efficient, flexible and versatile extraction tool which is ideally suitable for online conjunction with chromatographic methods.

  18. Trace analysis of chlorophenols in river water samples by stir bar sorptive extraction with in situ derivatization and thermal desorption-gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kawaguchi, M.; Ishii, Y.; Okanouchi, N.; Sakui, N.; Ito, R.; Inoue, K.; Nakazawa, H. [Hoshi Univ., Tokyo (Japan). Dept. of Analytical Chemistry, Faculty of Pharmaceutical Sciences; Saito, K. [Saitama Institute of Public Health, Saitama (Japan). Dioxin Research Group

    2004-09-15

    Many analytical methods for the determination of chlorophenols in water samples have been reported including gas chromatography-mass spectrometry (GC-MS). However, GC-MS was initially used for the determination of phenol compounds even though derivatization was required. The derivatization leads to sharper peaks and hence to better separation and higher sensitivity for the phenols. However, the derivatization faces the risk of contamination and hence an overestimation of chlorophenols concentration. In order to overcome these problems, in situ derivatization has been developed, which involves the simple addition of a reagent to a liquid sample. Recently, a new sorptive extraction technique that uses a stir bar coated with polydimethylsiloxane (PDMS) was developed. The technique is known as stir bar sorptive extraction (SBSE). We already reported that determination of 4-tert-octylphenol (OP) and 4-nonylphenol (NP) in river water4 and body fluid samples by using SBSE. In addition, SBSE with in situ derivatization has been successfully used in the determination of bisphenol A (BPA) in human body fluid samples6 and phenolic xenoestrogens in river water samples. The aim of this study is to determine trace amounts of chlorophenols in water samples by SBSE with in situ derivatization, followed by thermal desorption (TD)-GC-MS. The developed method was applied to determination of chlorophenols in river water samples.

  19. Rapid determination of moisture content in paper materials by multiple headspace extraction gas chromatography.

    Science.gov (United States)

    Xie, Wei-Qi; Chai, Xin-Sheng

    2016-04-22

    This paper describes a new method for the rapid determination of the moisture content in paper materials. The method is based on multiple headspace extraction gas chromatography (MHE-GC) at a temperature above the boiling point of water, from which an integrated water loss from the tested sample due to evaporation can be measured and from which the moisture content in the sample can be determined. The results show that the new method has a good precision (with the relative standard deviation <0.96%), high sensitivity (the limit of quantitation=0.005%) and good accuracy (the relative differences <1.4%). Therefore, the method is quite suitable for many uses in research and industrial applications.

  20. Headspace Solid Phase Micro Extraction Gas Chromatographic Determination of Fenthion in Human Serum

    Directory of Open Access Journals (Sweden)

    Kyriaki Machera

    2008-05-01

    Full Text Available A simple and effective analytical procedure was developed for the determination of fenthion residues in human serum samples. The sample treatment was performed using the headspace solid-phase micro extraction with polyacrylate fiber, which has the advantage to require low amount of serum (1 mL without tedious pre-treatment. The quantification of fenthion was carried out by gas chromatography-mass spectrometry and the recoveries ranged from 79 to 104% at two spiking levels for 6 replicates. Detection and quantification limits were calculated as 1.51 and 4.54 ng/mL of serum respectively. Two fenthion metabolites − fenoxon and fenthion–sulfoxide − were also identified.

  1. Determination of androgens and progestogens in environmental and biological samples using fabric phase sorptive extraction coupled to ultra-high performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Guedes-Alonso, Rayco; Ciofi, Lorenzo; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan; Bubba, Massimo Del; Kabir, Abuzar; Furton, Kenneth G

    2016-03-11

    Androgens and progestogens are two important groups of endocrine disrupting compounds (EDCs) which are implicated to produce severe detrimental impact over aquatic biota, even at very low concentrations of ngL(-1). For this reason, one of the major challenges to analytical chemists is the development of sensitive and selective extraction processes which allow the rapid and green determination of these emerging pollutants at low concentrations in environmental samples. Fabric phase sorptive extraction is a new, highly sensitive, efficient and solvent minimized technique which combine the advantages of sol-gel derived microextraction sorbents and the rich surface chemistry of cellulose fabric substrate. This process has several advantages such as minimum usage of organic solvents, short extraction times, small sample volumes and high analyte preconcentration factors. In this study, an extraction method based on sorptive fabric phase coupled to ultra-high-performance liquid chromatography tandem mass spectrometry detection (FPSE-UHPLC-MS/MS) has been developed for the determination of four progestogens and six androgens in environmental and biological samples. All the parameters involved in the extraction, such as sample volume, extraction and desorption times, desorption solvent volume and sample pH values have been optimized. The developed method provides satisfactory limits of detection (between 1.7 and 264ngL(-1)), good recoveries and low relative standard deviations (below 10% in tap and osmosis water and below 20% in wastewater and urine). Subsequently, the method was used to analyse tap water, wastewater treated with different processing technologies and urine samples. The concentrations of the detected hormones ranged from 28.3 to 227.3 ngL(-1) in water samples and from 1.1 to 3.7μgL(-1) in urine samples.

  2. Comparison of volatile constituents extracted from model grape juice and model wine by stir bar sorptive extraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Caven-Quantrill, Darren J; Buglass, Alan J

    2011-02-18

    A stir bar sorptive extraction (SBSE) method coupled with gas chromatography-mass spectrometry was optimised for the analysis of volatile components of a model wine, based on a previously optimised method used for analysis of the same components in model grape juice. The presence of ethanol in the model wine sample matrix resulted in decreased sensitivity of the method toward most of the volatile constituents. Mean percent relative recoveries and reproducibilities (%CV) were 22.8% and 7.1%, respectively, compared with 28.4% and 8.5% for model grape juice. The mean limit of detection (LoD) ratio (juice:wine) was 0.25. Similar sensitivities for the two sample matrices using this method were achieved by changing the split ratio from 20:1 (grape juice) to 5:1 (wine), giving a mean limit of detection ratio (juice:wine) of 1.0, thus allowing direct comparison of chromatograms of volatile components in the two matrices. This enabled direct comparisons of grape juices and the wines derived from them by alcoholic yeast fermentation. The influence of ethanol concentration in the range 9-15% on method sensitivity is discussed, using an overlay of the total ion chromatograms. The use of a gas saver device for the 5:1 split ratio analysis of desorbed model wine aroma compounds is discussed in terms of preventing extraneous reaction of sorbent and stationary phases with air during analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

  3. Application of a Stir Bar Sorptive Extraction sample preparation method with HPLC for soil fungal biomass determination in soils from a detrital manipulation study.

    Science.gov (United States)

    Beni, Áron; Lajtha, Kate; Kozma, János; Fekete, István

    2017-05-01

    Ergosterol is a sterol found ubiquitously in cell membranes of filamentous fungi. Although concentrations in different fungal species span the range of 2.6 to 42μg/mL of dry mass, many studies have shown a strong correlation between soil ergosterol content and fungal biomass. The analysis of ergosterol in soil therefore could be an effective tool for monitoring changes in fungal biomass under different environmental conditions. Stir Bar Sorptive Extraction (SBSE) is a new sample preparation method to extract and concentrate organic analytes from liquid samples. SBSE was here demonstrated to be a simple, fast, and cost effective method for the quantitative analysis of ergosterol from field-collected soils. Using this method we observed that soil ergosterol as a measure of fungal biomass proved to be a sensitive indicator of soil microbial dynamics that were altered by changes in plant detrital inputs to soils in a long-term field experiment.

  4. Determination of synthetic phenolic antioxidants in soft drinks by stir-bar sorptive extraction coupled to gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cacho, Juan Ignacio; Campillo, Natalia; Viñas, Pilar; Hernández-Córdoba, Manuel

    2015-01-01

    The synthetic phenolic antioxidants butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT) and tert-butyl hydroquinone (TBHQ) were pre-concentrated by stir-bar sorptive extraction and thermally desorbed (SBSE-TD) before analysis by GC-MS. Several parameters affecting the derivatisation step and both SBSE extraction and thermal desorption were carefully optimised. When the analyses of BHA and TBHQ in their acetylated, silylated and underivatised forms were compared, the best results were obtained when the in-situ derivatisation procedure with acetic anhydride was employed. Quantification was carried out using carvacrol as the internal standard, providing quantification limits of between 0.11 and 0.15 ng ml(-1), depending on the compound. Recovery assays for samples spiked at two concentration levels, 1 and 5 ng ml(-1), provided recoveries in the 81-117% range. The proposed method was applied in the analysis canned soft drinks and the analytes were found in five of the 10 samples analysed.

  5. Aptamer-functionalized stir bar sorptive extraction coupled with gas chromatography-mass spectrometry for selective enrichment and determination of polychlorinated biphenyls in fish samples.

    Science.gov (United States)

    Lin, Saichai; Gan, Ning; Zhang, Jiabin; Qiao, Li; Chen, Yinji; Cao, Yuting

    2016-01-01

    In this paper, a novel aptamer-functionalized stir bar sorptive extraction (SBSE) was developed for selective enrichment of the low abundance polychlorinated biphenyls (PCBs) from fish samples. This approach was based on the immobilization of aptamer which could recognize 2,3',5,5'-tetrachlorobiphenyl (PCB72) and 2',3',4',5,5'-pentachlorobiphenyl (PCB106) on one kind of metal-organic frameworks (Zn4O(BDC)3, MOF-5). MOF-5 as a substrate was prepared by potential-controlled cathodic electrodeposition on stainless steel. This aptamer-functionalized stir bar sorptive extraction (Apt-MOF SBSE) fiber could be facile synthesized in one-step. PCB72 and PCB106 were employed as target analytes for selective extraction by the developed method. The adsorbed targets could be desorbed easily in pH 3.0 100mM glycine-HCl buffers and then extracted by the methylene chloride. Afterwards, the detection was carried out with gas chromatography-tandem mass spectrometry (GC-MS). The Apt-MOF SBSE pretreatment coupled with GC-MS exhibited high selectivity, good binding capacity, stability and reproducibility for the detection of PCBs. It provided a linear range of 0.02-250ngmL(-1) with a good coefficient of determination (R(2)=0.9991-0.9996) and the detection limit was 0.003-0.004ngmL(-1). More importantly, the method was successfully utilized for the determination of PCBs in fish samples with good enrichment factor (1930-2304). Therefore, this new SBSE coating opens up the possibility of selective enrichment of a given target PCBs from complex fish samples.

  6. Endemic Balkan parsnip Pastinaca hirsuta: the chemical profile of essential oils, headspace volatiles and extracts.

    Science.gov (United States)

    Jovanović, Snežana Č; Jovanović, Olga P; Petrović, Goran M; Stojanović, Gordana S

    2015-04-01

    The present study for the first time reports the chemical composition of the endemic Balkan parsnip Pastinaca hirsuta Pančić essential oil and headspace (HS) volatiles, obtained from fresh roots, stems, flowers and fruits, as well as fresh fruits n-hexane and diethyl ether extracts. According to GC-MS and GC-FID analyses, β-Pinene was one of the major components of the root and stem HS volatiles (50.6-24.1%). (E)-β-Ocimene was found in a significant percentage in the stem and flowers HS volatiles (31.6-57.3%). The most abundant constituent of the fruit HS, flower and fruit essential oils and both extracts was hexyl butanoate (70.5%, 31.1%, 80.4%, 47.4% and 52.7%, respectively). Apiole, accompanied by myristicin and (Z)-falcarinol, make up over 70% of the root essential oils. γ-Palmitolactone was the major component of the stem essential oils (51.9% at the flowering stage and 45.7% at the fruiting stage). Beside esters as dominant compounds, furanocoumarins were also identified in extracts. (Dis)similarity relations of examined plant samples were also investigated by the agglomerative hierarchical cluster analysis. The obtained results show there is difference in the composition of volatile components from different plant organs, while the stage of growth mainly affects the quantitative volatiles composition.

  7. Optimization of dynamic headspace extraction of the edible red algae Palmaria palmata and identification of the volatile components.

    Science.gov (United States)

    Le Pape, Marie-Annick; Grua-Priol, Joëlle; Prost, Carole; Demaimay, Michel

    2004-02-11

    A new extraction method was applied to the volatile compounds of Palmaria palmata. Dynamic headspace was optimized according to an experimental design, and descriptive sensory analysis and intensity and similarity tests were performed for each extract to assess their respective representativeness. Results showed that extract obtained with crushed algae after a 30 min purge was the most representative. GC-MS analysis was then performed on this extract to identify the volatile components. Seven halogenated compounds, seven aldehydes, two ketones, three alcohols, and four miscellaneous compounds were identified. Among them, halogenated compounds were the most characteristic of red algae, and more particularly, iodoethane and iodopentane, which had yet been found in other seaweeds.

  8. Sensitive determination of organic acid preservatives in juices and soft drinks treated by monolith-based stir cake sorptive extraction and liquid chromatography analysis.

    Science.gov (United States)

    Lin, Fuhua; Nong, Shuyu; Huang, Xiaojia; Yuan, Dongxing

    2013-02-01

    A simple, efficient, and sensitive method for simultaneous determination of sorbic acid (SA), benzoic acid (BA), and cinnamic acid (CA) in juices and soft drinks was developed by stir cake sorptive extraction (SCSE) coupling to high-performance liquid chromatography with diode array detection. The SCSE based on polymeric ionic liquid-based monolith (PILM) as extractive medium was used to concentrate these three organic acid preservatives. Because hydrophobic and ion-exchange interactions co-contributed to the extraction, the PILM-SCSE exhibited a high extractive capability towards analytes. To obtain optimum extraction performance, several SCSE parameters were investigated and discussed, including desorption solvent, pH value, ionic strength in the sample matrix, and the extraction and desorption time. Under the optimized extraction conditions, limits of detection of 0.16, 1.08, and 0.18 μg/L (S/N=3) and quantification limits of 0.52, 3.42, and 0.61 (S/N=10) were obtained for SA, BA, and CA, respectively. The method also showed good linearity and reproducibility, as well as advantages such as simplicity, low cost, and high feasibility. Finally, the proposed method was successfully applied to the determination of SA, BA, and CA in real juices and soft drinks, and the recoveries ranged from 63.0 to 107 %.

  9. New cold-fiber headspace solid-phase microextraction device for quantitative extraction of polycyclic aromatic hydrocarbons in sediment.

    Science.gov (United States)

    Ghiasvand, Ali Reza; Hosseinzadeh, Shokouh; Pawliszyn, Janusz

    2006-08-18

    A new automated headspace solid-phase microextraction (HS-SPME) sampling device was developed, with the capability of heating the sample matrix and simultaneously cooling the fiber coating. The device was evaluated for the quantitative extraction of polycyclic aromatic hydrocarbons (PAHs) from solid matrices. The proposed device improves the efficiency of the release of analytes from the matrix, facilitates the mass transfer into the headspace and significantly increases the partition coefficients of the analytes, by creating a temperature gap between the cold-fiber (CF) coating and the hot headspace. The reliability and applicability of previously reported cold-fiber devices are significantly enhanced by this improvement. In addition, it can be easily adopted for full automation of extraction, enrichment and introduction of different samples using commercially available autosampling devices. Sand samples spiked with PAHs were used as solid matrices and the effect of different experimental parameters were studied, including the extraction temperature, extraction time, moisture content, and the effect of sonication and modifier under optimal experimental conditions, linear calibration curves were obtained in the range of 0.0009-1000 ng/g, with regression coefficients higher than 0.99 and detection limits that ranged from 0.3 to 3 pg/g. Reproducible, precise and high throughput extraction, monitoring and quantification of PAHs were achieved with the automated cold-fiber headspace solid-phase microextraction (CF-HS-SPME) device coupled to GC-flame ionization detection. Determination of PAHs in certified reference sediments using the proposed approach exhibited acceptable agreement with the standard values.

  10. Optimization of the extraction conditions of the volatile compounds from chili peppers by headspace solid phase micro-extraction.

    Science.gov (United States)

    Junior, Stanislau Bogusz; de Marchi Tavares de Melo, Arlete; Zini, Cláudia Alcaraz; Godoy, Helena Teixeira

    2011-05-27

    A method involving headspace-solid phase micro-extraction (HS-SPME), gas chromatography with flame ionization detection (GC-FID) and gas chromatography with mass spectrometry (GC-MS) was developed and optimized to investigate the volatile composition of Capsicum chili peppers. Five SPME fibers were tested for extraction: carboxen/polydimethylsiloxane (CAR/PDMS-75μm), polydimethylsiloxane (PDMS-100μm), divinylbenzene/polydimethylsiloxane (DVB/PDMS-65μm), carbowax/divinylbenzene (CW/DVB-70μm), and divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS-50/30μm), the last of which was shown to be the most efficient fiber to trap the volatile compounds. Optimization of the extraction conditions was carried out using multivariate strategies such as factorial design and response surface methodology. Eighty three compounds were identified by GC-MS when using the optimized extraction conditions, the majority of which were esters. Copyright © 2011 Elsevier B.V. All rights reserved.

  11. An Electropolymerized Pyrrole-based Coating for Stir Bar Sorptive Extraction of Btex from Water Followed by Gas Chromatography-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    Babanezhad, Esmaeil; Mirabi, Ali; Ghodrati, Roghoieh

    2012-01-01

    A stir bar sorptive extraction (SBSE) technique was developed by the use of polypyrrole (PPy) sorbent, electropolymerized on the surface of a rod, as a possible alternative to solid-phase microextraction (SPME). Liquid desorption was subsequently employed to transfer the extracted analytes into the injection port of a gas chromatogra- phy-mass spectrometry (GC-MS). The PPy sorbent including polypyrrole-dodecyl sulfate (PPy-DS) was deposited on the surface of a stainless steel rod from the corresponding aqueous electrolyte by applying a constant deposition potential. The developed method was applied to the trace level extraction of BTEX (benzene, toluene, ethylbenzene, o,p-xylene) from aqueous sample. Optimization of influential experimental conditions including the voltage of power supply, the time of PPy electrodeposition, the extraction temperature, the ionic strength and the extraction time were also investigated. The detection limits of the method under optimized conditions were in the range of 0.01-0.1 ng.mL^-1. The relative standard deviations (RSD) at a concentration level of 1 ng.mL^-1 were obtained between 8% and 13% (n=6). The calibration curves of BTEX showed linearity in the range of 0.03 to 600 ngomL 1. The proposed method was successfully applied to the extraction of some selected BTEX from river water samples and the relative recoveries were higher than 90% for all the analytes.

  12. A molecularly imprinted polymer as the sorptive phase immobilized in a rotating disk extraction device for the determination of diclofenac and mefenamic acid in wastewater

    Energy Technology Data Exchange (ETDEWEB)

    Manzo, Valentina; Ulisse, Karla [Department of Inorganic and Analytical Chemistry, Faculty of Chemical and Pharmaceutical Sciences, University of Chile, P.O. Box 653, Santiago (Chile); Rodríguez, Inés [Department of Analytical and Inorganic Chemistry, Faculty of Chemical Sciences, University of Concepción (Chile); Pereira, Eduardo, E-mail: epereira@udec.cl [Department of Analytical and Inorganic Chemistry, Faculty of Chemical Sciences, University of Concepción (Chile); Richter, Pablo, E-mail: prichter@ciq.uchile.cl [Department of Inorganic and Analytical Chemistry, Faculty of Chemical and Pharmaceutical Sciences, University of Chile, P.O. Box 653, Santiago (Chile)

    2015-08-19

    The microextraction of diclofenac and mefenamic acid from water samples was performed by using rotating disk sorptive extraction (RDSE) with molecularly imprinted polymer (MIP) as the sorptive phase. The MIP was synthesized from the monomer 1-vinylimidazol (VI) together with the cross-linker divinylbenzene (DVB) using diphenylamine as the template molecule. Scanning electron microscopy (SEM) analyses of the MIP revealed clusters of spherical particles having a narrow size distribution, with diameters of approximately 1 μm. The optimized extraction conditions involved a disk rotation velocity of 3000 rpm, an extraction time of 120 min, a sample volume of 50 mL, and a sample pH of 2 as well as 25 mg of MIP immobilized in the disk. Desorption of the extracted analytes was performed with 5 mL of methanol for 10 min. Analysis by gas chromatography-mass spectrometry (GC–MS) was carried out after derivatization of the analytes with N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide (MTBSTFA). Nonmolecularly imprinted polymer (NIP) was also synthesized for comparison. It was observed that under the same conditions, MIP extracted significantly more NSAIDs containing diphenylamine (or part of this molecule) in their structure than NIP. Higher significant differences between MIP and NIP were observed for diclofenac, mefenamic acid and paracetamol, clearly indicating the effect of the template on the extraction. Recoveries of the method were between 100 and 112%, with relative standard deviations of 5–6%. The limits of detection were between 60 and 223 ng L{sup −1}. Water samples from a wastewater treatment plant (WWTP) of Santiago de Chile, were found to contain concentrations of these acidic drugs between 1.6 and 4.3 μg L{sup −1} and between 1.4 and 3.3 μg L{sup −1} in the influent and effluent, respectively. - Highlights: • A MIP immobilized in a rotating disk sucessfully extracts NSAIDs from wastewater. • MIP had remarkably superior binding

  13. Preparation of stir cake sorptive extraction based on polymeric ionic liquid for the enrichment of benzimidazole anthelmintics in water, honey and milk samples

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yulei [State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, Siming Road, P.O. Box 1009, Xiamen 361005 (China); Zhang, Jie [Key Lab of Urban Environment and Health, Institute of Urban Environment, Chinese Academy of Sciences (China); Huang, Xiaojia, E-mail: hxj@xmu.edu.cn [State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, Siming Road, P.O. Box 1009, Xiamen 361005 (China); Yuan, Dongxing [State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, Siming Road, P.O. Box 1009, Xiamen 361005 (China)

    2014-08-20

    Highlights: • A new polymeric ionic liquid-based monolith was prepared. • The monolith was used as the extractive medium of stir cake sorptive extraction. • The SCSE–AMIIDB can extract benzimidazole anthelmintics (BAs) effectively. • A combination of SCSE–AMIIDB–LD–HPLC/DAD was developed. • The combination was applied to monitor trace BAs in water, milk and honey samples. - Abstract: In this work, a new stir cake sorptive extraction (SCSE) using polymeric ionic liquid monolith as sorbent was prepared. The sorbent was obtained by in situ copolymerization of an ionic liquid, 1-allyl-3-methylimidazolium bis[(trifluoro methyl)sulfonyl]imide (AMII) and divinylbenzene (DB) in the presence of N,N-dimethylformamide. The influence of the content of ionic liquid and the porogen in the polymerization mixture on extraction performance was studied thoroughly. The physicochemical properties of the polymeric ionic liquid were characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. The usefulness of SCSE–AMIIDB was demonstrated by the enrichment of trace benzimidazole anthelmintics. Several parameters affecting the extraction efficiency were investigated, and under the optimized conditions, a simple and effective method for the determination of trace benzimidazoles residues in water, milk and honey samples was established by coupling SCSE–AMIIDB with high performance liquid chromatography/diode array detection (SCSE–AMIIDB–HPLC/DAD). Results indicated that the limits of detection (S/N = 3) for target compounds were 0.020–0.072 μg L{sup −1}, 0.035–0.10 μg L{sup −1} and 0.026–0.076 μg L{sup −1} in water, milk and honey samples, respectively. In addition, an acceptable reproducibility was achieved by evaluating the repeatability and intermediate precision with relative standard deviations (RSD) of less than 9% and 11%, respectively. Finally, the established AMII

  14. Fabric phase sorptive extraction of selected penicillin antibiotic residues from intact milk followed by high performance liquid chromatography with diode array detection.

    Science.gov (United States)

    Samanidou, Victoria; Michaelidou, Katia; Kabir, Abuzar; Furton, Kenneth G

    2017-06-01

    Fabric phase sorptive extraction (FPSE), a novel sorbent-based microextraction method, was evaluated as a simple and rapid strategy for the extraction of four penicillin antibiotic residues (benzylpenicillin, cloxacillin, dicloxacillin and oxacillin) from cows' milk, without prior protein precipitation. Time-consuming solvent evaporation and reconstitution steps were eliminated successfully from the sample preparation workflow. FPSE utilizes a flexible fabric substrate, chemically coated with sol-gel derived, highly efficient, organic-inorganic hybrid sorbent as the extraction medium. Herein short-chain poly(ethylene glycol) provided optimum extraction sensitivity for the selected penicillins, which were analysed using an RP-HPLC method, validated according to the European Decision 657/2002/EC. The limit of quantitation was 10μg/kg for benzylpenicillin, 20μg/kg for cloxacillin, 25μg/kg dicloxacillin and 30μg/kg oxacillin. These are a similar order of magnitude with those reported in the literature and (with the exception of benzylpenicillin) are less than the maximum residue limits (MRL) set by European legislation.

  15. Quantitative 31P NMR for Simultaneous Trace Analysis of Organophosphorus Pesticides in Aqueous Media Using the Stir Bar Sorptive Extraction Method

    Science.gov (United States)

    Ansari, S.; Talebpour, Z.; Molaabasi, F.; Bijanzadeh, H. R.; Khazaeli, S.

    2016-09-01

    The analysis of pesticides in water samples is of primary concern for quality control laboratories due to the toxicity of these compounds and their associated public health risk. A novel analytical method based on stir bar sorptive extraction (SBSE), followed by 31P quantitative nuclear magnetic resonance (31P QNMR), has been developed for simultaneously monitoring and determining four organophosphorus pesticides (OPPs) in aqueous media. The effects of factors on the extraction efficiency of OPPs were investigated using a Draper-Lin small composite design. An optimal sample volume of 4.2 mL, extraction time of 96 min, extraction temperature of 42°C, and desorption time of 11 min were obtained. The results showed reasonable linearity ranges for all pesticides with correlation coefficients greater than 0.9920. The limit of quantification (LOQ) ranged from 0.1 to 2.60 mg/L, and the recoveries of spiked river water samples were from 82 to 94% with relative standard deviation (RSD) values less than 4%. The results show that this method is simple, selective, rapid, and can be applied to other sample matrices.

  16. Water-compatible graphene oxide/molecularly imprinted polymer coated stir bar sorptive extraction of propranolol from urine samples followed by high performance liquid chromatography-ultraviolet detection.

    Science.gov (United States)

    Fan, Wenying; He, Man; You, Linna; Zhu, Xuewei; Chen, Beibei; Hu, Bin

    2016-04-22

    Due to the high selectivity and stability, molecularly imprinted polymers (MIPs) have been successfully applied in stir bar sorptive extraction (SBSE) as a special coating to improve the selective extraction capability for target analytes. However, traditional MIPs usually suffer from incompatibility in aqueous media and low adsorption capacity, which limit the application of MIP coated stir bar in aqueous samples. To solve these problems, a water-compatible graphene oxides (GO)/MIP composite coated stir bar was prepared in this work by in situ polymerization. The prepared water-compatible GO/MIP coated stir bar presented good mechanical strength and chemical stability, and its recognition ability in aqueous samples was improved due to the polymerization of MIP in water environment, the adsorption capacity for target analytes was also increased by the addition of GO in MIP pre-polymer solution. Based on it, a method of water-compatible GO/MIP coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detector (HPLV-UV) was proposed for the analysis of propranolol (PRO) in aqueous solution. The influencing factors of SBSE, such as sample pH, salt effect, stirring rate, extraction time, desorption solvent and desorption time, were optimized, and the analytical performance of the developed SBSE-HPLC-UV method was evaluated under the optimized conditions. The limit of detection (LOD) of the proposed method for PRO was about 0.37 μg L(-1), and the enrichment factor (EF) was 59.7-fold (theoretical EF was 100-fold). The reproducibility was also investigated at concentrations of 5 μg L(-1) and the relative standard deviation (RSD) was found to be 7.3% (n=7). The proposed method of GO/MIP coating-SBSE-HPLC-UV was successfully applied for the assay of the interested PRO drug in urine samples, and further extended to the investigation of the excretion of the drugs by monitoring the variation of the concentration of PRO in urine

  17. Polydimethylsiloxane/covalent triazine frameworks coated stir bar sorptive extraction coupled with high performance liquid chromatography-ultraviolet detection for the determination of phenols in environmental water samples.

    Science.gov (United States)

    Zhong, Cheng; He, Man; Liao, Huaping; Chen, Beibei; Wang, Cheng; Hu, Bin

    2016-04-08

    In this work, covalent triazine frameworks (CTFs) were introduced in stir bar sorptive extraction (SBSE) and a novel polydimethylsiloxane(PDMS)/CTFs stir bar coating was prepared by sol-gel technique for the sorptive extraction of eight phenols (including phenol, 2-chlorophenol, 2-nitrophenol, 4-nitrophenol, 2,4-dimethylphenol, p-chloro-m-cresol and 2,4-dichlorophenol, 2,4,6-trichlorophenol) from environmental water samples followed by high performance liquid chromatography-ultraviolet (HPLC-UV) detection. The prepared PDMS/CTFs coated stir bar showed good preparation reproducibility with the relative standard deviations (RSDs) ranging from 3.5 to 5.7% (n=7) in one batch, and from 3.7 to 9.3% (n=7) among different batches. Several parameters affecting SBSE of eight target phenols including extraction time, stirring rate, sample pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.08-0.30 μg/L. The linear range was 0.25-500 μg/L for 2-nitrophenol, 0.5-500 μg/L for phenol, 2-chlorophenol, 4-nitrophenol as well as 2,4-dimethylphenol, and 1-500 μg/L for p-chloro-m-cresol, 2,4-dichlorophenol as well as 2,4,6-trichlorophenol, respectively. The intra-day relative standard deviations (RSDs) were in the range of 4.3-9.4% (n=7, c=2 μg/L) and the enrichment factors ranged from 64.9 to 145.6 fold (theoretical enrichment factor was 200-fold). Compared with commercial PDMS coated stir bar (Gerstel) and PEG coated stir bar (Gerstel), the prepared PDMS/CTFs stir bar showed better extraction efficiency for target phenol compounds. The proposed method was successfully applied to the analysis of phenols in environmental water samples and good relative recoveries were obtained with the spiking level at 2, 10, 50 μg/L, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Simplifying sample preparation using fabric phase sorptive extraction technique for the determination of benzodiazepines in blood serum by high-performance liquid chromatography.

    Science.gov (United States)

    Samanidou, Victoria; Kaltzi, Ioanna; Kabir, Abuzar; Furton, Kenneth G

    2016-06-01

    Fabric phase sorptive extraction (FPSE), a recently introduced novel sample preparation technology, has been evaluated for the extraction of benzodiazepines from human blood serum. FPSE utilizes a flexible fabric surface as the substrate platform for creating sol-gel hybrid organic-inorganic sorbent coatings. FPSE media can be introduced directly into the sample containing the target analyte(s), requiring no need for prior sample pretreatment or clean-up. Benzodiazepines were selected as model analytes because they represent one of the most widely used therapeutic drugs in psychiatry and are also amongst the most frequently encountered drugs in forensic toxicology. The chromatographic separation of target analytes was performed on a LiChroCART-LiChrospher®100 RP-18e (5 µm, 250 × 4 mm) analytical column, operated at room temperature. Ternary gradient elution was applied with a mobile phase that consisted of acetonitrile, methanol and ammonium acetate (0.05 M), which was delivered at a flow rate of 1.0 mL/min. Diode array detection was performed with monitoring at 240 nm. FPSE was performed using cellulose fabric extraction media coated with sol-gel poly(ethylene glycol) (sol-gel PEG). Absolute recovery values in the equilibrium state for the examined benzodiazepines were found to be 27% for bromazepam, 63% for lorazepam, 42 % for diazepam and 39% for alprazolam. Copyright © 2015 John Wiley & Sons, Ltd.

  19. Comparison of different extraction methods for the determination of α- and β-thujone in sage (Salvia officinalis L.) herbal tea.

    Science.gov (United States)

    Arceusz, Agnieszka; Occhipinti, Andrea; Capuzzo, Andrea; Maffei, Massimo E

    2013-09-01

    Salvia officinalis L. (sage) is an important industrial plant used both for food and pharmaceutical purposes. The terpene fraction of this plant is responsible for many of its therapeutic and culinary properties. We used different extraction methods Tenax TA® purge and trap, headspace (HS) solid-phase microextraction, HS sorptive extraction, and stir bar sorptive extraction to analyze the terpene fraction extracted from sage tea by GC-MS. Twenty compounds were identified, including α-, β-thujone, and several other oxygenated monoterpenes (1,8-cineole, linalool, camphor, boneol, and bornyl acetate) and oxygenated sesquiterpenes (caryophyllene oxide, viridiflorol, humulene epoxide I, II, and III). Tenax TA® and HS sorptive extraction extracted a lower number of identified compounds, whereas HS solid-phase microextraction allowed the complete extraction of volatiles with particular reference to α- and β-thujone. The importance of the determination of thujones content in sage herbal tea is also discussed.

  20. Quantification of harman alkaloids in sour passion fruit pulp and seeds by a novel dual SBSE-LC/Flu (stir bar sorptive extraction-liquid chromatography with fluorescence detector) method

    OpenAIRE

    PEREIRA, Cíntia A. M.; Rodrigues,Thyago R.; YARIWAKE, Janete H.

    2014-01-01

    A method for the quantification of the alkaloids harmane and harmine in sour passion fruit (Passiflora edulis f. flavicarpa O. Degener, Passifloraceae) pulp and seeds by stir-bar sorptive extraction and high performance liquid chromatography with fluorescence detection (dual SBSE-LC/Flu) is described. The SBSE parameters were optimized using a fractional factorial design, and the dual SBSE-LC/Flu method was validated following the International Conference on Harmonisation of Technical Require...

  1. Determination of off-flavor compounds, 2-methylisoborneol and geosmin, in salmon fillets using stir bar sorptive extraction-thermal desorption coupled with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Ruan, E D; Aalhus, J L; Summerfelt, S T; Davidson, J; Swift, B; Juárez, M

    2013-12-20

    A sensitive and solvent-less method for the determination of musty and earthy off-flavor compounds, 2-methylisoborneol (MIB) and geosmin (GSM), in salmon tissue was developed using stir bar sorptive extraction-thermal desorption coupled with gas chromatography-mass spectrometry (SBSE-TD-GCMS). MIB and GSM were solid phase extracted using polydimethylsiloxane (PDMS) coated stir bars, analyzed by gas chromatography, and detected in full scan mode of mass selective detector (MSD). Using this method, the calibration curves of MIB and GSM were linear in the range of 0.3-100ng/L, with a correlation coefficient above 0.999 and RSDs less than 4% (n=4). The limit of detection (LOD, S/N=3, n=6) and limit of quantification (LOQ, S/N=10, n=6) of MIB and GSM were both ∼0.3 and 1ng/L, respectively. The recoveries of MIB and GSM were 22% and 29% by spike in 30ng/L standard compounds, 23% and 30% by spike-in 100ng/L standard compounds in salmon tissue samples with good precision (<8% of RSDs, n=6), respectively. The recoveries of MIB and GSM were better than reported methodologies using SPME fibres (<10%) in fish tissue samples. This method was successfully applied to monitor and characterize depurated salmon fillet samples (0, 3, 6 and 10 days).

  2. Stir bar sorptive extraction coupled to gas chromatography-mass spectrometry for the determination of bisphenols in canned beverages and filling liquids of canned vegetables.

    Science.gov (United States)

    Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

    2012-07-20

    This paper describes a method for the simultaneous determination of bisphenol A (BPA), bisphenol F (BPF), bisphenol Z (BPZ) and biphenol (BP), using stir bar sorptive extraction (SBSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). Several parameters affecting both extraction and thermal desorption of the SBSE stages were carefully optimized by multivariate designs. SBSE was performed with two derivatization procedures, in situ acetylation and in tube silylation, and the results were compared with those obtained when the analytes were not derivatized. The proposed method, determining the analytes as acyl derivatives, was applied to analyze commercially canned beverages, as well as the filling liquids of canned vegetables, providing detection limits of between 4.7 and 12.5 ng L⁻¹, depending on the compound. The intraday and interday precisions were lower than 6% in terms of relative standard deviation. Recovery studies at two concentration levels, 0.1 and 1 μg L⁻¹, were performed providing recoveries in the 86-122% range. The samples analyzed contained higher concentrations of BPA than of the other analytes.

  3. Extraction of formic and acetic acids from aqueous solution by dynamic headspace-needle trap extraction temperature and pH optimization.

    Science.gov (United States)

    Lou, Da-Wei; Lee, Xinqing; Pawliszyn, Janusz

    2008-08-08

    A combined method of dynamic headspace-needle trap sample preparation and gas chromatography for the determination of formic and acetic acids in aqueous solution was developed in this study. A needle extraction device coupled with a gas aspirating pump was intended to perform sampling and preconcentration of target compounds from aqueous sample before gas chromatographic analysis. The needle trap extraction (NTE) technique allows for the successful sampling of short chain fatty acids under dynamic conditions while keeping the headspace (HS) volume constant. Two important parameters, including extraction temperature and effect of acidification, have been optimized and evaluated using the needle trap device. The method detection limits for the compounds estimated were 87.2microg/L for acetic acid and 234.8microg/L for formic acid in spite of the low flame ionization detection response for formic acid and its low Henry's law constant in aqueous solution. Precision was determined based on the two real samples and ranged between 4.7 and 10.7%. The validated headspace-needle trap extraction method was also successfully applied to several environmental samples.

  4. Multi-Component Profiling of Trace Volatiles in Blood by Gas Chromatography/Mass Spectrometry with Dynamic Headspace Extraction.

    Science.gov (United States)

    Kakuta, Shoji; Yamashita, Toshiyuki; Nishiumi, Shin; Yoshida, Masaru; Fukusaki, Eiichiro; Bamba, Takeshi

    2015-01-01

    A dynamic headspace extraction method (DHS) with high-pressure injection is described. This dynamic extraction method has superior sensitivity to solid phase micro extraction, SPME and is capable of extracting the entire gas phase by purging the headspace of a vial. Optimization of the DHS parameters resulted in a highly sensitive volatile profiling system with the ability to detect various volatile components including alcohols at nanogram levels. The average LOD for a standard volatile mixture was 0.50 ng mL(-1), and the average LOD for alcohols was 0.66 ng mL(-1). This method was used for the analysis of volatile components from biological samples and compared with acute and chronic inflammation models. The method permitted the identification of volatiles with the same profile pattern as in vitro oxidized lipid-derived volatiles. In addition, the concentration of alcohols and aldehydes from the acute inflammation model samples were significantly higher than that for the chronic inflammation model samples. The different profiles between these samples could also be identified by this method. Finally, it was possible to analyze alcohols and low-molecular-weight volatiles that are difficult to analyze by SPME in high sensitivity and to show volatile profiling based on multi-volatile simultaneous analysis.

  5. Volatile flavour constituent patterns of Terras Madeirenses red wines extracted by dynamic headspace solid-phase microextraction.

    Science.gov (United States)

    Perestrelo, Rosa; Caldeira, Michael; Rodrigues, Freddy; Câmara, José S

    2008-06-01

    A suitable analytical procedure based on static headspace solid-phase microextraction (SPME) followed by thermal desorption gas chromatography-ion trap mass spectrometry detection (GC-(ITD)MS), was developed and applied for the qualitative and semi-quantitative analysis of volatile components of Portuguese Terras Madeirenses red wines. The headspace SPME method was optimised in terms of fibre coating, extraction time, and extraction temperature. The performance of three commercially available SPME fibres, viz. 100 mum polydimethylsiloxane; 85 mum polyacrylate, PA; and 50/30 mum divinylbenzene/carboxen on polydimethylsiloxane, was evaluated and compared. The highest amounts extracted, in terms of the maximum signal recorded for the total volatile composition, were obtained with a PA coating fibre at 30 degrees C during an extraction time of 60 min with a constant stirring at 750 rpm, after saturation of the sample with NaCl (30%, w/v). More than sixty volatile compounds, belonging to different biosynthetic pathways, have been identified, including fatty acid ethyl esters, higher alcohols, fatty acids, higher alcohol acetates, isoamyl esters, carbonyl compounds, and monoterpenols/C(13)-norisoprenoids.

  6. Polydimethylsiloxane/metal-organic frameworks coated stir bar sorptive extraction coupled to high performance liquid chromatography-ultraviolet detector for the determination of estrogens in environmental water samples.

    Science.gov (United States)

    Hu, Cong; He, Man; Chen, Beibei; Zhong, Cheng; Hu, Bin

    2013-10-04

    In this work, three kinds of metal-organic frameworks (MOFs), MOF-5, MOF-199 and IRMOF-3, were introduced in stir bar sorptive extraction (SBSE) and novel polydimethylsiloxane (PDMS)/MOFs (including PDMS/MOF-5, PDMS/MOF-199 and PDMS/IRMOF-3) coated stir bars were prepared by sol-gel technique. These PDMS/MOFs coatings were characterized and critically compared for the extraction of seven target estrogens (17-β-estradiol, dienestrol, diethylstilbestrol, estrone, 4-t-octylphenol, bisphenol-A and 17α-ethynylestradiol) by SBSE, and the results showed that PDMS/IRMOF-3 exhibited highest extraction efficiency. Based on the above facts, a novel method of PDMS/IRMOF-3 coating SBSE-high performance liquid chromatography ultraviolet (HPLC-UV) detection was developed for the determination of seven target estrogens in environmental waters. Several parameters affecting extraction of seven target estrogens by SBSE (PDMS/IRMOF-3) including extraction time, stirring rate, pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.15-0.35 μg/L. The linear range was 2-2,500 μg/L for 17α-ethynylestradiol and 1-2,500 μg/L for other estrogens. The relative standard deviations (RSDs) were in the range of 3.7-9.9% (n=8, c=20 μg/L) and the enrichment factors were from 30.3 to 55.6-fold (theoretical enrichment factor was 100-fold). The proposed method was successfully applied to the analysis of estrogens in environmental water samples, and quantitative recoveries were obtained for the spiking experiments.

  7. Preparation of a polymeric ionic liquid-based adsorbent for stir cake sorptive extraction of preservatives in orange juices and tea drinks.

    Science.gov (United States)

    Chen, Lei; Huang, Xiaojia

    2016-04-15

    In this study, a new polymeric ionic liquid-based adsorbent was prepared and used as the extraction medium of stir cake sorptive extraction (SCSE) of three organic acid preservatives, namely, p-hydroxybenzoic acid, sorbic acid and cinnamic acid. The adsorbent was synthesized by the copolymerization of 1-ally-3-vinylimidazolium chloride (AV) and divinylbenzene (DVB) in the presence of a porogen solvent containing 1-propanol and 1,4-butanediol. The effect of the content of monomer and the porogen solvent in the polymerization mixture on the extraction performance was investigated thoroughly. The adsorbent was characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. To obtain the optimal extraction conditions of SCSE/AVDVB for target analytes, key parameters including desorption solvent, adsorption and desorption time, ionic strength and pH value in sample matrix were studied in detail. The results showed that under the optimized conditions, the SCSE/AVDVB could extract the preservatives effectively through multiply interactions. At the same time, a simple and sensitive method by combining SCSE/AVDVB and high-performance liquid chromatography with diode array detection was developed for the simultaneous analysis of the target preservatives in orange juices and tea drinks. Low limits of detection (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target analytes were achieved within the range of 0.012-0.23 μg/L and 0.039-0.42 μg/L, respectively. The precision of the proposed method was evaluated in terms of intra- and inter-assay variability calculated as relative standard deviation (RSD), and it was found that the values were all below 10%. Finally, the proposed method was used to detect preservatives in different orange juice and tea drink samples successfully. The recoveries were in the range of 71.9-116%, and the RSDs were below 10% in the all cases.

  8. Analyses of nitrobenzene,benzene and aniline in environmental water samples by headspace solid phase micro-extraction coupled with gas chromatography-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    CHEN Ming; YIN Yongguang; TAI Chao; ZHANG Qinghua; LIU Jiyan; HU Jingtian; JIANG Guibin

    2006-01-01

    A headspace solid phase microextraction coupled with gas chromatography mass spectrometry (HS-SPME/GC-MS) method was established for analyzing nitrobenzene, benzene and aniline in environmental water samples simultaneously.Factors affecting extraction efficiency (SPME fiber selection, acidity, temperature, salt addition, extraction time, headspace, etc) were verified. Under optimal extraction conditions, the detection limits are 0.50, 0.11 and 1.00 μg/L for nitrobenzene, benzene and aniline, respectively. The results indicate that this method is capable of making sensitive and accuracy analyses on nitrobenzene, benzene and aniline in environmental water samples.

  9. In situ application of stir bar sorptive extraction as a passive sampling technique for the monitoring of agricultural pesticides in surface waters.

    Science.gov (United States)

    Assoumani, Azziz; Lissalde, Sophie; Margoum, Christelle; Mazzella, Nicolas; Coquery, Marina

    2013-10-01

    Grab sampling and automated sampling are not suitable or logistically too constraining for the monitoring of pesticides in dynamic streams located in agricultural watersheds. In this work, we applied stir bar sorptive extraction (SBSE) Twisters® directly in two small rivers of a French vineyard (herein referred to as "passive SBSE"), for periods of one or two weeks during a month, for the passive sampling of 19 agricultural pesticides. We performed qualitative and semi-quantitative comparisons of the performances of passive SBSE firstly to automated sampling coupled to analytical SBSE, and secondly to the polar organic chemical integrative sampler (POCIS), a well-known passive sampler for hydrophilic micropollutants. Applying passive SBSE in river waters allowed the quantification of more pesticides and in greater amounts than analytical SBSE as shown for samples collected concurrently. Also, passive SBSE and POCIS proved to be complementary techniques in terms of detected molecules; but only passive SBSE was able to integrate a concentration peak triggered by a quick flood event that lasted 5 h. Passive SBSE could be an interesting tool for the monitoring of moderately hydrophobic to hydrophobic organic micropollutants in changing hydrosystems. In this purpose, further studies will focus on the accumulation kinetics of target pesticides and the determination of their sampling rates. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. Use of passive stir bar sorptive extraction as a simple integrative sampling technique of pesticides in freshwaters: determination of sampling rates and lag-phases.

    Science.gov (United States)

    Assoumani, Azziz; Margoum, Christelle; Chataing, Sophie; Guillemain, Céline; Coquery, Marina

    2014-03-14

    Passive sampling represents a cost-effective approach and is more representative than grab sampling for the determination of contaminant concentrations in freshwaters. In this study, we performed the calibration of a promising tool, the passive stir bar sorptive extraction (SBSE), which has previously shown good performances for semi-quantitative monitoring of pesticides in a field study. We determined the sampling rates and lag-phases of 18 moderately hydrophobic to hydrophobic agricultural pesticides (2.18Sampling rates were between 1.3 and 121 mL d(-1) with satisfactory RSD for most pesticides (9-47%), and poor repeatability for 3 hydrophobic pesticides (59-83%). Lag-phases for all target pesticides were shorter than 2 h, demonstrating the efficiency of passive SBSE for the integration of transient concentration peaks of these contaminants in surface waters. The role of flow velocity on pesticide uptakes was investigated and we assumed a water boundary layer-controlled mass transfer for 5 pesticides with log Kow>3.3. Among these pesticides, we selected fenitrothion to evaluate its elimination, along with its deuterated analogue. Results showed 82% elimination of both compounds over the 7-day experiment and isotropic exchange for fenitrothion, making fenitrothion-d6 a promising PRC candidate for in situ applications. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Quantification approach for assessment of sparkling wine volatiles from different soils, ripening stages, and varieties by stir bar sorptive extraction with liquid desorption.

    Science.gov (United States)

    Coelho, Elisabete; Coimbra, Manuel A; Nogueira, J M F; Rocha, Sílvia M

    2009-03-01

    Stir bar sorptive extraction with liquid desorption followed by large volume injection coupled to gas chromatography-quadrupole mass spectrometry (SBSE-LD/LVI-GC-qMS) was applied for the quantification of varietal and fermentative volatiles in sparkling wines. The analytical data were performed by using suitable standards of monoterpene hydrocarbons (alpha-pinene), monoterpenols (linalool), sesquiterpenoids (E,E-farnesol, Z-nerolidol, and guaiazulene), C(13) norisoprenoids (beta-ionone), aliphatic and aromatic alcohols (hexanol and 2-phenylethanol), and esters (hexyl acetate and ethyl decanoate) as model compounds. The wine volatiles were quantified using the structurally related standards. The methodology showed good linearity over the concentration range tested, with correlation coefficients ranging from 0.950 to 0.997, and a reproducibility of 9-18%. The SBSE-LD/LVI-GC-qMS methodology allowed, in a single run, the quantification of 71 wine volatiles that can be quantified accurately at levels lower than their respective olfactory thresholds. This methodology was used for assessment of sparkling wine volatiles from different soils, ripening stages, and varieties. The variety and soil influenced significantly the volatile composition of sparkling wines; lower effect was observed for the ripening stage of grapes picked up one week before or after the maturity state.

  12. Volatile composition in raspberry cultivars grown in the Pacific Northwest determined by stir bar sorptive extraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Malowicki, Sarah M M; Martin, Robert; Qian, Michael C

    2008-06-11

    Twenty-nine volatile compounds in 'Chilliwack', 'Tulameen', 'Willamette', 'Yellow Meeker', and 'Meeker' raspberries were quantified using stir bar sorptive extraction (SBSE) paired with gas chromatography-mass spectrometry (GC-MS). Good correlation coefficients were obtained with most aroma-active compounds in raspberry, with quantification limits of 1 microg/kg. However, poor recoveries were observed for raspberry ketone and zingerone. Quantitative data showed that volatile concentrations varied for different cultivars. Large variations for alpha-ionone, beta-ionone, geraniol, linalool, and ( Z)-3-hexenol were observed in different raspberry cultivars. In addition, the volatile compositions in 'Meeker' raspberry grown at different locations also varied. The chiral isomeric ratios of raspberry ketone, alpha-ionone, alpha-pinene, linalool, terpinen-4-ol, delta-octalactone, delta-decalactone, and 6-methyl-5-hepten-2-ol were studied using a CyclosilB column. alpha-Ionone, alpha-pinene, delta-octalactone, and delta-decalactone had strong chiral isomeric preference, with more than 96% for one isomeric form. Much weaker chiral isomeric preference was observed for terpinen-4-ol, while linalool was almost a racemic mixture. Both growing locations and cultivars affect the isomeric ratio of linalool with a range of 37-51% for ( R)-linalool.

  13. Optimization of dynamic headspace extraction system for measurement of halogenated volatile organic compounds in liquid or viscous samples

    Science.gov (United States)

    Taniai, G.; Oda, H.; Kurihara, M.; Hashimoto, S.

    2010-12-01

    Halogenated volatile organic compounds (HVOCs) produced in the marine environment are thought to play a key role in atmospheric reactions, particularly those involved in the global radiation budget and the depression of tropospheric and stratospheric ozone. To evaluate HVOCs concentrations in the various natural samples, we developed an automated dynamic headspace extraction method for the determination of 15 HVOCs, such as chloromethane, bromomethane, bromoethane, iodomethane, iodoethane, bromochloromethane, 1-iodopropane, 2-iodopropane, dibromomethane, bromodichloromethane, chloroiodomethane, chlorodibromomethane, bromoiodomethane, tribromomethane, and diiodomethane. Dynamic headspace system (GERSTEL DHS) was used to purge the gas phase above samples and to trap HVOCs on the adsorbent column from the purge gas. We measured the HVOCs concentrations in the adsorbent column with gas chromatograph (Agilent 6890N)- mass spectrometer (Agilent 5975C). In dynamic headspace system, an glass tube containing Tenax TA or Tenax GR was used as adsorbent column for the collection of 15 HVOCs. The parameters for purge and trap extraction, such as purge flow rate (ml/min), purge volume (ml), incubation time (min), and agitator speed (rpm), were optimized. The detection limits of HVOCs in water samples were 1270 pM (chloromethane), 103 pM (bromomethane), 42.1 pM (iodomethane), and 1.4 to 10.2 pM (other HVOCs). The repeatability (relative standard deviation) for 15 HVOCs were < 9 % except chloromethane (16.2 %) and bromomethane (11.0 %). On the basis of the measurements for various samples, we concluded that this analytical method is useful for the determination of wide range of HVOCs with boiling points between - 24°C (chloromethane) and 181°C (diiodomethane) for the liquid or viscous samples.

  14. Polyaniline/cyclodextrin composite coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detection for the analysis of trace polychlorinated biphenyls in environmental waters.

    Science.gov (United States)

    Lei, Yun; He, Man; Chen, Beibei; Hu, Bin

    2016-04-01

    A novel polyaniline/α-cyclodextrin (PANI/α-CD) composite coated stir bar was prepared by sol-gel process for the analysis of polychlorinated biphenyls (PCBs) in this work. The preparation reproducibility of the PANI/α-CD-coated stir bar was good, with relative standard deviations (RSDs) ranging from 2.3% to 3.7% (n=7) and 2.0% to 3.8% (n=7) for bar to bar and batch to batch, respectively. Based on it, a novel method of PANI/α-CD-coated stir bar sorptive extraction (SBSE) followed by high performance liquid chromatography-ultraviolet (HPLC-UV) detection was developed for the determination of trace PCBs in environmental waters. To obtain the best extraction performance for target PCBs, several parameters affecting SBSE, such as extraction time, stirring rate, and ionic strength were investigated. Under optimal experimental conditions, the limits of detection (LODs) of the proposed method for seven PCBs were in the range of 0.048-0.22 μg/L, and the RSDs were 5.3-9.8% (n=7, c=1 μg/L). Enrichment factors (EFs) ranging from 39.8 to 68.4-fold (theoretical EF, 83.3-fold) for target analytes were achieved. The proposed method was successfully applied for the determination of seven target PCBs in Yangtze River water and East Lake water, and the recoveries were in the range of 73.0-120% for the spiked East Lake water samples and 82.7-121% for the spiked Yangtze River water samples, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Magnetic metal-organic frameworks coated stir bar sorptive extraction coupled with GC-MS for determination of polychlorinated biphenyls in fish samples.

    Science.gov (United States)

    Lin, Saichai; Gan, Ning; Qiao, Li; Zhang, Jiabin; Cao, Yuting; Chen, Yinji

    2015-11-01

    In this work, several kinds of the metal-organic framework (MOF) were evaluated the adsorption performance to PCB. Finally, MOF-5(Fe) was introduced in stir bar sorptive extraction (SBSE) as the adsorbent to extract six polychlorinated biphenyls (PCBs). Nd-Fe-B permanent magnet was employed as stir bar, which was then coated with Fe3O4-MOF-5(Fe) composite magnetic material, which was prepared by solvothermal method. The stir bar was then employed to extract and enrich six indicator PCBs (2,2',5,5'-tetrachlorobiphenyl, 2,2',4,5,5'-pentachlorobiphenyl, 2,2',3,4,4',5-hexachlorobiphenyl, 2,3,4,4,5-pentachlorobiphenyl, 2,2',4,4',5,5'-hexachlorobiphenyl, 2,2',3,4,4',5,5'-heptachlorobiphenyl) under stirring, then eluted by n-hexane under ultrasound. Its saturated adsorption amount was found to be 17.0-17.8 mg g(-1) and only 30 min were needed to reach adsorption equilibrium. The MOF-stir bar can be reused for 60 times with the recovery above 80%, which exhibited good stability. Under the optimal experimental conditions, MOF-5(Fe) based SBSE was coupled with GC-MS for detecting six PCBs. The limits of detection (S/N=3) of the developed method were 0.061-0.096 ng g(-1), with enrichment factors of 50-100 fold. And the linear ranges were 0.01-500 μg L(-1). The new method was successfully applied to assess PCBs in fish samples with satisfactory recovery ranging from 94.3% to 97.5%.

  16. Preparation of stir cake sorptive extraction based on polymeric ionic liquid for the enrichment of benzimidazole anthelmintics in water, honey and milk samples.

    Science.gov (United States)

    Wang, Yulei; Zhang, Jie; Huang, Xiaojia; Yuan, Dongxing

    2014-08-20

    In this work, a new stir cake sorptive extraction (SCSE) using polymeric ionic liquid monolith as sorbent was prepared. The sorbent was obtained by in situ copolymerization of an ionic liquid, 1-allyl-3-methylimidazolium bis[(trifluoro methyl)sulfonyl]imide (AMII) and divinylbenzene (DB) in the presence of N,N-dimethylformamide. The influence of the content of ionic liquid and the porogen in the polymerization mixture on extraction performance was studied thoroughly. The physicochemical properties of the polymeric ionic liquid were characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. The usefulness of SCSE-AMIIDB was demonstrated by the enrichment of trace benzimidazole anthelmintics. Several parameters affecting the extraction efficiency were investigated, and under the optimized conditions, a simple and effective method for the determination of trace benzimidazoles residues in water, milk and honey samples was established by coupling SCSE-AMIIDB with high performance liquid chromatography/diode array detection (SCSE-AMIIDB-HPLC/DAD). Results indicated that the limits of detection (S/N=3) for target compounds were 0.020-0.072 μg L(-1), 0.035-0.10 μg L(-1) and 0.026-0.076 μg L(-1) in water, milk and honey samples, respectively. In addition, an acceptable reproducibility was achieved by evaluating the repeatability and intermediate precision with relative standard deviations (RSD) of less than 9% and 11%, respectively. Finally, the established AMII-SCSE-HPLC/DAD method was successfully applied for the determination of benzimidazoles residues in milk, honey and environmental water samples. Recoveries obtained for the determination of benzimidazole anthelmintics in spiking samples ranged from 70.2% to 117.6%, with RSD below 12% in all cases.

  17. Determination of alkylphenols and phthalate esters in vegetables and migration studies from their packages by means of stir bar sorptive extraction coupled to gas chromatography-mass spectrometry.

    Science.gov (United States)

    Cacho, J I; Campillo, N; Viñas, P; Hernández-Córdoba, M

    2012-06-01

    This paper describes a method for the determination of three alkylphenols (APs), 4-tert-octylphenol (tOP), 4-n-octylphenol (OP) and 4-nonylphenol (NP), and six phthalate esters (PEs), dimethylphthalate (DMP), diethylphthalate (DEP), di-n-butylphthalate (DBP), n-butylbenzylphthalate (BBP), di-2-ethylhexylphthalate (DEHP) and di-n-octylphthalate (DOP), in vegetables using stir bar sorptive extraction (SBSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). Ultrasonic radiation was used to extract the analytes from the solid food matrix, and the extract obtained was preconcentrated by SBSE. The different parameters affecting both stages were carefully optimized. The method was applied to analyze commercial vegetables, in the form of plastic packed salads and canned greens, as well as the corresponding filling liquids of the canned food. Quantification of the samples was carried out against aqueous standards using an internal standard (anthracene). The analysis of a 2 g vegetable sample provided detection limits between 12.7 and 105.8 pg g⁻¹ for OP and DEHP, respectively. Migration studies from the plastic packages of the vegetables samples analyzed were carried out. DEP, DBP and DEHP were found to have migrated from the bags to the simulant and the same compounds were quantified in lettuce, corn salad, arugula, parsley and chard, at concentration levels in the 8-51 ng g⁻¹ range. However, OP and NP were found in only two vegetable samples and one filling liquid, but neither was detected in any package. The proposed method provided recoveries of 83-118%.

  18. Quantification of carbamazepine, carbamazepine-10,11-epoxide, phenytoin and phenobarbital in plasma samples by stir bar-sorptive extraction and liquid chromatography.

    Science.gov (United States)

    Queiroz, Regina Helena Costa; Bertucci, Carlo; Malfará, Wilson Roberto; Dreossi, Sônia Aparecida Carvalho; Chaves, Andréa Rodrigues; Valério, Daniel Augusto Rodrigues; Queiroz, Maria Eugênia Costa

    2008-09-29

    A sensitive and reproducible stir bar-sorptive extraction and high-performance liquid chromatography-UV detection (SBSE/HPLC-UV) method for therapeutic drug monitoring of carbamazepine, carbamazepine-10,11-epoxide, phenytoin and phenobarbital in plasma samples is described and compared with a liquid:liquid extraction (LLE/HPLC-UV) method. Important factors in the optimization of SBSE efficiency such as pH, extraction time and desorption conditions (solvents, mode magnetic stir, mode ultrasonic stir, time and number of steps) assured recoveries ranging from 72 to 86%, except for phenytoin (62%). Separation was obtained using a reverse phase C18 column with UV detection (210nm). The mobile phase consisted of water:acetonitrile (78:22, v/v). The SBSE/HPLC-UV method was linear over a working range of 0.08-40.0microgmL(-1) for carbamazepine, carbamazepine-10,11-epoxide and phenobarbital and 0.125-40.0microgmL(-1) for phenytoin, The intra-assay and inter-assay precision and accuracy were studied at three concentrations (1.0, 4.0 and 20.0microgmL(-1)). The intra-assay coefficients of variation (CVs) for all compounds were less than 8.8% and all inter-CVs were less than 10%. Limits of quantification were 0.08microgmL(-1) for carbamazepine, carbamazepine-10,11-epoxide and phenobarbital and 0.125microgmL(-1) for phenytoin. No interference of the drugs normally associated with antiepileptic drugs was observed. Based on figures of merit results, the SBSE/HPLC-UV proved adequate for antiepileptic drugs analyses from therapeutic levels. This method was successfully applied to the analysis of real samples and was as effective as the LLE/HPLC-UV method.

  19. A novel method for rapid determination of total solid content in viscous liquids by multiple headspace extraction gas chromatography.

    Science.gov (United States)

    Xin, Li-Ping; Chai, Xin-Sheng; Hu, Hui-Chao; Barnes, Donald G

    2014-09-05

    This work demonstrates a novel method for rapid determination of total solid content in viscous liquid (polymer-enriched) samples. The method is based multiple headspace extraction gas chromatography (MHE-GC) on a headspace vial at a temperature above boiling point of water. Thus, the trend of water loss from the tested liquid due to evaporation can be followed. With the limited MHE-GC testing (e.g., 5 extractions) and a one-point calibration procedure (i.e., recording the weight difference before and after analysis), the total amount of water in the sample can be determined, from which the total solid contents in the liquid can be calculated. A number of black liquors were analyzed by the new method which yielded results that closely matched those of the reference method; i.e., the results of these two methods differed by no more than 2.3%. Compared with the reference method, the MHE-GC method is much simpler and more practical. Therefore, it is suitable for the rapid determination of the solid content in many polymer-containing liquid samples.

  20. Preparation of a polymeric ionic liquid-based adsorbent for stir cake sorptive extraction of preservatives in orange juices and tea drinks

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Lei; Huang, Xiaojia, E-mail: hxj@xmu.edu.cn

    2016-04-15

    In this study, a new polymeric ionic liquid-based adsorbent was prepared and used as the extraction medium of stir cake sorptive extraction (SCSE) of three organic acid preservatives, namely, p-hydroxybenzoic acid, sorbic acid and cinnamic acid. The adsorbent was synthesized by the copolymerization of 1-ally-3-vinylimidazolium chloride (AV) and divinylbenzene (DVB) in the presence of a porogen solvent containing 1-propanol and 1,4-butanediol. The effect of the content of monomer and the porogen solvent in the polymerization mixture on the extraction performance was investigated thoroughly. The adsorbent was characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. To obtain the optimal extraction conditions of SCSE/AVDVB for target analytes, key parameters including desorption solvent, adsorption and desorption time, ionic strength and pH value in sample matrix were studied in detail. The results showed that under the optimized conditions, the SCSE/AVDVB could extract the preservatives effectively through multiply interactions. At the same time, a simple and sensitive method by combining SCSE/AVDVB and high-performance liquid chromatography with diode array detection was developed for the simultaneous analysis of the target preservatives in orange juices and tea drinks. Low limits of detection (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target analytes were achieved within the range of 0.012–0.23 μg/L and 0.039–0.42 μg/L, respectively. The precision of the proposed method was evaluated in terms of intra- and inter-assay variability calculated as relative standard deviation (RSD), and it was found that the values were all below 10%. Finally, the proposed method was used to detect preservatives in different orange juice and tea drink samples successfully. The recoveries were in the range of 71.9–116%, and the RSDs were below 10% in the all cases

  1. Determination of five booster biocides in seawater by stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Giráldez, I; Chaguaceda, E; Bujalance, M; Morales, E

    2013-01-04

    Stir bar sorptive extraction (SBSE) and thermal desorption (TD)-gas chromatography-mass spectrometry (GC-MS) have been optimized for the determination of five organic booster biocides (Chlorothalonil, Dichlofluanid, Sea-Nine 211, Irgarol 1051 and TCMTB) in seawater samples. The parameters affecting the desorption and absorption steps were investigated using 10 mL seawater samples. The optimised conditions consisted of an addition of 0.2 g mL(-1) KCl to the sample, which was extracted with 10mm length, 0.5mm film thickness stir bars coated with polydimethylsiloxane (PDMS), and stirred at 900 rpm for 90 min at room temperature (25 °C) in a vial. Desorption was carried out at 280 °C for 5 min under 50 mL min(-1) of helium flow in the splitless mode while maintaining a cryotrapping temperature of 20 °C in the programmed-temperature vaporization (PTV) injector of the GC-MS system. Finally, the PTV injector was ramped to a temperature of 280 °C and the analytes were separated in the GC and detected by MS using the selected-ion monitoring (SIM) mode. The detection limits of booster biocides were found to be in the range of 0.005-0.9 μg L(-1). The regression coefficients were higher than 0.999 for all analytes. The average recovery was higher than 72% (R.S.D.: 7-15%). All these figures of merit were established running samples in triplicate. This simple, accurate, sensitive and selective analytical method may be used for the determination of trace amounts of booster biocides in water samples from marinas.

  2. Jacket-free stir bar sorptive extraction with bio-inspired polydopamine-functionalized immobilization of cross-linked polymer on stainless steel wire.

    Science.gov (United States)

    Zhang, Zixin; Zhang, Wenpeng; Bao, Tao; Chen, Zilin

    2015-08-14

    Stainless steel wire (SSW) is a good substrate for stir bar sorptive extraction (SBSE). However, it is still a challenge to immobilize commonly used cross-linked polymers onto SSW. In this work, we present a new approach for immobilization of the cross-linked organic polymer onto SSW for jacket-free SBSE. A dopamine derivative was firstly synthesized; by introducing a mussel-inspired polydopamine process, a stable coating layer was finally generated on the surface of SSW. Secondly, the cross-linked polymer was synthesized on the polydopamine-modified SSW by using acetonitrile as the porogen, acrylamide (AA) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker and 2,2'-azobis (2-methylpropionitrile) as the initiator. A diluted pre-polymerization solution was carefully prepared to generate a thin layer of the polymer. The prepared poly(EGDMA-AA)-modified stir bar showed high stability and good tolerance toward stirring, ultrasonication, organic solvents, and strong acidic and basic conditions. Morphology and structure characterization of coatings were performed by scanning electron microscopy and Fourier transform infrared spectra, respectively. The prepared poly(EGDMA-AA)-modified stir bar showed great extraction efficiency toward protoberberines, with enrichment factors of 19-42. An SBSE-HPLC method was also developed for quantitative analysis of protoberberines. The method showed low limits of detection (0.06-0.15 ng mL(-1)), wide linear range (0.5-400 ng mL(-1)), good linearity (R≥0.9980) and good reproducibility (RSD≤3.60% for intra-day, RSD≤4.73% for inter-day). The developed method has been successfully applied to determine protoberberines in herb and rat plasma samples, with recoveries of 88.53-114.61%. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Quantitative determination of volatile organic compounds (VOC) in milk by multiple dynamic headspace extraction and GC-MS.

    Science.gov (United States)

    Ciccioli, Paolo; Brancaleoni, Enzo; Frattoni, Massimiliano; Fedele, Vincenzo; Claps, Salvatore; Signorelli, Federica

    2004-01-01

    A method for the accurate determination of volatile organic compounds (VOC) in milk samples has been developed and tested. It combines multiple dynamic headspace extraction with GC-MS. Absolute amounts of VOC in the liquid phase are obtained by determining the first order kinetic dependence of the stepwise extraction of the analytes and internal standards from the liquid matrix. Compounds released from milk were collected on a train of traps filled with different solid sorbents to cover all components having a number of carbon atoms ranging from 4 to 15. They were analysed by GC-MS after thermal desorption of VOC from the collecting traps. Quantification of VOC in milk was performed using deuterated compounds as internal standards. The method was used to follow seasonal variations of monoterpenes in goat milk and to detect the impact of air pollution on the quality of milk.

  4. Optimisation of supercritical fluid extraction of polycyclic aromatic hydrocarbons and their nitrated derivatives adsorbed on highly sorptive diesel particulate matter.

    Science.gov (United States)

    Portet-Koltalo, F; Oukebdane, K; Dionnet, F; Desbène, P L

    2009-09-28

    Supercritical fluid extraction (SFE) was performed to extract complex mixtures of polycyclic aromatic hydrocarbons (PAHs), nitrated derivatives (nitroPAHs) and heavy n-alkanes from spiked soot particulates that resulted from the incomplete combustion of diesel oils. This polluted material, resulting from combustion in a light diesel engine and collected at high temperature inside the particulate filter placed just after the engine, was particularly resistant to conventional extraction techniques, such as soxhlet extraction, and had an extraction behaviour that differed markedly from certified reference materials (SRM 1650). A factorial experimental design was performed, simultaneously modelling the influence of four SFE experimental factors on the recovery yields, i.e.: the temperature and the pressure of the supercritical fluid, the nature and the percentage of the organic modifier added to CO(2) (chloroform, tetrahydrofuran, methylene chloride), as a means to reach the optimal extraction yields for all the studied target pollutants. The results of modelling showed that the supercritical fluid pressure had to be kept at its maximum level (30 MPa) and the temperature had to be kept relatively low (75 degrees C). Under these operating conditions, adding 15% of methylene chloride to the CO(2) permitted quantitative extraction of not only light PAHs and their nitrated derivatives, but also heavy n-alkanes from the spiked soots. However, heavy polyaromatics were not quantitatively extracted from the refractory carbonaceous solid surface. As such, original organic modifiers were tested, including pyridine, which, as a strong electron donor cosolvent (15% into CO(2)), was the most successful. The addition of diethylamine to pyridine, which enhanced the electron donor character of the cosolvent, even increased the extraction yields of the heaviest PAHs, leading to a quantitative extraction of all PAHs (more than 79%) from the diesel particulate matter, with detection

  5. Multivariate analysis of the volatile components in tobacco based on infrared-assisted extraction coupled to headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Yang, Yanqin; Pan, Yuanjiang; Zhou, Guojun; Chu, Guohai; Jiang, Jian; Yuan, Kailong; Xia, Qian; Cheng, Changhe

    2016-11-01

    A novel infrared-assisted extraction coupled to headspace solid-phase microextraction followed by gas chromatography with mass spectrometry method has been developed for the rapid determination of the volatile components in tobacco. The optimal extraction conditions for maximizing the extraction efficiency were as follows: 65 μm polydimethylsiloxane-divinylbenzene fiber, extraction time of 20 min, infrared power of 175 W, and distance between the infrared lamp and the headspace vial of 2 cm. Under the optimum conditions, 50 components were found to exist in all ten tobacco samples from different geographical origins. Compared with conventional water-bath heating and nonheating extraction methods, the extraction efficiency of infrared-assisted extraction was greatly improved. Furthermore, multivariate analysis including principal component analysis, hierarchical cluster analysis, and similarity analysis were performed to evaluate the chemical information of these samples and divided them into three classifications, including rich, moderate, and fresh flavors. The above-mentioned classification results were consistent with the sensory evaluation, which was pivotal and meaningful for tobacco discrimination. As a simple, fast, cost-effective, and highly efficient method, the infrared-assisted extraction coupled to headspace solid-phase microextraction technique is powerful and promising for distinguishing the geographical origins of the tobacco samples coupled to suitable chemometrics.

  6. Sorptive extraction with in-sample acetylation for gas chromatography-mass spectrometry determination of ethylphenol species in wine samples.

    Science.gov (United States)

    Carpinteiro, I; Abuín, B; Rodríguez, I; Ramil, M; Cela, R

    2010-11-12

    An inexpensive and effective sample preparation procedure for the determination of three ethylphenolic off-flavours (4-ethylphenol, 4-ethylguaiacol and 4-ethylcathecol) in wine samples is presented. Analytes were in situ acetylated and concentrated using a disposable silicone sorbent (DSS) exposed to the diluted sample. After that, the analytes were recovered with ethyl acetate and determined by gas chromatography with mass spectrometry. The influence of different parameters (volume of acetic anhydride, basic catalyst, ionic strength, sorbent format, sampling mode and extraction time) on the efficiency of derivatization and extraction steps is discussed. Under optimized conditions, 2 mL of wine were diluted with 15 mL of an aqueous solution of potassium bicarbonate (5%, m/v) in a 22 mL vessel, containing 2 g of sodium chloride. The volume of acetic anhydride and the extraction time were set at 90 μL and 2 h, and the extraction was carried out at room temperature (20±2°C). Analytes were concentrated using a silicone disc (5 mm diameter × 0.5 mm thickness) and further desorbed with 0.2 mL of ethyl acetate. The achieved limits of quantification (LOQs), defined as the concentration of each compound providing a signal 10 times higher than the baseline noise, stayed between 5 and 15 ng mL(-1). The method provided a linear response range of up to 5000 ng mL(-1) and relative recoveries from 91% to 116%. The 4-ethylphenol off-flavour was detected in most red wine samples at concentrations of up to 2700 ng mL(-1). Copyright © 2010 Elsevier B.V. All rights reserved.

  7. β-cyclodextrin-bonded silica particles as novel sorbent for stir bar sorptive extraction of phenolic compounds.

    Science.gov (United States)

    Faraji, Hakim; Husain, Syed Waqif; Helalizadeh, Masoumeh

    2011-01-01

    A stir bar coated with β-cyclodextrin-bonded-silica (CDS) as novel sorbent has been developed and used to analyze seven phenolic compounds in aqueous samples, followed by thermal desorption and gas chromatography-mass spectrometric detection. Significant parameters affecting sorption process such as the time and temperature of sorption and desorption, ionic strength, pH and stirring rate have been optimized and discussed. The coating has a high thermal stability up to 300°C and long application lifetime (80 times). The porous structure of CDS coating provides high surface area and allows high extraction efficiency. Under the selected conditions, linearity range of 0.1-400 μg/L, limit of quantifications of 0.08-3.3 μg/L and method detection limits of 0.02-1.00 μg/L have been obtained. A satisfactory repeatability (RSD ≤ 6.5, n = 7) with good linearity (0.9975 ≤ r(2) ≤ 0.9996) of results illustrated a good performance of the present method. The recovery of different natural water samples was higher than 81.5%.

  8. A robust method for determining water-extractable alkylphenol polyethoxylates in textile products by reaction-based headspace gas chromatography.

    Science.gov (United States)

    Zhang, Shu-Xin; Chai, Xin-Sheng; Huang, Bo-Xi; Mai, Xiao-Xia

    2015-08-07

    Alkylphenol polyethoxylates (APEO), surfactants used in the production of textiles, have the potential to move from the fabric to the skin of the person wearing the clothes, posing an inherent risk of adverse health consequences. Therefore, the textile industry needs a fast, robust method for determining aqueous extractable APEO in fabrics. The currently-favored HPLC methods are limited by the presence of a mixture of analytes (due to the molecular weight distribution) and a lack of analytical standards for quantifying results. As a result, it has not been possible to reach consensus on a standard method for the determination of APEO in textiles. This paper addresses these limitations through the use of reaction-based head space-gas chromatography (HS-GC). Specifically, water is used to simulate body sweat and extract APEO. HI is then used to react the ethoxylate chains to depolymerize the chains into iodoethane that is quantified through HS-GC, providing an estimate of the average amount of APEO in the clothing. Data are presented to justify the optimal operating conditions; i.e., water extraction at 60°C for 1h and reaction with a specified amount of HI in the headspace vial at 135°C for 4h. The results show that the HS-GC method has good precision (RSDtextile and related materials. As such, the method should be a strong candidate to become a standard method for such determinations.

  9. Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

    Directory of Open Access Journals (Sweden)

    Đurović-Pejčev Rada

    2016-01-01

    Full Text Available A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME in combination with liquid-solid sample preparation (LS was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl content was perfor-med using 100 μm polydimethyl-siloxane (PDMS fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS was used for detection and quantification, obtaining relative standard deviation (RSD below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 μg kg-1 of each herbicide. Limits of detection (LOD were less than 1.2 μg kg-1 for all the studied herbicides. [Projekat Ministarstva nauke Republike Srbije, br. TR31043 i br. III43005

  10. Preparation of stir cake sorptive extraction based on poly(4-vinylbenzoic acid-divinylbenzene) monolith and its application in sensitive determination of β-agonists in milk and swine urine samples

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Xiaojia, E-mail: hxj@xmu.edu.cn; Chen, Linli; Yuan, Dongxing

    2013-11-15

    Highlights: • A new poly(4-vinylbenzoic acid-divinylbenzene) monolith was first prepared. • The porous monolith was used as sorbent of stir cake sorptive extraction. • The new sorbent could extract β-agonists effectively by multiple interactions. • Method of determination of trace β-agonists in milk and urine samples was developed. -- Abstract: In this study, a new stir cake sorptive extraction (SCSE) based on poly(4-vinylbenzoic acid-divinylbenzene) (VBADB) monolith was prepared. The effect of preparation conditions of monolith on extraction efficiencies was investigated in detail. Several characteristic techniques, such as elemental analysis, infrared spectroscopy, mercury intrusion porosimetry and scanning electron microscopy were used to characterize the monolithic material. The combination of SCSE-VBADB with high-performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS) detection was developed for sensitive determination of ultra-trace β-agonists in milk and swine urine samples. In order to obtain the optimal extraction conditions of SCSE-VBADB for β-agonists, several extractive parameters, including pH values and ionic strength in sample matrix, extraction and desorption time were optimized. Under the optimum conditions, the limits of detection (S/N = 3) for the target analytes were 0.007–0.030 μg/L in milk and 0.002–0.011 μg/L in swine urine, respectively. Excellent method reproducibility was achieved in terms of intraday and interday precisions, indicated by the RSDs of both <10.0%, respectively. Finally, the proposed method was successfully used to detect β-agonists in different milk and swine urines samples. Acceptable recoveries ranged from 50.3% to 113% and 50.1% to 92.2% for milk and swine urine samples, respectively; and the RSDs for reproducibility were less than 8.0% for target analytes in all real samples.

  11. Trace-Level Volatile Quantitation by DART-MS following Headspace Extraction - Optimization and Validation in Grapes.

    Science.gov (United States)

    Jastrzembski, Jillian A; Bee, Madeleine Y; Sacks, Gavin L

    2017-10-02

    Ambient Ionization - Mass Spectrometry (AI-MS) techniques like Direct Analysis in Real Time (DART) offer the potential for rapid quantitative analyses of trace volatiles in food matrices, but performance is generally limited by the lack of pre-concentration and extraction steps. The sensitivity and selectivity of AI-MS approaches can be improved through solid-phase microextraction (SPME) with appropriate thin-film geometries, e.g. solid phase mesh enhanced sorption from headspace (SPMESH). This work improves the SPMESH-DART-MS approach for use in food analyses, and validates the approach for trace volatile analysis for two compounds in real samples (grape macerates). SPMESH units prepared with different sorbent coatings were evaluated for their ability to extract a range of odor-active volatiles, with polydimethylsiloxane/divinylbenzene giving the most satisfactory results. In combination with high-resolution mass spectrometry (HRMS), detection limits for SPMESH-DART-MS under 4 ng/L in less than 30 s acquisition times could be achieved for some volatiles (3-isobutyl-2-methoxypyrazine (IBMP), β-damascenone). A comparison of SPMESH-DART-MS and SPME-GC-MS quantitation of linalool and IBMP demonstrates excellent agreement between the two methods using real grape samples (r2≥0.90), although linalool measurements appeared to also include isobaric interferences.

  12. Ultrasonic nebulization extraction-heating gas flow transfer-headspace single drop microextraction of essential oil from pericarp of Zanthoxylum bungeanum Maxim.

    Science.gov (United States)

    Wei, Shigang; Zhang, Huihui; Wang, Yeqiang; Wang, Lu; Li, Xueyuan; Wang, Yinghua; Zhang, Hanqi; Xu, Xu; Shi, Yuhua

    2011-07-22

    The ultrasonic nebulization extraction-heating gas flow transfer coupled with headspace single drop microextraction (UNE-HGFT-HS-SDME) was developed for the extraction of essential oil from Zanthoxylum bungeanum Maxim. The gas chromatography-mass spectrometry was applied to the determination of the constituents in the essential oil. The contents of the constituents from essential oil obtained by the proposed method were found to be more similar to those obtained by hydro-distillation (HD) than those obtained by ultrasonic nebulization extraction coupled with headspace single drop microextraction (UNE-HS-SDME). The heating gas flow was firstly used in the analysis of the essential oil to transfer the analytes from the headspace to the solvent microdrop. The relative standard deviations for determining the five major constituents were in the range from 1.5 to 6.7%. The proposed method is a fast, sensitive, low cost and small sample consumption method for the determination of the volatile and semivolatile constituents in the plant materials.

  13. Profiling of volatile compounds in APC(Min/+) mice blood by dynamic headspace extraction and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Kakuta, Shoji; Nishiumi, Shin; Yoshida, Masaru; Fukusaki, Eiichiro; Bamba, Takeshi

    2015-10-15

    Various volatile compounds as well as hydrophilic compounds exist in the blood. For example, 2-alkenals, 4-hydroxy-2-alkenals, and ketoaldehydes have been reported as oxidized lipid-derived volatiles in blood. These specific volatiles have been associated with diseases; however, multi-volatile analyses have not been performed. In this study, volatile profiling of APC(Min/+) mouse plasma by dynamic headspace extraction was performed for multi-volatile analysis. In total, 19 volatiles were detected in the plasma of mice, based on information regarding oxidized lipid-derived volatile compounds, and eight of these compounds differed significantly between normal and diseased mice. 2-Methyl-2-butanol and benzyl alcohol were previously unreported in blood samples. Furthermore, 3,5,5-trimethyl-2(5H)-furanone was only detected in normal mice. 5-Methyl-3-hexanone and benzaldehyde have been detected in subjects with gastrointestinal diseases and lung cancer, respectively. Therefore, volatile profiling can be used to detect differences between samples and to identify compounds associated with diseases.

  14. Extraction and preconcentration of residual solvents in pharmaceuticals using dynamic headspace-liquid phase microextraction and their determination by gas chromatography-flame ionization detection.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Dehghani, Hamideh; Yadeghari, Adeleh; Khoshmaram, Leila

    2017-02-01

    The present study describes a microextraction and determination method for analyzing residual solvents in pharmaceutical products using dynamic headspace-liquid phase microextraction technique followed by gas chromatography-flame ionization detection. In this method dimethyl sulfoxide (μL level) placed into a GC liner-shaped extraction vessel is used as a collection/extraction solvent. Then the liner is exposed to the headspace of a vial containing the sample solution. The effect of different parameters influencing the microextraction procedure including collection/extraction solvent type and its volume, ionic strength, extraction time, extraction temperature and concentration of NaOH solution used in dissolving the studied pharmaceuticals are investigated and optimized. Under the optimum extraction conditions, the method showed wide linear ranges between 0.5 and 5000 mg L(-1) . The other analytical parameters were obtained in the following ranges: enrichment factors 240-327, extraction recoveries 72-98% and limits of detection 0.1-0.8 mg L(-1) in solution and 0.6-3.2 μg g(-1) in solid. Relative standard deviations for the extraction of 100 mg L(-1) of each analyte were obtained in the ranges of 4-7 and 5-8% for intra-day (n = 6) and inter-day (n = 4) respectively. Finally the target analytes were determined in different samples such as erythromycin, azithromycin, cefalexin, amoxicillin and co-amoxiclav by the proposed method.

  15. Extração sortiva em barra de agitação para análise de fármacos em fluidos biológicos Stir-bar sorptive extraction for drugs analysis in biological fluids

    Directory of Open Access Journals (Sweden)

    Andréa Rodrigues Chaves

    2008-01-01

    Full Text Available A novel solventless sample preparation, stir-bar sorptive extraction (SBSE, for extraction, and sample enrichment of organic compounds from biological fluids, is described in this manuscript from principle to applications. The SBSE is based on sorptive extraction, whereby the compounds are extracted into a polymer coating, polydimethylsiloxane (PDMS, on a magnetic stirring rod. The extraction is controlled by the partitioning coefficient of drugs between the PDMS and sample matrix, and upon the sample-extraction medium phase ratio. The SBSE technique has been applied successfully, with high sensitivities, to biomedical analysis of volatiles and for semi-volatiles drugs from biological sample, including urine, plasma, and saliva. SBSE combined with in situ derivatization, drugs quite more polar (e.g. metabolites also can be analyzed.

  16. Multiple automated headspace in-tube extraction for the accurate analysis of relevant wine aroma compounds and for the estimation of their relative liquid-gas transfer rates.

    Science.gov (United States)

    Zapata, Julián; Lopez, Ricardo; Herrero, Paula; Ferreira, Vicente

    2012-11-30

    An automated headspace in-tube extraction (ITEX) method combined with multiple headspace extraction (MHE) has been developed to provide simultaneously information about the accurate wine content in 20 relevant aroma compounds and about their relative transfer rates to the headspace and hence about the relative strength of their interactions with the matrix. In the method, 5 μL (for alcohols, acetates and carbonyl alcohols) or 200 μL (for ethyl esters) of wine sample were introduced in a 2 mL vial, heated at 35°C and extracted with 32 (for alcohols, acetates and carbonyl alcohols) or 16 (for ethyl esters) 0.5 mL pumping strokes in four consecutive extraction and analysis cycles. The application of the classical theory of Multiple Extractions makes it possible to obtain a highly reliable estimate of the total amount of volatile compound present in the sample and a second parameter, β, which is simply the proportion of volatile not transferred to the trap in one extraction cycle, but that seems to be a reliable indicator of the actual volatility of the compound in that particular wine. A study with 20 wines of different types and 1 synthetic sample has revealed the existence of significant differences in the relative volatility of 15 out of 20 odorants. Differences are particularly intense for acetaldehyde and other carbonyls, but are also notable for alcohols and long chain fatty acid ethyl esters. It is expected that these differences, linked likely to sulphur dioxide and some unknown specific compositional aspects of the wine matrix, can be responsible for relevant sensory changes, and may even be the cause explaining why the same aroma composition can produce different aroma perceptions in two different wines. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. Determination of volatile compounds in Magnolia bark by microwave-assisted extraction coupled to headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Sha, Yun F; Huang, Tao M; Shen, Shun; Duan, Geng L

    2004-05-01

    A method is described for the determination of volatile compounds in Magnolia bark using microwave-assisted extraction coupled to headspace solid-phase microextraction (MAE-HS-SPME), followed by gas chromatography with mass spectrometry (GC-MS). Parameters affecting the extraction efficiency, such as sampling time and temperature, microwave irradiation power and desorption time, were investigated to achieve the optimal conditions. The result obtained was compared with that of steam distillation; only small differences existed between these two methods. Therefore, the proposed method seems to be a feasible and relatively simple, fast and solvent-free procedure for identification of essential oils in Magnolia bark.

  18. Direct Analysis of Volatile Organic Compounds in Foods by Headspace Extraction Atmospheric Pressure Chemical Ionisation Mass Spectrometry.

    Science.gov (United States)

    Perez-Hurtado, P; Palmer, E; Owen, T; Aldcroft, C; Allen, M H; Jones, J; Creaser, C S; Lindley, M R; Turner, M A; Reynolds, J C

    2017-08-30

    The rapid screening of volatile organic compounds (VOCs) by direct analysis has potential applications in the areas of food and flavour science. Currently the technique of choice for VOC analysis is gas chromatography-mass spectrometry (GC/MS). However, the long chromatographic run times and elaborate sample preparation associated with this technique have led a movement towards direct analysis techniques, such as selected ion flow tube mass spectrometry (SIFT-MS), proton transfer reaction mass spectrometry (PTR-MS) and electronic noses. The work presented here describes the design and construction of a Venturi jet-pump based modification for a compact mass spectrometer which enables the direct introduction of volatiles for qualitative and quantitative analysis. Volatile organic compounds were extracted from the headspace of heated vials into the atmospheric pressure chemical ionization source of a quadrupole mass spectrometer using a Venturi pump. Samples were analysed directly with no prior sample preparation. Principal component analysis was used to differentiate between different classes of samples RESULTS: The interface is shown to be able to routinely detect problem analytes such as fatty acids and biogenic amines without the requirement of a derivatisation step, and is shown to be able to discriminate between four different varieties of cheese with good intra and inter-day reproducibility using an unsupervised principal component analysis model. Quantitative analysis is demonstrated using indole standards with limits of detection and quantification of 0.395 μg/mL and 1.316 μg/mL, respectively. The described methodology can routinely detect highly reactive analytes such as volatile fatty acids and diamines without the need for a derivatisation step or lengthy chromatographic separations. The capability of the system was demonstrated by discriminating between different varieties of cheese and monitoring the spoilage of meats. This article is protected by

  19. Sol-gel coating of poly(ethylene glycol)-grafted multiwalled carbon nanotubes for stir bar sorptive extraction and its application to the analysis of polycyclic aromatic hydrocarbons in water.

    Science.gov (United States)

    Ekbatani Amlashi, Nadiya; Hadjmohammadi, Mohammad Reza

    2016-09-01

    Poly(ethylene glycol) grafted onto carboxyl-terminated multi-walled carbon nanotubes were prepared by the sol-gel technique as a stationary phase for stir bars. The analytical methodology included stir bar sorptive extraction with micellar desorption followed by liquid chromatography. Polycyclic aromatic hydrocarbons were used as the model compounds to evaluate the extraction performance. The extraction efficiency, for the determination of polycyclic aromatic hydrocarbons from water samples, was optimized based on a chemometrics approach. The effect of the experimental parameters on the extraction response was investigated and the optimum extraction conditions were selected. Under the optimum conditions, the proposed method showed a good linearity within the different ranges for different analytes (e.g. 0.05-500 ng/mL for phenanthrene), a square of the correlation coefficient was higher than 0.999, and an appropriate limit of detection in the range of 0.013-0.072 ng/mL. The recoveries in all cases were above 94%, with relative standard deviations below 2.4%.

  20. Coupling of multi-walled carbon nanotubes/polydimethylsiloxane coated stir bar sorptive extraction with pulse glow discharge-ion mobility spectrometry for analysis of triazine herbicides in water and soil samples.

    Science.gov (United States)

    Zou, Nan; Yuan, Chunhao; Liu, Shaowen; Han, Yongtao; Li, Yanjie; Zhang, Jialei; Xu, Xiang; Li, Xuesheng; Pan, Canping

    2016-07-29

    An analytical method based on stir bar sorptive extraction (SBSE) coupled with pulse glow discharge-ion mobility spectrometry (PGD-IMS) was developed for analysis of three triazine pesticide residues in water and soil samples. An injection port with sealing device and stir bars hold device were designed and constructed to directly position the SBSE fiber including the extracted samples into the heating device, making desorption and detection of analytes proceeded simultaneously. The extraction conditions such as SBSE solid phase material, extraction time, extraction temperature, pH value and salt concentration were optimized. Mixture of MWCNTs-COOH and PDMS were shown to be effective in enriching the triazines. The LODs and LOQs of three triazines were found to be 0.006-0.015μgkg(-1) and 0.02-0.05μgkg(-1), and the linear range was 0.05-10μgL(-1) with determination coefficients from 0.9987 to 0.9993. The SBSE-PGD-IMS method was environmentally friendly without organic solvent consumption in the entire experimental procedures, and it was demonstrated to be a commendable rapid analysis technique for analysis of triazine pesticide residues in environmental samples on site. The proposed method was applied for the analysis of real ground water, surface water and soil samples.

  1. Use of headspace mulberry paper bag micro solid phase extraction for characterization of volatile aromas of essential oils from Bulgarian rose and Provence lavender.

    Science.gov (United States)

    Won, Mi-Mi; Cha, Eun-Ju; Yoon, Ok-Kyung; Kim, Nam-Sun; Kim, Kun; Lee, Dong-Sun

    2009-01-05

    In this study, a new sampling method called headspace mulberry paper bag micro solid phase extraction (HS-MPB-mu-SPE) combined to gas chromatography-mass spectrometry has been applied for the analysis of volatile aromas of liquid essential oils from Bulgarian rose and Provence lavender. The technique uses an adsorbent (Tenax TA) contained in a mulberry paper bag, minimal amount of organic solvent. Linearities for the six-points calibration curves were excellent. LOD values were in the rage from 0.38 ng mL(-1) to 0.77 ng mL(-1). Overall, precision and recovery were generally good. Phenethyl alcohol and citronellol were the main components in the essential oil from Bulgarian rose. Linalyl acetate and linalool were the most abundant components in the essential oils from true lavender or lavandin. Additionally, the relative extraction efficiencies of proposed method have been compared with HS-SPME. The overall extraction efficiency was evaluated by the relative concentration factors (CF) of the several characteristic components. CF values by HS-MPB-mu-SPE were lower than those by headspace solid phase microextraction (HS-SPME). The HS-MPB-mu-SPE method is very simple to use, inexpensive, rapid, requires small sample amounts and solvent consumption. In addition, this method allowed combining of extraction, enrichment, and clean-up in a single step. HS-MPB-mu-SPE and GC/MS is a promising technique for the characterization of volatile aroma compounds from liquid essential oils.

  2. Sorptive extraction using polydimethylsiloxane/metal-organic framework coated stir bars coupled with high performance liquid chromatography-fluorescence detection for the determination of polycyclic aromatic hydrocarbons in environmental water samples.

    Science.gov (United States)

    Hu, Cong; He, Man; Chen, Beibei; Zhong, Cheng; Hu, Bin

    2014-08-22

    In this work, metal-organic frameworks (MOFs, Al-MIL-53-NH₂) were synthesized via the hydrothermal method, and novel polydimethylsiloxane/metal-organic framework (PDMS/MOFs, PDMS/Al-MIL-53-NH₂)-coated stir bars were prepared by the sol-gel technique. The preparation reproducibility of the PDMS/MOFs-coated stir bar was good, with relative standard deviations (RSDs) ranging from 4.8% to 14.9% (n=7) within one batch and from 6.2% to 16.9% (n=6) among different batches. Based on this fact, a new method of PDMS/MOFs-coated stir bar sorptive extraction (SBSE) and ultrasonic-assisted liquid desorption (UALD) coupled with high performance liquid chromatography-fluorescence detection (HPLC-FLD) was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. To obtain the best extraction performance for PAHs, several parameters affecting SBSE, such as extraction time, stirring rate, and extraction temperature, were investigated. Under optimal experimental conditions, wide linear ranges and good RSDs (n=7) were obtained. With enrichment factors (EFs) of 16.1- to 88.9-fold (theoretical EF, 142-fold), the limits of detection (LODs, S/N=3) of the developed method for the target PAHs were found to be in the range of 0.05-2.94 ng/L. The developed method was successfully applied to the analysis of PAHs in Yangtze River and East Lake water samples.

  3. Solvent-assisted stir bar sorptive extraction by using swollen polydimethylsiloxane for enhanced recovery of polar solutes in aqueous samples: Application to aroma compounds in beer and pesticides in wine.

    Science.gov (United States)

    Ochiai, Nobuo; Sasamoto, Kikuo; David, Frank; Sandra, Pat

    2016-07-15

    A novel solvent-assisted stir bar sorptive extraction (SA-SBSE) technique was developed for enhanced recovery of polar solutes in aqueous samples. A conventional PDMS stir bar was swollen in several solvents with log Kow ranging from 1.0 to 3.5 while stirring for 30min prior to extraction. After extraction, thermal desorption - gas chromatography - (tandem) mass spectrometry (TD-GC-(MS/)MS) or liquid desorption - large volume injection (LD-LVI)-GC-MS were performed. An initial study involved investigation of potential solvents for SA-SBSE by weighing of the residual solvent in the swollen PDMS stir bar before and after extraction. Compared to conventional SBSE, SA-SBSE using diethyl ether, methyl isobutyl ketone, dichloromethane, diisopropyl ether and toluene provided higher recoveries from water samples for test solutes with log Kow2.5. The performance of the SA-SBSE method using dichloromethane, diisopropyl ether, and cyclohexane is illustrated with analyses of aroma compounds in beer and of pesticides in wine. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

  4. Coupling stir bar sorptive extraction-dispersive liquid-liquid microextraction for preconcentration of triazole pesticides from aqueous samples followed by GC-FID and GC-MS determinations.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Djozan, Djavanshir; Nouri, Nina; Bamorowat, Mehdi; Shalamzari, Mohammad Safi

    2010-06-01

    Stir bar sorptive extraction (SBSE) combined with dispersive liquid-liquid microextraction (DLLME) has been developed as a new approach for the extraction of six triazole pesticides (penconazole, hexaconazole, diniconazole, tebuconazole, triticonazole and difenconazole) in aqueous samples prior to GC-flame ionization detection (GC-FID). A series of parameters that affect the performance of both steps were thoroughly investigated. Under optimized conditions, aqueous sample was stirred using a stir bar coated with octadecylsilane (ODS) and then target compounds on the sorbent (stir bar) were desorbed with methanol. The extract was mixed with 25 microL of 1,1,2,2-tetrachloroethane and the mixture was rapidly injected into sodium chloride solution 30% w/v. After centrifugation, an aliquot of the settled organic phase was analyzed by GC-FID. The methodology showed broad linear ranges for the six triazole pesticides studied, with correlation coefficients higher than 0.993, lower LODs and LOQs between 0.53-24.0 and 1.08-80.0 ng/mL, respectively, and suitable precision (RSD FID determination. In short, by coupling SBSE with DLLME, advantages of two methods are combined to enhance the selectivity and sensitivity of the method. This method showed higher enrichment factors (282-1792) when compared with conventional methods of sample preparation to screen pesticides in aqueous samples.

  5. Characterisation of the flavour profile from Graciano Vitis vinifera wine variety by a novel dual stir bar sorptive extraction methodology coupled to thermal desorption and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Arbulu, Maria; Sampedro, M Carmen; Sanchez-Ortega, Alicia; Gómez-Caballero, Alberto; Unceta, Nora; Goicolea, M Aranzazu; Barrio, Ramón J

    2013-05-13

    The aim of this work was to develop a new analytical technique for the study of the organoleptic compounds (flavour profile) of the Graciano Vitis vinifera wine variety. The cv. Graciano is a singular variety of red grapes with its origins in La Rioja and Navarra (northern Spain). This variety transfers an intense red colour, aroma and high acidity to musts and provides greater longevity and, consequently, a better capacity for ageing wine. A new dual-stir bar sorptive extraction approach coupled with thermal desorption (TD) and GC-MS has been used to extract the volatile and semivolatile compounds. In this extraction step, the optimal values for the experimental variables were obtained through the Response Surface Methodology (RSM). Full scan chromatogram data were evaluated with two deconvolution software tools, and the results were compared. The volatile and semivolatile components were identified with an MS match ≥80%. As a result, the flavour metabolome of the Graciano Vitis vinifera wine variety was obtained, and 205 metabolites were identified using different databases. These metabolites were grouped into esters, acids, alcohols, nitrogen compounds, furans, lactones, ketones, aldehydes, phenols, terpenes, norisoprenoids, sulphur compounds, acetals and pyrans. The majority of the metabolites observed had already been reported in the literature; however, this work also identified new, previously unreported metabolites in red wines, which may be characteristic of the Graciano variety. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Ultrasonic nebulization extraction coupled with headspace single-drop microextraction of volatile and semivolatile compounds from the seed of Cuminum cyminum L.

    Science.gov (United States)

    Zhang, Huihui; Shi, Yuhua; Wei, Shigang; Wang, Yinghua; Zhang, Hanqi

    2011-08-15

    Ultrasonic nebulization extraction (UNE) coupled with headspace single-drop microextraction (HS-SDME) was developed. In the UNE process, the analytes were transferred from the aqueous phase to the gas phase. Then the analytes were transferred from the gas phase to the solvent phase by the carrier gas and extracted and enriched with suspended microdrop solvent. Finally, the microdrop solvent injected into GC-MS system. The parameters affecting extraction performance, such as type of suspended solvent, microdrop volume, flow rate of carrier gas, temperature of extraction vessel and extraction time were investigated and optimized. The proposed method can be applied for the extraction and enrichment of the volatile and semivolatile compounds simultaneously. The extraction efficiency of the proposed method was compared with that of ultrasonic extraction (UE) and UE-HS-SDME. Compared with UE-HS-SDME, the contents of constituents in the extract obtained by the proposed method were closer to those obtained by hydrodistillation (HD), which is a standard extraction method.

  7. Direct thermal desorption in the analysis of cheese volatiles by gas chromatography and gas chromatography-mass spectrometry: comparison with simultaneous distillation-extraction and dynamic headspace.

    Science.gov (United States)

    Valero, E; Sanz, J; Martínez-Castro, I

    2001-06-01

    Direct thermal desorption (DTD) has been used as a technique for extracting volatile components of cheese as a preliminary step to their gas chromatographic (GC) analysis. In this study, it is applied to different cheese varieties: Camembert, blue, Chaumes, and La Serena. Volatiles are also extracted using other techniques such as simultaneous distillation-extraction and dynamic headspace. Separation and identification of the cheese components are carried out by GC-mass spectrometry. Approximately 100 compounds are detected in the examined cheeses. The described results show that DTD is fast, simple, and easy to automate; requires only a small amount of sample (approximately 50 mg); and affords quantitative information about the main groups of compounds present in cheeses.

  8. pH-resistant titania hybrid organic-inorganic coating for stir bar sorptive extraction of drugs of abuse in urine samples followed by high performance liquid chromatography-ultraviolet visible detection.

    Science.gov (United States)

    Lan, Lidan; Hu, Bin; Yu, Chunhe

    2010-11-05

    An organic-inorganic hybrid titania-hydroxy-terminated silicone oil (titania-OH-TSO) stir bar coating was prepared by sol-gel method. The extraction performance of titania-OH-TSO coated stir bar was evaluated and compared with poly(dimethysiloxane) (PDMS), poly(dimethysiloxane)-divinylbenzene (PDMS-DVB), poly(dimethysiloxane)-β-cyclodextrin (PDMS-β-CD) and C(18) coated stir bar with five polar drugs of abuse including amphetamine (PA), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and ketamine (Ke) as the model analytes. The experimental results revealed that the titania-OH-TSO coated stir bar exhibited highly pH-resistant ability, good preparation reproducibility, superior selectivity and high extraction efficiency for the target compounds. Based on this fact, a new method of titania-OH-TSO coated stir bar sorptive extraction (SBSE) combined with high performance liquid chromatography (HPLC)-ultraviolet visible (UV) detection was developed for the analysis of five drugs of abuse in urine samples. The factors affecting the extraction efficiency of SBSE such as sample pH, desorption solvent, sample volume, extraction time, desorption time, stirring rate and ionic strength were investigated and the optimal extraction conditions were established. Under the optimized conditions, the limits of detection (LODs) for titania-OH-TSO coated SBSE-HPLC-UV determination of five polar drugs of abuse were in the range of 2.3-9.1 μg/L with relative standard deviations (RSDs) ranging from 7.3 to 8.9% (c=300 μg/L, n=6), and all of the target compounds exhibited good linearity over a concentration range of 30-3000 μg/L. The developed method was applied to the determination of amphetamines and Ke in urine samples of drug abusers with satisfactory results.

  9. Use of experimental design in the investigation of stir bar sorptive extraction followed by ultra-high-performance liquid chromatography-tandem mass spectrometry for the analysis of explosives in water samples.

    Science.gov (United States)

    Schramm, Sébastien; Vailhen, Dominique; Bridoux, Maxime Cyril

    2016-02-12

    A method for the sensitive quantification of trace amounts of organic explosives in water samples was developed by using stir bar sorptive extraction (SBSE) followed by liquid desorption and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The proposed method was developed and optimized using a statistical design of experiment approach. Use of experimental designs allowed a complete study of 10 factors and 8 analytes including nitro-aromatics, amino-nitro-aromatics and nitric esters. The liquid desorption study was performed using a full factorial experimental design followed by a kinetic study. Four different variables were tested here: the liquid desorption mode (stirring or sonication), the chemical nature of the stir bar (PDMS or PDMS-PEG), the composition of the liquid desorption phase and finally, the volume of solvent used for the liquid desorption. On the other hand, the SBSE extraction study was performed using a Doehlert design. SBSE extraction conditions such as extraction time profiles, sample volume, modifier addition, and acetic acid addition were examined. After optimization of the experimental parameters, sensitivity was improved by a factor 5-30, depending on the compound studied, due to the enrichment factors reached using the SBSE method. Limits of detection were in the ng/L level for all analytes studied. Reproducibility of the extraction with different stir bars was close to the reproducibility of the analytical method (RSD between 4 and 16%). Extractions in various water sample matrices (spring, mineral and underground water) have shown similar enrichment compared to ultrapure water, revealing very low matrix effects.

  10. Automated in-syringe single-drop head-space micro-extraction applied to the determination of ethanol in wine samples.

    Science.gov (United States)

    Srámková, Ivana; Horstkotte, Burkhard; Solich, Petr; Sklenářová, Hana

    2014-05-30

    A novel approach of head-space single-drop micro-extraction applied to the determination of ethanol in wine is presented. For the first time, the syringe of an automated syringe pump was used as an extraction chamber of adaptable size for a volatile analyte. This approach enabled to apply negative pressure during the enrichment step, which favored the evaporation of the analyte. Placing a slowly spinning magnetic stirring bar inside the syringe, effective syringe cleaning as well as mixing of the sample with buffer solution to suppress the interference of acetic acid was achieved. Ethanol determination was based on the reduction of a single drop of 3mmol L(-1) potassium dichromate dissolved in 8mol L(-1) sulfuric acid. The drop was positioned in the syringe inlet in the head-space above the sample with posterior spectrophotometric quantification. The entire procedure was carried out automatically using a simple sequential injection analyzer system. One analysis required less than 5min including the washing step. A limit of detection of 0.025% (v/v) of ethanol and an average repeatability of less than 5.0% RSD were achieved. The consumption of dichromate reagent, buffer, and sample per analysis were only 20μL, 200μL, and 1mL, respectively. The results of real samples analysis did not differ significantly from those obtained with the references gas chromatography method. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Characterisation of dissolved organic compounds in hydrothermal fluids by stir bar sorptive extraction - gas chomatography - mass spectrometry. Case study: the Rainbow field (36°N, Mid-Atlantic Ridge

    Directory of Open Access Journals (Sweden)

    Konn Cecile

    2012-11-01

    Full Text Available Abstract The analysis of the dissolved organic fraction of hydrothermal fluids has been considered a real challenge due to sampling difficulties, complexity of the matrix, numerous interferences and the assumed ppb concentration levels. The present study shows, in a qualitative approach, that Stir Bar Sorptive Extraction (SBSE followed by Thermal Desorption – Gas Chromatography – Mass Spectrometry (TD-GC-MS is suitable for extraction of small sample volumes and detection of a wide range of volatile and semivolatile organic compounds dissolved in hydrothermal fluids. In a case study, the technique was successfully applied to fluids from the Rainbow ultramafic-hosted hydrothermal field located at 36°14’N on the Mid-Atlantic Ridge (MAR. We show that n-alkanes, mono- and poly- aromatic hydrocarbons as well as fatty acids can be easily identified and their retention times determined. Our results demonstrate the excellent repeatability of the method as well as the possibility of storing stir bars for at least three years without significant changes in the composition of the recovered organic matter. A preliminary comparative investigation of the organic composition of the Rainbow fluids showed the great potential of the method to be used for assessing intrafield variations and carrying out time series studies. All together our results demonstrate that SBSE-TD-GC-MS analyses of hydrothermal fluids will make important contributions to the understanding of geochemical processes, geomicrobiological interactions and formation of mineral deposits.

  12. Method for improving accuracy in full evaporation headspace analysis.

    Science.gov (United States)

    Xie, Wei-Qi; Chai, Xin-Sheng

    2017-03-21

    We report a new headspace analytical method in which multiple headspace extraction is incorporated with the full evaporation technique. The pressure uncertainty caused by the solid content change in the samples has a great impact to the measurement accuracy in the conventional full evaporation headspace analysis. The results (using ethanol solution as the model sample) showed that the present technique is effective to minimize such a problem. The proposed full evaporation multiple headspace extraction analysis technique is also automated and practical, and which could greatly broaden the applications of the full-evaporation-based headspace analysis. This article is protected by copyright. All rights reserved.

  13. Comparison of the sensitivity of different aroma extraction techniques in combination with gas chromatography-mass spectrometry to detect minor aroma compounds in wine.

    Science.gov (United States)

    Gamero, Amparo; Wesselink, Wilma; de Jong, Catrienus

    2013-01-11

    MicroVinification platforms are used for screening purposes to study aroma development in wine. These high-throughput methodologies require flavor analysis techniques that allow fast detection of a high number of aroma compounds which often appear in very low concentrations (μg/l). In this work, a selection of aroma extraction techniques in combination with gas chromatography-mass spectrometry (GC-MS) were evaluated to detect minor wine aroma compounds in low sample volume. The techniques evaluated were headspace (HS), headspace solid-phase dynamic extraction (HS-SPDE), headspace solid-phase microextraction (HS-SPME), direct immersion solid-phase microextraction (DI-SPME), stir bar sorptive extraction (SBSE) and monolithic material sorptive extraction (MMSE). DI-SPME showed the highest sensitivity as expressed by detection of the highest percentage of total aroma compounds at concentrations around 0.1 μg/l. SBSE and MMSE followed DI-SPME in terms of sensitivity. HS-SPME was less sensitive but considered sensitive enough for detection of most of the volatile compounds present in highly aromatic wines. Matrix effect was shown to strongly affect aroma extraction and therefore the sensitivity of the different extraction methods. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. Aroma quality assessment of Korean fermented red pepper paste (gochujang) by aroma extract dilution analysis and headspace solid-phase microextraction-gas chromatography-olfactometry.

    Science.gov (United States)

    Kang, Kyung-Mo; Baek, Hyung-Hee

    2014-02-15

    The objective of this study was to assess aroma quality of gochujang using purge and trap, simultaneous steam distillation and solvent extraction (SDE), and headspace solid-phase microextraction (HS-SPME), followed by gas chromatography-olfactometry (GC-O). Nineteen and 28 aroma-active compounds were detected by aroma extract dilution analysis of purge and trap and SDE, respectively. Diallyl disulfide and 3-isobutyl-2-methoxypyrazine played a significant role in the aroma quality of gochujang. Twelve aroma-active compounds were detected by HS-SPME-GC-O based on sample dilution analysis. Methional, diallyl disulfide, and 3-isobutyl-2-methoxypyrazine were the most intense aroma-active compounds. 3-Isobutyl-2-methoxypyrazine was identified for the first time in gochujang.

  15. Determination of nonylphenol and octylphenol in paper by microwave-assisted extraction coupled to headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Latorre, A; Lacorte, S; Barceló, D; Montury, M

    2005-02-18

    A novel and simple method for the determination of active endocrine disrupter compounds (octylphenol OP, and nonylphenol NP) in paper using microwave-assisted extraction (MAE) and headspace solid-phase microextraction, coupled with gas chromatography-mass spectrometry has been developed. Parameters affecting the efficiency in the MAE process such as exposure time and extraction solvent were studied in order to determine operating conditions. The optimised method was linear over the range studied (1.25-125 microg kg(-1) for OP and 9.50-950 microg kg(-1) for NP) and showed good level of precision, with a RSD lower than 10% and detection limits at 0.10 and 4.56 microg kg(-1) for OP and NP, respectively. The results obtained from six different types of paper revealed the presence of the target compounds in all samples analysed, at levels ranging between 3 and 211 microg kg(-1).

  16. Development of a Method for the Quantitation of Three Thiols in Beer, Hop, and Wort Samples by Stir Bar Sorptive Extraction with in Situ Derivatization and Thermal Desorption-Gas Chromatography-Tandem Mass Spectrometry.

    Science.gov (United States)

    Ochiai, Nobuo; Sasamoto, Kikuo; Kishimoto, Toru

    2015-08-05

    A method for analysis of hop-derived polyfunctional thiols, such as 4-sulfanyl-4-methylpentan-2-one (4S4M2Pone), 3-sulfanylhexan-1-ol (3SHol), and 3-sulfanylhexyl acetate (3SHA), in beer, hop water extract, and wort at nanogram per liter levels was developed. The method employed stir bar sorptive extraction with in situ derivatization (der-SBSE) using ethyl propiolate (ETP), followed by thermal desorption and gas chromatography-tandem mass spectrometry (TD-GC-MS/MS) with selected reaction monitoring (SRM) mode. A prior step involved structural identification of the ETP derivatives of the thiols by TD-GC-quadrupole-time-of-flight mass spectrometry with parallel sulfur chemiluminescence detection (Q-TOF-MS/SCD) after similar der-SBSE. The der-SBSE conditions of the ETP concentration, buffer concentration, salt addition, and extraction time profiles were investigated, and the performance of the method was demonstrated with spiked beer samples. The limits of detection (LODs) (0.19-27 ng/L) are below the odor threshold levels of all analytes. The apparent recoveries at 10-100 ng/L (99-101%) and the repeatabilities [relative standard deviation (RSD) of 1.3-7.2%; n = 6] are also good. The method was successfully applied to the determination of target thiols at nanogram per liter levels in three kinds of beer samples (hopped with Cascade, Citra, and Nelson Sauvin) and the corresponding hop water extracts and wort samples. There was a clear correlation between the determined values and the characteristics of citrus hop aroma for each sample.

  17. Differentiation of the volatile profile of microbiologically contaminated canned tomatoes by dynamic headspace extraction followed by gas chromatography-mass spectrometry analysis.

    Science.gov (United States)

    Bianchi, F; Careri, M; Mangia, A; Mattarozzi, M; Musci, M; Concina, I; Falasconi, M; Gobbi, E; Pardo, M; Sberveglieri, G

    2009-01-15

    The aromatic profile of microbiologically contaminated canned tomatoes was analyzed by the dynamic headspace extraction technique coupled with gas chromatography-mass spectrometry. Canned tomatoes contaminated with Escherichia coli, Saccharomyces cerevisiae and Aspergillus carbonarius were analyzed after 2 and 7 days. About 100 volatiles were detected, among which alcohols, aldehydes and ketones were the most abundant compounds. Gas chromatographic peak areas were used for statistical purposes. First, principal component analysis was carried out in order to visualize data trends and clusters. Then, linear discriminant analysis was performed in order to detect the set of volatile compounds ables to differentiate groups of analyzed samples. Five volatile compounds, i.e. ethanol, beta-myrcene, o-methyl styrene, 6-methyl-5-hepten-2-ol and 1-octanol, were found to be able to better discriminate between uncontaminated and contaminated samples. Prediction ability of the calculated model was estimated to be 100% by the "leave-one-out" cross-validation. An electronic nose device was then used to analyze the same contaminated and not contaminated canned tomato samples. Preliminary results were compared with those obtained by dynamic headspace gas chromatography-mass spectrometry, showing a good agreement.

  18. Ultrasonic nebulization extraction coupled with headspace single drop microextraction and gas chromatography-mass spectrometry for analysis of the essential oil in Cuminum cyminum L.

    Science.gov (United States)

    Wang, Lu; Wang, Ziming; Zhang, Huihui; Li, Xueyuan; Zhang, Hanqi

    2009-08-04

    A novel method for analysis of essential oil in Cuminum cyminum L. using simultaneous ultrasonic nebulization extraction and headspace single drop microextraction (UNE-HS-SDME) followed by gas chromatography-mass spectrometry was developed. Experimental parameters, including the kind of suspended solvent, microdrop volume, sample amount, extraction time, enrichment time and salt concentration were examined and optimized. Compared with hydrodistillation (HD), UNE-HS-SDME provides the advantages of a small amount of sample (50 mg), time-saving (20 min), simplicity, cheapness and low toxicity. In addition, UNE-HS-SDME also provided higher enrichment efficiency and sensitivity compared with stirring extraction (SE)-HS-SDME, ultrasonic assistant extraction (UAE) and UNE. Some constituents in the essential oil, were identified and the detection limits for beta-pinene, p-cymene and gamma-terpinene range from 6.67 pLL(-1) to 14.8 pLL(-1). The results indicated that the UNE-HS-SDME is simple and highly efficient extraction and enrichment technique.

  19. Static headspace gas chromatography-mass spectrometry for the one-step derivatisation and extraction of eleven aldehydes in drinking water.

    Science.gov (United States)

    Serrano, María; Gallego, Mercedes; Silva, Manuel

    2013-09-13

    Low-molecular-mass aldehydes (LMMAs) are water disinfection by-products formed by the reaction of ozone and/or chlorine with natural organic matter in water. LMMAs are mutagenic and carcinogenic compounds, which are detected at ng/L levels in water. An analytical method that allows simultaneous derivatisation and extraction of LMMAs in water has been developed using the classical static headspace technique coupled with gas chromatography-mass spectrometry (HS-GC-MS). Important parameters controlling the derivatisation of LMMAs with o-2,3,4,5,6-pentafluorobenzylhydroxylamine, oxime-products extraction and headspace generation were optimised to obtain the highest sensitivity, completing the entire process in 20min. For the first time the derivatisation reaction was carried out at alkaline pH adjusted with sodium hydrogen carbonate which exerts a significant enhancement effect on the derivatisation efficiency of the aldehydes; up to 20-fold with respect to those obtained in weak acid media as recommended by EPA Method 556.1. The addition of 200μL of n-hexane, as a chemical modifier, favoured the volatilisation of oxime-products, increasing the sensitivity of the method. The proposed method allows the achieving of detection limits from 2 to 80ng/L and has excellent precision (RSD average value of 6.4%) and accuracy (recovery ranging from 97% to 99%) for LMMA quantifications in drinking water samples. Finally, the HS-GC-MS method was validated relative to EPA Method 556.1 for the analysis of drinking water samples subjected to several disinfection treatments.

  20. Atmospheric pressure gas chromatography-time-of-flight-mass spectrometry (APGC-ToF-MS) for the determination of regulated and emerging contaminants in aqueous samples after stir bar sorptive extraction (SBSE).

    Science.gov (United States)

    Pintado-Herrera, Marina G; González-Mazo, Eduardo; Lara-Martín, Pablo A

    2014-12-03

    This work presents the development, optimization and validation of a multi-residue method for the simultaneous determination of 102 contaminants, including fragrances, UV filters, repellents, endocrine disruptors, biocides, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), and several types of pesticides in aqueous matrices. Water samples were processed using stir bar sorptive extraction (SBSE) after the optimization of several parameters: agitation time, ionic strength, presence of organic modifiers, pH, and volume of the derivatizing agent. Target compounds were extracted from the bars by liquid desorption (LD). Separation, identification and quantification of analytes were carried out by gas chromatography (GC) coupled to time-of-flight (ToF-MS) mass spectrometry. A new ionization source, atmospheric pressure gas chromatography (APGC), was tested. The optimized protocol showed acceptable recovery percentages (50-100%) and limits of detection below 1ngL(-1) for most of the compounds. Occurrence of 21 out of 102 analytes was confirmed in several environmental aquatic matrices, including seawater, sewage effluent, river water and groundwater. Non-target compounds such as organophosphorus flame retardants were also identified in real samples by accurate mass measurement of their molecular ions using GC-APGC-ToF-MS. To the best of our knowledge, this is the first time that this technique has been applied for the analysis of contaminants in aquatic systems. By employing lower energy than the more widely used electron impact ionization (EI), AGPC provides significant advantages over EI for those substances very susceptible to high fragmentation (e.g., fragrances, pyrethroids).

  1. Developing qualitative extraction profiles of coffee aromas utilizing polymeric ionic liquid sorbent coatings in headspace solid-phase microextraction gas chromatography-mass spectrometry.

    Science.gov (United States)

    López-Darias, Jessica; Anderson, Jared L; Pino, Verónica; Afonso, Ana M

    2011-11-01

    Two solid-phase microextraction (SPME) sorbent coatings based on polymeric ionic liquids (PILs) have been utilized for the analysis of complex coffee aroma samples. The PIL-based SPME coatings examined, namely, poly(1-(4-vinylbenzyl)-3-hexadecylimidazolium bis[(trifluoromethyl)sulfonyl]imide) [poly(VBHDIm(+) NTf(2)(-))], with ~14-μm thickness, and poly(1-vinyl-3-hexylimidazolium chloride) [poly(ViHIm(+)Cl(-))], with ~8-μm thickness, were employed for the headspace determination of up to 49 analytes from four different coffee beans: two French roast coffees of different brands, Sumatra coffee, and decaffeinated Sumatra coffee. The analysis was conducted using gas chromatography coupled to mass spectrometry. For comparative purposes, the commercial polyacrylate (PA, 85-μm film thickness) SPME coating was utilized under the same extraction conditions. The three SPME coatings tested behaved quite differently as a function of the families of compounds extracted. Thus, the poly(VBHDIm(+) NTf(2)(-) ) coating was extremely selective for aldehydes while also exhibiting good extraction efficiencies for acids. The poly-(ViHIm(+) Cl(-)) coating exhibited superior performance for aromatic alcohols, and the PA coating worked better for heterocyclic aromatics. Both PIL-based SPME sorbent coatings demonstrated exceptional selectivity and extraction efficiency when dealing with complex coffee aromas in spite of their small film thicknesses.

  2. GC-MS analysis of headspace and liquid extracts for metabolomic differentiation of citrus Huanglongbing and zinc deficiency in leaves of 'Valencia' sweet orange from commercial groves.

    Science.gov (United States)

    Cevallos-Cevallos, Juan Manuel; García-Torres, Rosalía; Etxeberria, Edgardo; Reyes-De-Corcuera, José Ignacio

    2011-01-01

    Citrus Huanglongbing (HLB) is considered the most destructive citrus disease worldwide. Symptoms-based detection of HLB is difficult due to similarities with zinc deficiency. To find metabolic differences between leaves from HLB-infected, zinc-deficient, and healthy 'Valencia' orange trees by using GC-MS based metabolomics. Analysis based on GC-MS methods for untargeted metabolite analysis of citrus leaves was developed and optimized. Sample extracts from healthy, zinc deficient, or HLB-infected sweet orange leaves were submitted to headspace solid phase micro-extraction (SPME) and derivatization treatments prior to GC-MS analysis. Principal components analysis achieved correct classification of all the derivatized liquid extracts. Analysis of variance revealed 6 possible biomarkers for HLB, of which 5 were identified as proline, β-elemene, (-)trans- caryophyllene, and α-humulene. Significant (P < 0.05) differences in oxo-butanedioic acid, arabitol, and neo-inositol were exclusively detected in samples from plants with zinc deficiency. Levels of isocaryophyllen, α-selinene, β-selinene, and fructose were significantly (P < 0.05) different in healthy leaves only. Results suggest the potential of using identified HLB biomarkers for rapid differentiation of HLB from zinc deficiency. Copyright © 2010 John Wiley & Sons, Ltd.

  3. GC/MS analysis of volatiles obtained by headspace solid-phase microextraction and simultaneous-distillation extraction from Rabdosia serra (MAXIM.) HARA leaf and stem.

    Science.gov (United States)

    Lin, Lianzhu; Zhuang, Mingzhu; Lei, Fenfen; Yang, Bao; Zhao, Mouming

    2013-01-15

    Volatiles in Rabdosia serra were investigated by headspace solid phase microextraction (HS-SPME) and simultaneous-distillation extraction (SDE). The HS-SPME technique was previously evaluated to optimise sampling conditions. A total of 56 and 48 compounds including alcohols, aldehydes, hydrocarbons, ketones, carboxylic acid, ester, and aromatics were identified in leaf and stem by optimised HS-SPME method (CAR/PDMS fibre; incubation time, 10 min; extraction temperature, 50°C; extraction time, 40 min), respectively. 1-Octen-3-ol and (2E)-hexenal had significant contribution to R. serra aroma. Cluster analysis indicated that leaf and stem exhibited different volatile diversity. Air drying was favourable for the retention of the volatiles, while freeze- and sun-drying led to the loss of volatiles. SDE method preferred to the analysis of compounds with low volatility including fatty acids and esters. HS-SPME was a useful technique for the analysis of readily volatile components for the characteristics of R. serra aroma.

  4. An Effective Method to Detect Volatile Intermediates Generated in the Bioconversion of Coal to Methane by Gas Chromatography-Mass Spectrometry after In-Situ Extraction Using Headspace Solid-Phase Micro-Extraction under Strict Anaerobic Conditions.

    Science.gov (United States)

    Liu, Jianmin; Wang, Baoyu; Tai, Chao; Wu, Li; Zhao, Han; Guan, Jiadong; Chen, Linyong

    2016-01-01

    Bioconversion of coal to methane has gained increased attention in recent decades because of its economic and environmental advantages. However, the mechanism of this process is difficult to study in depth, partly because of difficulties associated with the analysis of intermediates generated in coal bioconversion. In this investigation, we report on an effective method to analyze volatile intermediates generated in the bioconversion of coal under strict anaerobic conditions. We conduct in-situ extraction of intermediates using headspace solid-phase micro-extraction followed by detection by gas chromatography-mass spectrometry. Bioconversion simulation equipment was modified and combined with a solid-phase micro-extraction device. In-situ extraction could be achieved by using the combined units, to avoid a breakdown in anaerobic conditions and to maintain the experiment continuity. More than 30 intermediates were identified qualitatively in the conversion process, and the variation in trends of some typical intermediates has been discussed. Volatile organic acids (C2-C7) were chosen for a quantitative study of the intermediates because of their importance during coal bioconversion to methane. Fiber coating, extraction time, and solution acidity were optimized in the solid-phase micro-extraction procedure. The pressure was enhanced during the bioconversion process to investigate the influence of headspace pressure on analyte extraction. The detection limits of the method ranged from 0.0006 to 0.02 mmol/L for the volatile organic acids and the relative standard deviations were between 4.6% and 11.5%. The volatile organic acids (C2-C7) generated in the bioconversion process were 0.01-1.15 mmol/L with a recovery range from 80% to 105%. The developed method is useful for further in-depth research on the bioconversion of coal to methane.

  5. Time since discharge of 9mm cartridges by headspace analysis, part 2: Ageing study and estimation of the time since discharge using multivariate regression.

    Science.gov (United States)

    Gallidabino, M; Romolo, F S; Weyermann, C

    2017-03-01

    Estimating the time since discharge of spent cartridges can be a valuable tool in the forensic investigation of firearm-related crimes. To reach this aim, it was previously proposed that the decrease of volatile organic compounds released during discharge is monitored over time using non-destructive headspace extraction techniques. While promising results were obtained for large-calibre cartridges (e.g., shotgun shells), handgun calibres yielded unsatisfying results. In addition to the natural complexity of the specimen itself, these can also be attributed to some selective choices in the methods development. Thus, the present series of papers aimed to systematically evaluate the potential of headspace analysis to estimate the time since discharge of cartridges through the use of more comprehensive analytical and interpretative techniques. Following the comprehensive optimisation and validation of an exhaustive headspace sorptive extraction (HSSE) method in the first part of this work, the present paper addresses the application of chemometric tools in order to systematically evaluate the potential of applying headspace analysis to estimate the time since discharge of 9mm Geco cartridges. Several multivariate regression and pre-treatment methods were tested and compared to univariate models based on non-linear regression. Random forests (RF) and partial least squares (PLS) proceeded by pairwise log-ratios normalisation (PLR) showed the best results, and allowed to estimate time since discharge up to 48h of ageing and to differentiate recently fired from older cartridges (e.g., less than 5h compared to more than 1-2 days). The proposed multivariate approaches showed significant improvement compared to univariate models. The effects of storage conditions were also tested and results demonstrated that temperature, humidity and cartridge position should be taken into account when estimating the time since discharge.

  6. Atmospheric pressure gas chromatography–time-of-flight-mass spectrometry (APGC–ToF-MS) for the determination of regulated and emerging contaminants in aqueous samples after stir bar sorptive extraction (SBSE)

    Energy Technology Data Exchange (ETDEWEB)

    Pintado-Herrera, Marina G.; González-Mazo, Eduardo; Lara-Martín, Pablo A., E-mail: pablo.lara@uca.es

    2014-12-03

    Graphical abstract: Examples of identification of target (triclosan, TCS) and non-target (tributhyl phosphate, TBP) compounds in environmental water samples by APGC–ToF-MS. Some confirmation criteria are shown (i.e. mass spectra, isotopic distribution, and accurate mass). - Highlights: • 102 regulated and emerging contaminants are simultaneously extracted by SBSE. • APGC–ToF-MS is presented as an alternative to EI for the analysis of microcontaminants. • Identification of non-target compounds in environmental matrices is also explored. - Abstract: This work presents the development, optimization and validation of a multi-residue method for the simultaneous determination of 102 contaminants, including fragrances, UV filters, repellents, endocrine disruptors, biocides, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), and several types of pesticides in aqueous matrices. Water samples were processed using stir bar sorptive extraction (SBSE) after the optimization of several parameters: agitation time, ionic strength, presence of organic modifiers, pH, and volume of the derivatizing agent. Target compounds were extracted from the bars by liquid desorption (LD). Separation, identification and quantification of analytes were carried out by gas chromatography (GC) coupled to time-of-flight (ToF-MS) mass spectrometry. A new ionization source, atmospheric pressure gas chromatography (APGC), was tested. The optimized protocol showed acceptable recovery percentages (50–100%) and limits of detection below 1 ng L{sup −1} for most of the compounds. Occurrence of 21 out of 102 analytes was confirmed in several environmental aquatic matrices, including seawater, sewage effluent, river water and groundwater. Non-target compounds such as organophosphorus flame retardants were also identified in real samples by accurate mass measurement of their molecular ions using GC-APGC–ToF-MS. To the best of our knowledge, this is the first time that this

  7. Quantitative analysis of phosphoric acid esters in aqueous samples by isotope dilution stir-bar sorptive extraction combined with direct analysis in real time (DART)-Orbitrap mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bridoux, Maxime C., E-mail: maxime.bridoux@cea.fr [CEA, DAM, DIF, F-91297 Arpajon (France); Malandain, Hélène [SANTEN SAS, 1 rue Pierre Fontaine, Bâtiment Genavenir IV, F-91058 Evry (France); Leprince, Françoise; Progent, Frédéric; Machuron-Mandard, Xavier [CEA, DAM, DIF, F-91297 Arpajon (France)

    2015-04-15

    Highlights: • Theory and modeling of organophosphorus SBSE extraction are presented. • Organophosphorus are quantitatively analyzed by isotopic dilution SBSE/DART/Orbitrap-MS. • PDMS coated Twisters™ extract phosphate acid esters in the neutral form from water samples. • Good linearity between concentrations and relative peak areas (0.1–750 ng mL{sup −1}). • This novel SBSE/DART/Orbitrap-MS method should be very valuable for on-site sampling/monitoring - Abstract: A novel hyphenated technique, namely the combination of stir bar sorptive extraction (SBSE) with isotope dilution direct analysis in real time (DART) Orbitrap™ mass spectrometry (OT-MS) is presented for the extraction of phosphoric acid alkyl esters (tri- (TnBP), di- (HDBP), and mono-butyl phosphate (H2MBP)) from aqueous samples. First, SBSE of phosphate esters was performed using a Twister™ coated with 24 μL of polydimethylsiloxane (PDMS) as the extracting phase. SBSE was optimized for extraction pH, phase ratio (PDMS volume/aqueous phase volume), stirring speed, extraction time and temperature. Then, coupling of SBSE to DART/Orbitrap-MS was achieved by placing the Twister™ in the middle of an open-ended glass tube between the DART and the Orbitrap™. The DART mass spectrometric response of phosphate esters was probed using commercially available and synthesized alkyl phosphate ester standards. The positive ion full scan spectra of alkyl phosphate triesters (TnBP) was characterized by the product of self-protonation [M + H]{sup +} and, during collision-induced dissociation (CID), the major fragmentation ions corresponded to consecutive loss of alkyl chains. Negative ionization gave abundant [M − H]{sup −} ions for both HDnBP and H2MnBP. Twisters™ coated with PDMS successfully extracted phosphate acid esters (tri-, di- and mono-esters) granted that the analytes are present in the aqueous solution in the neutral form. SBSE/DART/Orbitrap-MS results show a good linearity between

  8. Comparison of Headspace Solid-Phase Microextraction with Simultaneous Steam Distillation Extraction for the Analysis of the Volatile Constituents in Chinese Apricot

    Institute of Scientific and Technical Information of China (English)

    CHEN Mei-xia; CHEN Xue-sen; WANG Xin-guo; CI Zhi-juan; LIU Xiao-li; HE Tian-ming; ZHANG Li-jie

    2006-01-01

    Volatile constituents in fully mature fruits of apricot (Prunus armeniaca L.) cultivar Xinshiji were extracted using headspace solid-phase microextraction (HS-SPME) and simultaneous steam distillation extraction (SSDE) and then analyzed using capillary gas chromatography and gas chromatography-mass spectrometry. A total of 70 components were identified by HSSPME, including 20 esters, 19 hydrocarbons, 5 alcohols, 5 ketones, 4 acids, 4 lactones, 3 aldehydes, and 10 miscellaneous components, with the esters being the dominant constituent. On the basis of the odor unit values, it is believed that the following compounds probably contributed to the fresh apricot odor: hexyl acetate, β-ionone, butyl acetate, (E)-2-hexenal,linalool, limonene, γ-decalactone, and hexanal. A total of 49 components were also detected by SSDE, including 13 hydrocarbons, 9 alcohols, 7 aldehydes, 9 esters, 4 ketones, 4 lactones, 2 acids, and 1 miscellaneous component, of which the monoterpene alcohols were the dominant constituents. It could be judged from the odor unit values that the following compounds were the major contributors to boiled apricot aroma: β-ionone, linalool, hexyl acetate, γ-dodecalactone, γ-decalactone, (E)-2-hexenal, hexanal, γ-octalactone, phenylacetaldehyde, butyl acetate, limonene, α-terpineol, and δ-decalactone.The results show that HS-SPME is a simple, rapid, and solvent-free method, which is an alternative to the classical SSDE.

  9. [Determination of 2,4,6-trichloroanisole in wine by head-space solid phase micro-extraction and gas chromatography-mass spectrometry].

    Science.gov (United States)

    Liu, Qing; Zhong, Qiding; Li, Jingguang; Xing, Jiangtao; Huang, Feifei; Zhao, Yunfeng; Wu, Yongning

    2012-07-01

    To establish a method of combining gas chromatography-mass spectrometry (GC-MS) with head-space solid phase micro-extraction (HS-SPME) for the detection of 2,4,6-trichloroanisole (2,4,6-TCA) in wine. 2,4,6-TCA in wine were extracted by polydimethylsiloxane (PDMS,100 microm) fiber for 15 min under 35 degrees C in a water bath. The fiber was then transferred into the injection port of the GC-MS and separated by a CP-SIL 8CB-MS capillary column (30m x 0.25mm x 0.25 microm), and detected by mass spectrometry using d5-2,4,6-TCA as an internal standard. The linear range for 2,4,6-TCA was 5 (60ng/L, the detection limit was 0.06ng/L. The recovery of standard addition (5, 10, 20ng/L) was in the range of 79.8% (101.6% with relative standard deviations (RSD, n=5) wine.

  10. A novel dispersive micro solid phase extraction using zein nanoparticles as the sorbent combined with headspace solid phase micro-extraction to determine chlorophenols in water and honey samples by GC-ECD.

    Science.gov (United States)

    Farhadi, Khalil; Matin, Amir Abbas; Amanzadeh, Hatam; Biparva, Pourya; Tajik, Hossein; Farshid, Amir Abbas; Pirkharrati, Hossein

    2014-10-01

    This study presents a new technique, dispersive micro solid phase extraction (DMSPE) combined with headspace solid phase micro-extraction (HS-SPME) for extraction and determination of chlorophenols (CPs) in water and honey samples using a Gas Chromatography-Electron Capture Detector (GC-ECD). Zein nanoparticles were made by liquid-liquid dispersion and applied for the first time as the sorbent phase in DMSPE. In the proposed DMSPE-HS-SPME method, 1% w/v of ethanolic zein solution was added to an aqueous sample and then a dose of the in-situ generated zein nanoparticles was applied to a pre-concentration of target analytes. Thermal desorption of analytes was performed after the isolating sorbent phase, and then HS-SPME was applied for enrichment prior to introducing to gas chromatography. All the important parameters influencing efficiency of the extraction process such effects of salt, pH, sorbent concentration, temperature, sorbent solution volume in DMSPE procedure, extraction temperature, extraction time, desorption temperature and time in the HS-SPME procedure were investigated and optimized. Results showed that under optimum extraction conditions, detection limits (signal to noise ratio=3) were in the range of 0.08-0.6 ng mL(-1) and evaluations for relative standard deviations (RSDs %) were between 6.62% and 8.36%.

  11. Variation in Scent Compounds of Oil-Bearing Rose (Rosa damascena Mill. Produced by Headspace Solid Phase Microextraction, Hydrodistillation and Solvent Extraction

    Directory of Open Access Journals (Sweden)

    Sabri Erbaş

    2016-03-01

    Full Text Available In this research, rose oil and rose water were hydro-distilled from the fresh oil-bearing rose flowers (Rosa damascena Mill. using Clevenger-type apparatus. Rose concretes were extracted from the fresh rose flowers by using non-polar solvents, e.g. diethyl ether, petroleum ether, cyclo-hexane, chloroform and n-hexane, and subsequently by evaporation of the solvents under vacuum. Absolutes were produced from the concretes with ethyl alcohol extraction at -20°C, leaving behind the wax and other paraffinic substances. Scent compounds of all these products detected by gas chromatography (GC-FID/GC-MS were compared with the natural scent compounds of fresh rose flower detected by using headspace solid phase microextraction (HS-SPME with carboxen/polydimethylsiloxane (CAR/PDMS fiber. A total of 46 compounds analysis were identified by HS-SPME-GC-MS in the fresh flower, and a total of 15 compounds were identified by GC-MS in the hydrodistilled rose oil. While main compounds in rose oil were geraniol (35.4%, citronellol (31.6%, and nerol (15.3%, major compound in fresh rose flower, rose water and residue water was phenylethyl alcohol (43.2, 35.6 and 98.2%, respectively. While the highest concrete yield (0.7% was obtained from diethyl ether extraction, the highest absolute yield (70.9% was obtained from the n-hexane concrete. The diethyl ether concrete gave the highest productivity of absolute, as 249.7 kg of fresh rose flowers was needed to produce 1 kg of absolute.

  12. Parameters optimization using experimental design for headspace solid phase micro-extraction analysis of short-chain chlorinated paraffins in waters under the European water framework directive.

    Science.gov (United States)

    Gandolfi, F; Malleret, L; Sergent, M; Doumenq, P

    2015-08-07

    The water framework directives (WFD 2000/60/EC and 2013/39/EU) force European countries to monitor the quality of their aquatic environment. Among the priority hazardous substances targeted by the WFD, short chain chlorinated paraffins C10-C13 (SCCPs), still represent an analytical challenge, because few laboratories are nowadays able to analyze them. Moreover, an annual average quality standards as low as 0.4μgL(-1) was set for SCCPs in surface water. Therefore, to test for compliance, the implementation of sensitive and reliable analysis method of SCCPs in water are required. The aim of this work was to address this issue by evaluating automated solid phase micro-extraction (SPME) combined on line with gas chromatography-electron capture negative ionization mass spectrometry (GC/ECNI-MS). Fiber polymer, extraction mode, ionic strength, extraction temperature and time were the most significant thermodynamic and kinetic parameters studied. To determine the suitable factors working ranges, the study of the extraction conditions was first carried out by using a classical one factor-at-a-time approach. Then a mixed level factorial 3×2(3) design was performed, in order to give rise to the most influent parameters and to estimate potential interactions effects between them. The most influent factors, i.e. extraction temperature and duration, were optimized by using a second experimental design, in order to maximize the chromatographic response. At the close of the study, a method involving headspace SPME (HS-SPME) coupled to GC/ECNI-MS is proposed. The optimum extraction conditions were sample temperature 90°C, extraction time 80min, with the PDMS 100μm fiber and desorption at 250°C during 2min. Linear response from 0.2ngmL(-1) to 10ngmL(-1) with r(2)=0.99 and limits of detection and quantification, respectively of 4pgmL(-1) and 120pgmL(-1) in MilliQ water, were achieved. The method proved to be applicable in different types of waters and show key advantages, such

  13. Determination of 20 Pesticides in Water Sample by GC - MS with Stir Bar Sorptive Extraction%搅拌棒吸附子萃取与GC-MS法测定水中20种有机氯农药

    Institute of Scientific and Technical Information of China (English)

    朱定姬; 黄克建; 林翠梧; 李宏森; 刘晓锋; 李璐; 罗正坚

    2009-01-01

    A new method for the simultaneous determination of 20 organochlorine pesticides, inclu-ding α-BHC, γ-BHC, β3-BHC, heptachlor, δ-BHC, aldrin, heptachlor epoxide, γ-chlordane, cis-chlordane, endosulfan I , p, p'-DDE, dieldrin, endrin, p, p'-DDD, endosulfan Ⅱ , p, p'-DDT, endrin hexadrin, endosulfan sulfate, methoxychlor and endrin ketone in water samples was developed by stir bar sorptive extraction (SBSE) coupled with gas chromatography - mass spectrome-try (GC - MS). The samples was extracted by stir bar and desorbed by methanol. The analytes were separated on a J & W DB-35 MS(30 m × 0. 25 mm × 0. 25 μm) column, and detected by GC - MS un-der selected ion monitoring (SIM) mode. Effects of extraction time, addition of salt and methanol on extraction efficiency were studied. The calibration curves showed a good linearity between 2. 5 μg/L and 20 μg/L for 20 organochlorine pesticides. The limits of detection (S/N = 3 ) ranged from 0. 008 μg/L to 0. 118 μg/L. The average recoveries of 20 organochlorine pesticides in water sample at two spiked concentration levels of 2.5, 20 μg/L ranged from 52% to 117% with RSDs less than 13% (n = 6). The method was rapid, simple, sensitive, and was applied to determine the real water with satisfactory results.%建立了搅拌棒吸附子萃取/气相色谱-质谱法(SBSE/GC-MS)同时检测水中α-六六六、γ-六六六、β-六六六、七氯、δ-六六六、艾氏剂、环氧七氯、γ-氯丹、顺-氯丹、硫丹Ⅰ、p,p-滴滴伊、狄氏剂、异狄氏剂、p,p-滴滴滴、硫丹Ⅱ、p,p-滴滴涕、异狄氏剂醛、硫丹硫酸盐、甲氧滴滴涕、异狄氏剂酮20种有机氯农药含量的方法.样品在室温下经拌棒吸附子搅拌吸附,甲醇解吸附后,以J&W DB-35 MS(30 m×0.25 mm×0.25 μm)石英毛细管色谱柱为分析柱,气相色谱-质谱选择离子流模式检测.考察了萃取时间、氯化钠及甲醇加入量等对萃取的影响.实验结果表明:在2.5 ~20.0

  14. Determination of volatile organic compounds including alcohols in refill fluids and cartridges of electronic cigarettes by headspace solid-phase micro extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lim, Hyun-Hee; Shin, Ho-Sang

    2017-02-01

    An analytical method for the detection of 14 volatile organic compounds (VOCs) was developed to investigate VOCs in refill fluids and cartridges of electronic cigarettes (EC) using headspace solid-phase micro extraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). In total, 14 VOCs were identified and quantified in 283 flavored liquids, 21 nicotine liquids, and 12 disposable cartridges. The detected concentration ranges of the VOCs are as follows: benzene (0.008-2.28 mg L(-1)), toluene (0.006-0.687 mg L(-1)), ethylbenzene (0.01-1.21 mg L(-1)), m-xylene (0.002-1.13 mg L(-1)), p-xylene (0.007-2.8 mg L(-1)), o-xylene (0.004-2.27 mg L(-1)), styrene (0.011-0.339 mg L(-1)), ethyl acetate (0.3-669.9 mg L(-1)), ethanol (16-38,742 mg L(-1)), methanol (66-3375 mg L(-1)), pyridine (0.077-99.7 mg L(-1)), acetylpyrazine (0.077-147 mg L(-1)), 2,3,5-trimethylpyrazine (0.008-96.8 mg L(-1)), and octamethylcyclotetrasiloxane (0.1-57.2 mg L(-1)). Benzene, toluene, ethylbenzene, m-xylene, p-xylene, and o-xylene coexisted in samples, which may have originated from the use of petrogenic hydrocarbons as an extraction solvent for flavor and nicotine from natural plants. The maximum detected concentrations of benzene, methanol, and ethanol in liquid samples were found in quantities higher than their authorized maximum limits as residual solvents in pharmaceutical products.

  15. [Determination of 2-methylisoborneol and geosmin in drinking water using headspace solid phase micro-extraction coupled with gas chromatography-mass-spectrometry].

    Science.gov (United States)

    Cheng, Jianguo; Liu, Kaiying; Bai, Mindong; Cheng, Chao; Yu, Yixuan; Zhou, Xinying

    2015-12-01

    The odorous compounds of 2-methylisoborneol (2-MIB) and geosmin (GSM) heavily produced and released in water source are one of the most important factors leading to off-flavor emergencies and resident water consumption panic in drinking water. A headspace solid phase micro-extraction ( HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) method was established for the simultaneous determination of these two trace earthy and musty compounds in reservoir water, reservoir soil and tap water. The conditions of HS-SPME, such as salt amount, extraction time and extraction temperature, were optimized based on orthogonal analysis. The qualitative and quantitative analyses of 2-MIB and GSM were carried out in the electron impact (EI) -selective ion scanning mode. The results showed that the linear relationship between peak area and concentration of 2-MIB and GSM was good enough (r2 0.998) from 5 to 1 000 ng/L, the limits of detection were 0.72 ng/L for 2-MIB, 0.34 ng/L for GSM and the limits of quantification were 2.40 ng/L for 2-MIB, 1.13 ng/L for GSM. When the target samples spiked in the range of 10-600 ng/L, the average recoveries of the target compounds were 93.6% - 107.7% ( RSD ≤ 6.1%, n = 6). Based on the above method, the target compounds in reservoir water, reservoir soil and tap water in a certain region of Liaoning Province were analyzed. The results showed that the two target odors in reservoir water were 3.0 -3.6 ng/L. As for the extract of the soil around the reservoir, 2-MIB was 8.1 ng/L and GSM was 17.8 ng/L. The odorous substances were not detected in the tap water. This method is simple, accurate, reliable, highly sensitive and no need of organic solvents. And it is suitable for the detection of 2-MIB and GSM in drinking water.

  16. An assessment of the liquid-gas partitioning behavior of major wastewater odorants using two comparative experimental approaches: liquid sample-based vaporization vs. impinger-based dynamic headspace extraction into sorbent tubes.

    Science.gov (United States)

    Iqbal, Mohammad Asif; Kim, Ki-Hyun; Szulejko, Jan E; Cho, Jinwoo

    2014-01-01

    The gas-liquid partitioning behavior of major odorants (acetic acid, propionic acid, isobutyric acid, n-butyric acid, i-valeric acid, n-valeric acid, hexanoic acid, phenol, p-cresol, indole, skatole, and toluene (as a reference)) commonly found in microbially digested wastewaters was investigated by two experimental approaches. Firstly, a simple vaporization method was applied to measure the target odorants dissolved in liquid samples with the aid of sorbent tube/thermal desorption/gas chromatography/mass spectrometry. As an alternative method, an impinger-based dynamic headspace sampling method was also explored to measure the partitioning of target odorants between the gas and liquid phases with the same detection system. The relative extraction efficiency (in percent) of the odorants by dynamic headspace sampling was estimated against the calibration results derived by the vaporization method. Finally, the concentrations of the major odorants in real digested wastewater samples were also analyzed using both analytical approaches. Through a parallel application of the two experimental methods, we intended to develop an experimental approach to be able to assess the liquid-to-gas phase partitioning behavior of major odorants in a complex wastewater system. The relative sensitivity of the two methods expressed in terms of response factor ratios (RFvap/RFimp) of liquid standard calibration between vaporization and impinger-based calibrations varied widely from 981 (skatole) to 6,022 (acetic acid). Comparison of this relative sensitivity thus highlights the rather low extraction efficiency of the highly soluble and more acidic odorants from wastewater samples in dynamic headspace sampling.

  17. Use of an autosampler for dynamic headspace extraction of volatile compounds from grains and effect of added water on the extraction.

    Science.gov (United States)

    Ram, M S; Seitz, L M; Rengarajan, R

    1999-10-01

    An autosampler attached to a purge and trap instrument was used to aid routine analyses of grain samples for volatile compounds associated with off-odors. Trapped volatiles were transferred to a gas chromatograph/mass spectrometer instrument for separation and detection. Dynamic extraction of volatiles from approximately 18 g of whole grain at 80 degrees C was accomplished by purging helium through a sample vial with a Teflon-lined septum on each end. The autosampler automatically added internal standard to the sample before purging began, which required the addition of 1 mL of water for complete transfer of the standard to the sample. The added water enhanced extraction of 1-octen-3-ol, 1-octen-3-one, and some other compounds from soybeans but not from starchy grains such as corn and wheat. Addition of a free radical scavenger, such as citric acid, greatly diminished the recovery of 1-octen-3-ol and 1-octen-3-one from soybeans.

  18. Sorptivity and liquid infiltration into dry soil

    Science.gov (United States)

    Culligan, Patricia J.; Ivanov, Vladimir; Germaine, John T.

    2005-10-01

    The sorptivity S quantifies the effect of capillarity on liquid movement in a porous material. For liquid infiltration into an initially dry material, S is a parameter that is contingent on both liquid and material properties as well as the maximum liquid content behind the infiltrating front, θm. Scaling analyses are used to derive a dimensionless, intrinsic sorptivity S∗ that is constant for different liquids, Miller-similar materials and different values of θm. The analyses confirm that S is dependent on β1/2, where β = cos ϕ is a measure of the wettability of the liquid. They also indicate a power law relationship between S and Se(av), the average liquid saturation behind the infiltrating front. Seventeen water and eleven Soltrol 220 horizontal infiltration experiments are reported in uniform, dry sand. Test results show that water is partially wetting in the sand. They also confirm that S∝Se(av)d, where d = 3.2 for the experimental conditions. The usefulness of a general, dimensionless Boltzmann variable is demonstrated to normalize infiltration profiles for the different liquids. An approximate method for sorptivity calculation is shown to provide an accurate estimate of S∗.

  19. Multidimensional gas chromatography-mass spectrometry determination of 3-alkyl-2-methoxypyrazines in wine and must. A comparison of solid-phase extraction and headspace solid-phase extraction methods.

    Science.gov (United States)

    Culleré, Laura; Escudero, Ana; Campo, Eva; Cacho, Juan; Ferreira, Vicente

    2009-05-01

    Two different strategies for the quantitative determination of 3-alkyl-2-methoxypyrazines in wine and must have been developed and validated. Comparison between both the techniques has been presented and the most adequate has been applied to the determination of these compounds in different samples of wine, made from several varieties of grapes, and also in different samples of must made from Cabernet Sauvignon grapes. Both the methods consisted of a dynamic headspace coupled with a solid-phase extraction (HS-SPE) and solid-phase extraction (SPE) directly from the sample, coupled with multidimensional gas chromatography-mass spectrometry system (MDGC-MS). Both of them require resins LiChrolut EN, and analyte elution has been carried out with dichloromethane. The repeatability of both methodologies was evaluated at two concentration levels. The relative standard deviations (RSD%) were acceptable in every case, but smaller when working with HS-SPE. The recoveries obtained for the three analytes with the two methodologies were almost 100%, with the exception of IBMP, which had a recovery of only 70% with HS-SPE. The linearity was satisfactory with both methods for the range of occurrence of methoxypyrazines in wine and must. The limits of detection of the direct SPE technique were much lower than those of HS-SPE in every case. Direct SPE method detection limits ranged from 0.09 to 0.15 ng L(-1). The method based on direct SPE was chosen finally because it had better detection limits and was easier and quicker than the HS-SPE-based method. It has been applied to the determination of these components in 36 wine and 17 musts samples. The quantitative results suggest that the Spanish wines show meaningless amounts of these compounds. IBMP has been found just in between 1.9 and 15 ng L(-1).

  20. Differences between Lipids Extracted from Five Species Are Not Sufficient To Explain Biomagnification of Nonpolar Organic Chemicals

    DEFF Research Database (Denmark)

    Jahnke, Annika; Holmbäck, Jan; Andersson, Rina Argelia

    2015-01-01

    headspace from spiked olive oil to determine their sorptive capacities. Lipids from seal blubber and pork bacon solely composed of triglycerides had capacities similar to that of olive oil; lipids from mussels, herring, and guillemot egg had quantifiable fractions of phospholipids and cholesterol and showed...... capacities reduced by factors of up to 2.3-fold. Generally, the sorptive capacities of the lipids were not elevated relative to the olive oil controls and are unlikely to explain a substantial part of biomagnification....

  1. Vinegar classification based on feature extraction and selection from headspace solid-phase microextraction/gas chromatography volatile analyses: a feasibility study.

    Science.gov (United States)

    Pizarro, C; Esteban-Díez, I; Sáenz-González, C; González-Sáiz, J M

    2008-02-04

    Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography (GC) and multivariate data analysis were applied to classify different vinegar types (white and red, balsamic, sherry and cider vinegars) on the basis of their volatile composition. The collected chromatographic signals were analysed using the stepwise linear discriminant analysis (SLDA) method, thus simultaneously performing feature selection and classification. Several options, more or less restrictive according to the final number of considered categories, were explored in order to identify the one that afforded highest discrimination ability. The simplicity and effectiveness of the classification methodology proposed in the present study (all the samples were correctly classified and predicted by cross-validation) are promising and encourage the feasibility of using a similar strategy to evaluate the quality and origin of vinegar samples in a reliable, fast, reproducible and cost-efficient way in routine applications. The high quality results obtained were even more remarkable considering the reduced number of discriminant variables finally selected by the stepwise procedure. The use of only 14 peaks enabled differentiation between cider, balsamic, sherry and wine vinegars, whereas only 3 variables were selected to discriminate between red (RW) and white wine (WW) vinegars. The subsequent identification by gas chromatography-mass spectrometry (GC-MS) of the volatile compounds associated with the discriminant peaks selected in the classification process served to interpret their chemical significance.

  2. Headspace Analysis of Ammonium Nitrate

    Science.gov (United States)

    2017-01-25

    Naval Research Laboratory Washington, DC 20375-5320 NRL/MR/6110--17-9709 Headspace Analysis of Ammonium Nitrate January 25, 2017 Approved for public...TELEPHONE NUMBER (include area code) b. ABSTRACT c. THIS PAGE 18. NUMBER OF PAGES 17. LIMITATION OF ABSTRACT Headspace Analysis of Ammonium Nitrate G...isobutane reagent ion from analysis of ammonia desorbed from packed tungsten oxide sampling tube .................. 18 E-1 Executive Summary The

  3. An Economical Method for Static Headspace Enrichment for Arson Analysis

    Science.gov (United States)

    Olesen, Bjorn

    2010-01-01

    Static headspace analysis of accelerants from suspected arsons is accomplished by placing an arson sample in a sealed container with a carbon strip suspended above the sample. The sample is heated, cooled to room temperature, and then the organic components are extracted from the carbon strip with carbon disulfide followed by gas chromatography…

  4. 搅拌棒萃取-热脱附/气质联用法测定水中2-MIB和土臭素%Determination of 2-Methylisoborneol and Geosmin in Water Using Stir Bar Sorptive Extraction-Thermal Desorption/Gas Chromatography Coupled with Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    范苓; 张晓赟; 秦宏兵; 顾海东

    2013-01-01

    A method using stir bar sorptive extraction ( SBSE)-thermal desorption ( TD)/gas chromatogra-phy coupled with mass spectrometry ( GCMS) was developed to determinate ultra-trace level of 2-methylisoborneol (2-MIB) and geosmin in water .SBSE and TD parameters were optimized through blank spiked sample .The method showed good linearity ( r>0 .999 ) over concentration range from 1 ng/L to 200 ng/L and high sensitivity ( the MDL of 2-MIB and geosmin were 0 .31 ng/L and 0 .15 ng/L respectively ) .The spiked recovery of blank and real samples ranged from 82 .4%to 116%with RSD <10%.%采用搅拌棒萃取-热脱附/气质联用法测定水中2-甲基异莰醇和土臭素,优化了搅拌棒萃取和热脱附进样的条件。试验表明:两种目标化合物在1.00 ng/L~200 ng/L范围内线性良好,2-甲基异莰醇的相关系数为0.9993,土臭素的相关系数为0.9997,方法检出限分别为0.31 ng/L和0.15 ng/L;空白和实际样品的加标回收率为82.4%~116%,测定结果的RSD<10%。

  5. Characterization of the Typical Potent Odorants in Chinese Roasted Sesame-like Flavor Type Liquor by Headspace Solid Phase Microextraction-Aroma Extract Dilution Analysis, with Special Emphasis on Sulfur-Containing Odorants.

    Science.gov (United States)

    Sha, Sha; Chen, Shuang; Qian, Michael; Wang, Chengcheng; Xu, Yan

    2017-01-11

    The aroma profile of Chinese roasted sesame-like flavor type liquor was investigated by means of headspace solid phase microextraction-aroma extract dilution analysis (HS-SPME-AEDA). Sixty-three odor-active regions were detected by HS-SPME-AEDA with flavor dilution (FD) factors >5, and 58 of these were further identified. Among them, ethyl hexanoate, 2-furfurylthiol, dimethyl trisulfide, 3-methylbutanal, ethyl butanoate, ethyl 2-methylbutanoate, ethyl pentanoate, and ethyl 4-methylpentanoate appeared with the highest FD factors. In particular, eight sulfur-containing odorants were identified to be potentially important to roasted sesame-like flavor type liquor. The concentration of these odor-active compounds was further quantitated by combination of four different quantitative measurements, and 36 odorants had concentrations higher than their corresponding odor thresholds. On the basis of the odor activity values (OAVs), 2-furfurylthiol (OAV 1182), dimethyl trisulfide (OAV 220), β-damascenone (OAV 116), and methional (OAV 99) could be responsible for the unique aroma of roasted sesame-like flavor type liquor. An aroma recombination model prepared by mixing 36 aroma compounds with OAVs >1 showed a good similarity to the aroma of the original roasted sesame-like flavor type liquor. For the first time, 2-furfurylthiol was determined to be a typical potent odorant in roasted sesame-like flavor type liquor by omission study.

  6. Determination of off-flavor compounds, 2-methylisoborneol and geosmin, in salmon fillets using stir bar sorptive extraction–thermal desorption coupled with gas chromatography–mass spectrometry

    Science.gov (United States)

    A sensitive and solvent-less method for the determination of musty and earthy off-flavor compounds, 2-methylisoborneol (MIB) and geosmin (GSM), in salmon tissue was developed using stir bar sorptive extraction -thermal desorption coupled with gas chromatography -mass spectrometry (SBSE -TD -GCMS). M...

  7. Variation in Scent Compounds of Oil-Bearing Rose (Rosa damascena Mill.) Produced by Headspace Solid Phase Microextraction, Hydrodistillation and Solvent Extraction

    OpenAIRE

    Sabri Erbaş; Hasan Baydar

    2016-01-01

    In this research, rose oil and rose water were hydro-distilled from the fresh oil-bearing rose flowers (Rosa damascena Mill.) using Clevenger-type apparatus. Rose concretes were extracted from the fresh rose flowers by using non-polar solvents, e.g. diethyl ether, petroleum ether, cyclo-hexane, chloroform and n-hexane, and subsequently by evaporation of the solvents under vacuum. Absolutes were produced from the concretes with ethyl alcohol extraction at -20°C, leaving behind the wax and othe...

  8. Gas flow headspace liquid phase microextraction.

    Science.gov (United States)

    Yang, Cui; Qiu, Jinxue; Ren, Chunyan; Piao, Xiangfan; Li, Xifeng; Wu, Xue; Li, Donghao

    2009-11-06

    There is a trend towards the use of enrichment techniques such as microextraction in the analysis of trace chemicals. Based on the theory of ideal gases, theory of gas chromatography and the original headspace liquid phase microextraction (HS-LPME) technique, a simple gas flow headspace liquid phase microextraction (GF-HS-LPME) technique has been developed, where the extracting gas phase volume is increased using a gas flow. The system is an open system, where an inert gas containing the target compounds flows continuously through a special gas outlet channel (D=1.8mm), and the target compounds are trapped on a solvent microdrop (2.4 microL) hanging on the microsyringe tip, as a result, a high enrichment factor is obtained. The parameters affecting the enrichment factor, such as the gas flow rate, the position of the microdrop, the diameter of the gas outlet channel, the temperatures of the extracting solvent and of the sample, and the extraction time, were systematically optimized for four types of polycyclic aromatic hydrocarbons. The results were compared with results obtained from HS-LPME. Under the optimized conditions (where the extraction time and the volume of the extracting sample vial were fixed at 20min and 10mL, respectively), detection limits (S/N=3) were approximately a factor of 4 lower than those for the original HS-LPME technique. The method was validated by comparison of the GF-HS-LPME and HS-LPME techniques using data for PAHs from environmental sediment samples.

  9. Volatile constituents from flower of Tianmian Cucurbita moschata Duch. by head-space solid micro-extraction coupled with GC-MS%HS-SPME-GC-MS分析甜面大南瓜花挥发性成分

    Institute of Scientific and Technical Information of China (English)

    李昌勤; 卢引; 李新铮; 邢晗; 康文艺

    2012-01-01

    Objective: To study the volatile constituents in flowers of Cucurbita moschata Duch. (Tianmian). Methods The volatiles were analyzed by head-space solid micro-extraction,coupled with GC-MS and Kovats indices for the first time. A quantitative analysis in percent was performed by peak area normalization measurements to search the volatile constituents from flowers of C. moschata Duch. (Tianmian). Results 37 compounds were identified from the male flowers and 16 from the female flowers,98.24% and 94.45% of the total essential constituents respectively,the male flowers and the female had 10 common components. Conclusion =The volatile constituents were different between the female flowers and the male of C. moschata.%目的:分析甜面大南瓜花挥发性成分。方法:采用顶空固相微萃取和气质联用技术(HS-SPME-GC-MS),结合保留指数法,首次采用峰面积归一化法计算各化合物的相对百分含量来分析甜面大南瓜花挥发性成分。结果:从甜面大南瓜雄花和雌花中分别鉴定出37和16种化合物,分别占总峰面积的98.24%和94.45%。其中雄花和雌花有10种共有成分。结论:发现甜面大南瓜雌雄花的挥发性成分具有差别。

  10. Dynamic headspace time-extended helix liquid-phase microextraction.

    Science.gov (United States)

    Huang, Shih-Pin; Chen, Pai-Shan; Huang, Shang-Da

    2009-05-15

    Liquid-phase microextraction (LPME) has been proved to be a fast, inexpensive and effective sample pre-treatment technique for the analyses of pesticides and many other compounds. In this investigation, a new headspace microextraction technique, dynamic headspace time-extended helix liquid-phase microextraction (DHS-TEH-LPME), is presented. In this work, use of a solvent cooling system, permits the temperature of the extraction solvent to be lowered. Lowering the temperature of the extraction solvent not only reduces solvent loss but also extends the feasible extraction time, thereby improving extraction efficiency. Use of a larger volume of the solvent not only extends the feasible extraction time but also, after extraction, leaves a larger volume to be directly injected into the gas chromatography (GC) to increase extraction efficiency and instrument signal. The DHS-TEH-LPME technique was used to extract six organochlorine pesticides (OCPs) from 110ml water samples that had been spiked with the analytes at ng/l levels, and stirred for 60min. The proposed method attained enrichments up to 2121 fold. The effects of extraction solvent identity, sample agitation, extraction time, extraction temperature, and salt concentration on extraction performance were also investigated. The method detection limits (MDLs) varied from 0.2 to 25ng/l. The calibration curves were linear for at least 2 orders of magnitude with R(2)>==0.996. Relative recoveries in river water were more than 86%.

  11. Solar sorptive cooling. Technologies, user requirements, practical experience, future prospects

    Energy Technology Data Exchange (ETDEWEB)

    Treffinger, P. [DLR Deutsches Zentrum fuer Luft- und Raumfahrt e.V., Hardthausen (Germany); Hertlein, H.P. [eds.] [Forschungsverbund Sonnenenergie, Koeln (Germany)

    1998-09-01

    Sorptive cooling techniques permit the use of low-temperature solar heat, i.e. a renewable energy of low cost and world-wide availability. The Forschungsverbund Sonnenenergie intends to develop solar sorptive cooling technologies to the prototype stage and, in cooperation with the solar industry and its end users, to promote practical application in air conditioning of buildings and cold storage of food. The workshop presents an outline of the state of development of solar sorptive cooling from the view of users and developers. Exemplary solar cooling systems are described, and the potential of open and closed sorptive processes is assessed. Future central activities will be defined in an intensive discussion between planners, producers, users and developers. [German] Der Einsatz von Sorptionstechniken zur Kaelteerzeugung erlaubt es, als treibende Solarenergie Niedertemperatur-Solarwaerme einzusetzen, also eine regenerative Energie mit sehr geringen Kosten und weltweiter Verfuegbarkeit. Der Forschungsverbund Sonnenenergie hat sich als Aufgabe gestellt, die Techniken der solaren Sorptionskuehlung bis zum Prototyp zu entwickeln und mit Industrie und Nutzern die praktische Anwendung voranzubringen. Die Anwendungsfelder sind die Klimatisierung von Gebaeuden und die Kaltlagerung von Lebensmitteln. Der Workshop gibt einen Ueberblick zum Entwicklungsstand der solaren Sorptionskuehlung aus der Sicht der Anwender und Entwickler. Bereits ausgefuehrte Beispiele zur solaren Kuehlung werden vorgestellt und das Potential geschlossener und offener Sorptionsverfahren angegeben. In intensiver Diskussion zwischen Planern, Herstellern, Nutzern und Entwicklern sollen kuenftige Arbeitsschwerpunkte herausgearbeitet werden. (orig.)

  12. Fast characterization of cheeses by dynamic headspace-mass spectrometry.

    Science.gov (United States)

    Pérès, Christophe; Denoyer, Christian; Tournayre, Pascal; Berdagué, Jean-Louis

    2002-03-15

    This study describes a rapid method to characterize cheeses by analysis of their volatile fraction using dynamic headspace-mass spectrometry. Major factors governing the extraction and concentration of the volatile components were first studied. These components were extracted from the headspace of the cheeses in a stream of helium and concentrated on a Tenax TA trap. They were then desorbed by heating and injected directly into the source of a mass spectrometer via a short deactivated silica transfer line. The mass spectra of the mixture of volatile components were considered as fingerprints of the analyzed substances. Forward stepwise factorial discriminant analysis afforded a limited number of characteristic mass fragments that allowed a good classification of the batches of cheeses studied.

  13. Analysis of volatile organic compounds emitted from aircraft carpets:comparison using headspace and dynamic chamber tests 

    Institute of Scientific and Technical Information of China (English)

    WANG Chao; YANG Xu-Dong; GAO Peng

    2014-01-01

    Volatile organic compounds (VOCs) emitted from three types of carpets used in aircrafts were compared by using headspace and dynamic chamber tests. The headspace samples contained many compounds that were not detected in the dynamic chamber test;in addition, the dominant VOCs found by these two methods were different. The findings indicate that for highly sorptive materials such as carpets, headspace analysis may give inaccurate indication of actual VOC emissions, and it is necessary to conduct dynamic chamber tests over a certain period of time in order to identify the true emission characteristics. From the dynamic chamber tests, 2-ethyl-1-hexanol was the main VOC emitted from all three carpets. The study also examined the emission characteristics of aircraft carpets. In all experiments, total VOC (TVOC) concentration peaked within a few hours after the start of the experiment and was followed by rapid decay. The emission parameters of TVOC emitted by all three carpets were calculated and the simulated data matched the measured data well.

  14. Comparative analysis of headspace volatiles of Chinese Rosa rugosa.

    Science.gov (United States)

    Feng, Li-Guo; Chen, Chen; Sheng, Li-Xia; Liu, Ping; Tao, Jun; Su, Jia-Le; Zhao, Lan-Yong

    2010-11-16

    The floral headspace compounds of Chinese Rosa rugosa germplasms that were isolated by an automated headspace sampler with built-in trap, and followed by gas chromatography-mass spectrometry for identification and quantification. Up to 33 volatile compounds were identified from the 23 rose germplasms, including nine alcohols, five esters, three alkanes, 10 terpenes, three aldehydes, two ketones, and one ether. The main floral components identified were 2-phenylethanol, β-citronellol, ethanol, and n-hexane. 'xizi', 'miaofengshan', 'xiangciguo', and 'tangbai' contained the highest amounts of 2-phenylethanol at 84.66 μg·g⁻¹, β-citronellol at 70.98 μg·g⁻¹, ethanol at 83.87 μg·g⁻¹, and n-hexane at 18.23 μg·g⁻¹, respectively. 'Rongchengyesheng', 'tanghong', 'xizi', 'miaofengshan', and 'baizizhi' could be considered good materials for extracting rose oil and breeding new cultivars.

  15. 顶空气相色谱法测定大孔树脂提取物中的残留溶剂研究%Determination of residual solvents in macroporous resin extracts by Head-space capillary gas chromatography

    Institute of Scientific and Technical Information of China (English)

    刘冬; 杨敬芝; 杜守颖; 张东明; 赵立敏; 陈雯

    2009-01-01

    目的:建立了测定大孔树脂淫羊藿提取物、栀子提取物以及HP中乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯残留有机溶剂含量的顶空气相色谱法.方法:采用顶空气相色谱法,FID检测器,以20%~50%二甲基亚砜为溶媒,顶空预热温度为90℃,预热时间为10 min,进样口温度为180℃,检测器温度为250℃,以氮气为载气,使用DB-1交联毛细管柱(60m×0.32mm,1 μm),程序升温,实现了各组分的基线分离.结果:乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯在各自对应的浓度范围内,线性关系良好;乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯的最小检测限分别为2.72,0.22,0.03,0.03,0.28,0.33,0.03,0.31 μg·mL~(-1);加样回收率均在75%以上,精密度较好.结论:经方法学验证,该方法灵敏、准确、可靠,可适用于大孔树脂淫羊藿提取物、栀子提取物及HP中乙醇、正己烷、苯、甲苯、甲基环己烷、二甲苯、苯乙烯、二乙烯苯等残留有机溶剂的测定.%Objective:This paper reports a Head-space GC method for determination of enthanol,hexane,benzene,toluene,methyl cyclohexane,xylene,styrene,divinyl benzene in macroporous resin extractions.Method:The analytical coluren was DB-1(60m×0.32mm,1μm).The injector temperature was 180℃ and the detector tempemture was 250℃.The column temperature was programmed raised.The carrier gas was nitrogen and the solvent was 20%-50% dimethyl sulfoxide.Results:The stand curve were linear for each solvents in the range of each consistencv.The average recoveries were all more than 75%.Conclusion:This method is simple,rapid and precise,it is suitable for measurement of residual solvents in macroporous resin extracts.

  16. 顶空固相微萃取法与水蒸气蒸馏法提取姜黄挥发性成分的比较%Comparison of volatile components from Curcuma longa extracted by headspace solid-phase microextraction and steam distillation

    Institute of Scientific and Technical Information of China (English)

    樊钰虎; 刘江; 王泽秀; 张涛

    2012-01-01

    Objective: To compare the volatile components from Curcuma longa extract by headspace solid - phase microextraction and steam distillation, and verify the analysis results bu PC A technology. Methods: The volatile oils from Curcuma longa were extracted by using steam distillation or headspace solid - phase microextraction. Then the oils were analyzed by GC - MS combined with principal components analysis (PCA). Results: The results indicated that totally 48 different volatile compounds were identified in the extracts, with 41 from headspace solid - phase microextraction and 33 from steam distillation. Among which,26 mutual compounds were detected. Conclusion:There were some differences between the two methods. PCA was further used in validating the differences and similarities. As compared with steam distillation, both the number and varieties of the constituents were more in the volatile oils extracted by solid - phase microextraction. Solid - phase microextraction was obviously superior to steam distillation.%目的:采用顶空固相微萃取和水蒸气蒸馏法分别提取姜黄挥发性成分并进行GC-MS比较分析,并结合PCA技术对分析结果进行验证.方法:采用顶空固相微萃取法和水蒸气蒸馏法提取姜黄挥发性成分,运用GC-MS技术,结合计算机检索对其挥发性成分进行分离鉴定,并通过PCA技术对结果进行验证.结果:2种方法共鉴定出48个挥发性成分,其中顶空固相微萃取法鉴定出41种挥发性化学成分,水蒸气蒸馏法鉴定出33种挥发性化学成分,共有成分为26种.结论:2种方法鉴定出的挥发性成分及其相对含量上存在一定差异,PCA分析亦进一步验证了其异同.与水蒸气蒸馏法比较,顶空固相微萃取法所得挥发性成分数目和种类较多,顶空固相微萃取法比水蒸气蒸馏法具有明显的优越性.

  17. Dynamic headspace liquid-phase microextraction of alcohols.

    Science.gov (United States)

    Saraji, Mohammad

    2005-01-07

    A method was developed using dynamic headspace liquid-phase microextraction and gas chromatography-mass spectrometry for extraction and determination of 9 alcohols from water samples. Four different solvents, hexyl acetate, n-octanol, o-xylene and n-decane were studied as extractants. The analytes were extracted using 0.8 microl of n-octanol from the headspace of a 2 ml sample solution. The effect of sampling volume, solvent volume, sample temperature, syringe plunger withdrawal rate and ionic strength of the solution on the extraction performance were studied. A semiautomated system including a variable speed stirring motor was used to ensure a uniform movement of syringe plunger through the barrel. The method provided a fairly good precision for all compounds (5.5-9.3%), except methanol (16.4%). Detection limits were found to be between 1 and 97 microg/l within an extraction time of approximately 9.5 min under GC-MS in full scan mode.

  18. Mechano-sorptive creep of Portuguese pinewood chemically modified

    Directory of Open Access Journals (Sweden)

    Barroso Lopes Duarte

    2014-03-01

    Full Text Available The effect of chemical modification on mechano-sorptive creep in bending was studied by experimental work. Stakes with 20 × 20 × 400 mm RTL of Portuguese wood species (Pinus pinaster Aiton modified with 1,3-dimethylol-4,5- dihydroxyethyleneurea (DMDHEU, m-methylated melamine resin (MMF, tetraethoxysilane (TEOS and amid wax (WA were measured under asymmetric moistening conditions over a period of 42 days (app. 1000 hours with stress level (SL of 12 MPa, according to ENV 1156.

  19. Headspace - Guided Meditation and Mindfulness Techniques.

    Science.gov (United States)

    2016-08-03

    Mindfulness has been recommended by the National Institute for Health and Care Excellence and the NHS to help mental wellbeing, but can the Headspace app be used by nurses and health professionals in clinical settings?

  20. Selective fiber used for headspace solid-phase microextraction of abused drugs in human urine

    OpenAIRE

    Sunanta Wangkarn

    2007-01-01

    A sensitive and selective fiber for simultaneous analysis of three drugs of abuse (amphetamine, methamphetamine and ephedrine) in urine samples was explored using headspace solid phase microextraction and gas chromatography with flame ionization detection. Several parameters affecting extraction such as extraction time, extraction temperature, pH of solution and salt concentrations were investigated. Among five commercially available fibers, divinylbenzene/carboxen/ polydimethylsiloxane is th...

  1. Transport simulation of sorptive contaminants considering sediment-associated processes

    Institute of Scientific and Technical Information of China (English)

    LI Ruijie; LU Shasha; ZHENG Jun

    2012-01-01

    Sediment-associated processes,such as sediment erosion,deposition,and pore water diffusion/advection affect sorptive contaminant transport.By considering these processes,we developed an equation to simulate contaminant transport.Erosion and deposition processes are considered as erosion and deposition fluxes of sediment,and adsorption-desorption processes of contaminants by sediment are simulated using the Langmuir Equation.Pore water diffusion is calculated based on the contaminant concentration gradient across the sediment-water interface.Pore water advection is estimated using pore water contained in the sediments of erosion flux.The equation is validated to simulate total phosphorus concentrations in Guanhe estuary in the northern Jiangsu,China.The simulated total phosphorus concentrations show better agreement with field observations compared to estimations that do consider sediment-associated processes.

  2. Sorptive removal of tetracycline from water by palygorskite

    Energy Technology Data Exchange (ETDEWEB)

    Chang, Po-Hsiang [Department of Earth Sciences, National Cheng Kung University, 1 University Road, Tainan 70101, Taiwan (China); Li, Zhaohui, E-mail: li@uwp.edu [Department of Earth Sciences, National Cheng Kung University, 1 University Road, Tainan 70101, Taiwan (China); Department of Geosciences, University of Wisconsin-Parkside, 900 Wood Road, Kenosha, WI 53144 (United States); Yu, Tsai-Luen; Munkhbayer, Sandagdori; Kuo, Tzu-Hsing; Hung, Yu-Chiao; Jean, Jiin-Shuh [Department of Earth Sciences, National Cheng Kung University, 1 University Road, Tainan 70101, Taiwan (China); Lin, Kao-Hung [Sustainable Environmental Research Center, National Cheng Kung University, Tainan 70101, Taiwan (China)

    2009-06-15

    Extensive use of pharmaceuticals and growth hormone in farm animal and live stocks has resulted in their frequent detection in soils, groundwater, and wastewater. The fate and transport of these compounds are strongly affected by their sorptive behavior to the soil minerals and humic materials. In this research, we conducted the sorption of tetracycline (TC), a common antibiotic, on palygorskite (PFL-1), a fibrous clay mineral of high surface area and high sorptivity towards organic compounds. The results showed that the sorption capacity of TC on PFL-1 was as high as 210 mmol/kg at pH 8.7. The sorption was relatively fast and reached equilibrium in 2 h. Solution pH and ionic strength had significant effects on TC sorption. The sorption of TC by palygorskite is endothermic and the free energy of sorption is in the range of -10 to -30 kJ/mol, suggesting a strong physical sorption. The X-ray diffraction patterns before and after TC sorption revealed no changes in d-spacing and intensity under different pH and initial TC concentrations, indicating that the sorbed TC molecules are on the external surface of the mineral in contrast to intercalation of TC into swelling clays, such as montmorillonite. The small positive value of entropy change suggested that TC molecules are in disordered arrangement on palygorskite surfaces. Surface sorption of TC on PFL-1 is further supported by the derivative of gravimetric analysis and by the calculation of the amount of TC sorption normalized to the surface area. The results suggest that palygorskite could be a good candidate to remove TC from wastewater containing higher amounts of TC.

  3. Determination of volatile organic compounds in water using headspace knotted hollow fiber microextraction.

    Science.gov (United States)

    Chen, Pai-Shan; Tseng, Yu-Hsiang; Chuang, Yuh-Lin; Chen, Jung-Hsuan

    2015-05-22

    An efficient and effective headspace microextraction technique named static headspace knotted hollow fiber microextraction (HS-K-HFME) has been developed for the determination of volatile organic compounds (VOCs) in water samples. The knot-shaped hollow fiber is filled with 25μL of the extraction solvent. The excess solvent forms a large droplet (13μL) and is held in the center of the knot. Even after 20min of extraction time at high temperature (95°C) without cooling, there was still enough volume of extraction solvent for gas chromatography-mass spectrometry (GC-MS) analysis, which extends the choice of solvents for headspace LPME. Moreover, the knot-shaped fiber has a larger extraction contact interface, which increases the rate of mass transfer between the headspace and extraction solvent film attached to the fiber, thus improving the extraction efficiency. The effects of extraction solvent, temperature, stirring rate, salt concentration and extraction time on extraction performance were optimized. The calibration curves exhibited coefficients of determination (R(2)) ranging from 0.9957 to 0.9999 and the limit of detection (LOD) ranged from 0.2 to 10μgL(-1). Relative standard deviations (RSDs) ranged from 4.5% to 11.6% for intraday measurements (n=5). Interday (n=15) values were between 2.2% and 12.9%. The relative recoveries (RRs) ranged from 90.3% to 106.0% for river water and 95.9% to 103.6% for wastewater.

  4. 同时蒸馏萃取和动态顶空萃取法提取焙烤小麦胚芽中风味物质%Analysis of Volatile Aroma Components in Baked Wheat Germ by Simultaneous Distillation and Extraction or Dynamic Headspace Extraction Coupled with GC-MS

    Institute of Scientific and Technical Information of China (English)

    呼德; 张颖; 张甜甜; 侯建军; 任雅琳; 陈存社

    2012-01-01

    The purpose of this study was to compare the analytical results obtained for the volatile composition of baked wheat germ by simultaneous distillation extraction (SDE) and dynamic headspace extraction (DHE) coupled with GC-MS. A total of 101 volatile compounds were identified from baked wheat germ by both methods, including 15 aldehydes, 8 alcohols, 11 hydrocarbons, 12 ketones, 6 ester, 5 phenols, 10 acids, 6 ethers and 28 nitrogen-containing heterocyclic compounds. Among them, aldehydes and nitrogen-containing heterocyclic compounds were identified as dominant volatile compounds responsible for the flavor of baked wheat germ. Great differences were observed among the peak areas of the same volatile compounds measured by both methods, but almost the same types of volatile compounds were identified from baked wheat germ, especially the critical aroma-active compounds. Therefore, similar results could be obtained for the composition of aromatic compounds by SDE/GC-MS and DHE/GC-MS.%为研究焙烤小麦胚芽中的挥发性风味成分,采用动态顶空萃取(DHS)与同时蒸馏萃取(SDE)两种方法提取焙烤小麦胚芽中的风味物质,并通过气质联机(GC-MS)进行风味成分的分离与鉴定,结果共鉴定出101种化合物,包括醛类15种、醇类8种、烃类11种、酮类12种、酯类6种、酚类5种,酸类10种、醚类6种、含氮杂环类28种,其中挥发性的醛以及含氮类杂环化合物构成了焙烤小麦胚芽的风味主体。两种方法检测出的香味化合物的峰面积偏差较大,但鉴定出的化合物种类大致相同,特别是焙烤麦芽香味中的关键香味成分。从香味成分的构成考虑,DHs/GC-MS与sDE/GC-MS的分析结果较为相似。

  5. Headspace solvent microextraction-gas chromatography-mass spectrometry for the analysis of volatile compounds from Foeniculum vulgare Mill.

    Science.gov (United States)

    Fang, Lianghua; Qi, Meiling; Li, Ting; Shao, Qinglong; Fu, Ruonong

    2006-06-07

    A novel and rapid headspace solvent microextraction followed by gas chromatography-mass spectrometry (HSME-GC-MS) for the analysis of the volatile compounds of Foeniculum vulgare Mill is described. HSME parameters including extracting solvent, extraction temperature and time, headspace volume and particle size were optimized. As a result, benzyl alcohol was finally used for the extraction at 70 degrees C for 20 min with headspace volume of 12.1 ml and particle size of 120 mesh. Under the determined conditions, the powered samples of Foeniculum vulgare Mill were directly applied for the analysis. A comparison of HSME-GC-MS, solid phase microextraction (SPME)-GC-MS and steam distillation (SD)-GC-MS methods was made and showed that the HSME-GC-MS method was simple, inexpensive and effective and can be used for the analysis of volatile compounds in traditional Chinese medicines (TCMs).

  6. Volatile profile of yellow passion fruit juice by static headspace and solid phase microextraction techniques

    Directory of Open Access Journals (Sweden)

    Gilberto Costa Braga

    2015-02-01

    Full Text Available The profile of volatile compounds of yellow passion fruit juice was analyzed by solid phase microextraction headspace (HS-SPME and optimized static headspace (S-HS extraction techniques. Time, temperature, NaCl concentration and sample volume headspace equilibrium parameters was adjusted to the S-HS technique. The gaseous phase in the headspace of samples was collected and injected into a gas chromatograph coupled to a mass spectrometer. In the HS-SPME technique was identified 44 volatile compounds from the yellow passion fruit juice, but with S-HS only 30 compounds were identified. Volatile esters were majority in both techniques, being identified ethyl butanoate, ethyl hexanoate, (3z-3-hexenyl acetate, hexyl acetate, hexyl butanoate and hexyl hexanoate. Aldehydes and ketones were not identified in S-HS, but were in HS-SPME. β-Pinene, p-cymene, limonene, (Z-β-ocimene, (E-β-ocimene, γ-terpinene, α-terpinolene and (E -4,8-dimethyl-1, 3,7 - nonatriene terpenes were identified in both techniques. This study showed that the S-HS optimized extraction technique was effective to recovery high concentrations of the major volatile characteristics compounds in the passion fruit, such as ethyl butanoate and ethyl hexanoate, which can be advantageous due to the simplicity of the method.

  7. 顶空液相微萃取-气相色谱法测定指甲油中的苯类物质%Determination of benzene substances in nail polish by headspace liquid-phase micro extraction combined with gas chromatography

    Institute of Scientific and Technical Information of China (English)

    宋吉英; 郭峰

    2012-01-01

    本实验采用顶空液相微萃取法,正辛醇作为萃取溶剂,样品在30℃水浴条件下搅拌顶空萃取25 min.待测物结合气相色谱分析方法,采用程序升温和分流进样,用氢火焰离子化检测器建立了测定指甲油中苯类物质的新方法.各种目标物的线性相关系数在0.9833 ~0.9934之间,加标回收率在95.88%-97.70%之间.该方法稳定可靠,分析结果良好.%A new method was developed for the determination of benzene substances by headspace liquid-phase micro extraction-gas chromatography. The sample was agitated in 30 ℃ water for 25 min, octanol was extraction solvent. The FID detector, temperature-programmed method and split injection were chosen. The linearly dependent coefficient was 0.983 3-0.993 4 and spiking average recovery was 95. 88% ~ 97. 70% . The results show that the method is reliable and sensitive on the real samples.

  8. Comparative Analysis of Headspace Volatiles of Chinese Rosa rugosa

    Directory of Open Access Journals (Sweden)

    Lan-Yong Zhao

    2010-11-01

    Full Text Available The floral headspace compounds of Chinese Rosa rugosa germplasms that were isolated by an automated headspace sampler with built-in trap, and followed by gas chromatography-mass spectrometry for identification and quantification. Up to 33 volatile compounds were identified from the 23 rose germplasms, including nine alcohols, five esters, three alkanes, 10 terpenes, three aldehydes, two ketones, and one ether. The main floral components identified were 2-phenylethanol, β-citronellol, ethanol, and n-hexane. ‘xizi’, ‘miaofengshan’, ‘xiangciguo’, and ‘tangbai’ contained the highest amounts of 2-phenylethanol  at 84.66 μg·g-1, β-citronellol at 70.98 μg·g-1, ethanol at 83.87 μg·g-1, and n-hexane at 18.23 μg·g-1, respectively. ‘Rongchengyesheng’, ‘tanghong’, ‘xizi’, ‘miaofengshan’, and ‘baizizhi’ could be considered good materials for extracting rose oil and breeding new cultivars.

  9. Statistical Modeling Efforts for Headspace Gas

    Energy Technology Data Exchange (ETDEWEB)

    Weaver, Brian Phillip [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2016-03-17

    The purpose of this document is to describe the statistical modeling effort for gas concentrations in WIPP storage containers. The concentration (in ppm) of CO2 in the headspace volume of standard waste box (SWB) 68685 is shown. A Bayesian approach and an adaptive Metropolis-Hastings algorithm were used.

  10. Comparison between dynamic headspace and headspace solid-phase microextraction for gas chromatography of BTEX in urine.

    Science.gov (United States)

    Brcić Karaconji, Irena; Skender, Ljiljana

    2007-12-01

    The aim of this study was to compare two extraction procedures: dynamic headspace-purge and trap (PT) and headspace solid-phase microextraction (HS-SPME) for gas chromatographic determination of benzene, toluene, ethylbenzene, and isomeric xylenes (BTEX) in urine with photoionization (PID) and mass spectrometric (MS) detection, respectively. Both methods showed linearity in the range of interest [(50-2000) ng L-1], good accuracy (80% to 100%), and repeatability (RSD< or =11%). Detection limits were in the low ng L-1 level for both methods, although slightly greater sensitivity was found for the PT method. In comparison with PT, HS-SPME was simpler and required less time for analysis. Although the analytical features of both examined methods are appropriate for biomonitoring of environmental exposure to BTEX, only the HS-SPME-GC-MS method is recommended for routine analysis of BTEX in urine. The method was applied for the quantitative analysis of BTEX in urine samples collected from non-smokers (n=10) and smokers (n=10).

  11. Sorptive affinity of ionic surfactants on silt loamy soil

    Directory of Open Access Journals (Sweden)

    Xingchao Qi

    2016-10-01

    Full Text Available Due to their broad applications, ionic surfactants have already been released into or utilized in soil and environmental systems. However, current understanding on the sorption behavior of surfactants onto soils is still limited. This work systematically investigated the sorption kinetics and isotherms of one cationic surfactant, cetyltrimethylammonium bromide (CTAB, and one anionic surfactant, sodium dodecyl sulfate (SDS, onto a silt loamy soil to determine the governing sorption mechanisms. The pseudo-second-order rate equation described the sorption kinetics data better than the pseudo-first-order rate equation. Experimental data showed that the sorption equilibrium for CTAB and SDS were reached at 24 and 240 h, respectively. Langmuir equation was better than Freundlich equation in simulating the sorption isotherms of CTAB and SDS on the soil. Soil Langmuir maximum sorption capacity of CTAB was much higher than that to SDS. When the experimental temperature increased, the sorption of CTAB and SDS on the soil decreased. In addition, the sorptive process of the surfactants on the soil was spontaneous and exothermal, as indicated by the absolute values of Gibbs free energy and enthalpy. The results also indicated that physical sorption was the dominant mechanism for the sorption of the two surfactants on the soil. Findings from this work are crucial to understand the environmental behaviors of ionic surfactants.

  12. Modeling the effect of initial soil moisture on sorptivity and infiltration

    Science.gov (United States)

    Stewart, Ryan; Abou Najm, Majdi; Rupp, David; Selker, John

    2016-04-01

    Soil capillarity, often associated with the parameter sorptivity, is a primary control on infiltration during short-duration rainfall and irrigation events. However, most mathematical models used to quantify capillarity are only valid for dry antecedent conditions. In this study, we examine how the capillary component of sorptivity (i.e., wetting front potential) varies with initial soil water content, and use this finding to provide a simple modification to the classic Green-Ampt sorptivity model. The modified model has many practical applications, including 1) describing the relative sorptivity of a soil at various water contents; 2) quantifying saturated hydraulic conductivity from sorptivity measurements; and 3) interpreting transient time behavior of single ring infiltration (i.e., beerkan) measurements. The model is especially useful in low permeability soils, where steady-state conditions may not be attained for hours or even days, and in shrink-swell soils, where rapid infiltration measurements are often desired so as not to induce substantial material swelling.

  13. Characterization of volatile compounds of Daucus crinitus Desf. Headspace Solid Phase Microextraction as alternative technique to Hydrodistillation

    OpenAIRE

    Tabti Boufeldja; Allali Houcine; Desjobert Jean-Marie; Djabou Nassim; El Amine Dib Mohammed; Muselli Alain; Costa Jean

    2010-01-01

    Background : Traditionally, the essential oil of aromatic herbs is obtained using hydrodistillation (HD). Because the emitted volatile fraction plays a fundamental role in a plant's life, various novel techniques have been developed for its extraction from plants. Among these, headspace solid phase microextraction (HS-SPME) can be used to obtain a rapid fingerprint of a plant's headspace. Daucus crinitus Desf. is a wild plant that grows along the west coast of Algeria. Only a single study ...

  14. Dynamic headspace analysis of fresh tomato juices.

    Science.gov (United States)

    Sucan, M K; Russell, G F

    2001-01-01

    The methods used to isolate volatile compounds for GC analyses can cause profound effects on the quantitative and qualitative composition of the injected sample, and exert a great influence in the resultant bioactivity of volatiles. Especially with plant tissues like tomatoes, the isolation of volatile constituents using classical methods may yield results which are not representative of the chemicals present in the natural material. Headspace sampling methods may be advantageous in capturing the same volatile compounds emitted from tomatoes that are detected by the human nose. This study utilized an extremely sensitive dynamic headspace sampling with thermal desorption method to determine volatile components of fresh tomato juices. The method proved very sensitive for the isolation of tomato volatiles and concentrations of flavor compounds were much greater than related literature studies.

  15. Headspace liquid-phase microextraction of methamphetamine and amphetamine in urine by an aqueous drop

    Energy Technology Data Exchange (ETDEWEB)

    He Yi [Department of Sciences, John Jay College of Criminal Justice, City University of New York, 445 W 59th Street, New York, NY 10019 (United States)]. E-mail: yhe@jjay.cuny.edu; Vargas, Angelica [Department of Sciences, John Jay College of Criminal Justice, City University of New York, 445 W 59th Street, New York, NY 10019 (United States); Kang, Youn-Jung [Department of Sciences, John Jay College of Criminal Justice, City University of New York, 445 W 59th Street, New York, NY 10019 (United States)

    2007-04-25

    This study developed a headspace liquid-phase microextraction (LPME) method by using a single aqueous drop in combination with high performance liquid chromatography (HPLC)-UV detection for the determination of methamphetamine (MAP) and amphetamine (AP) in urine samples. The analytes, volatile and basic, were released from sample matrix into the headspace first, and then protonated and dissolved in an aqueous H{sub 3}PO{sub 4} drop hanging in the headspace by a HPLC syringe. After extraction, this drop was directly injected into HPLC. Parameters affecting extraction efficiency were investigated and optimized. This method showed good linearity in the investigated concentration range of 1.0-1500 {mu}g L{sup -1}, repeatability of the extraction (R.S.D. < 5%, n = 6), and low detection limits (0.3 {mu}g L{sup -1} for both analytes). Enrichment factors of about 400-fold and 220-fold were achieved for MAP and AP, respectively, at optimum conditions. The feasibility of the method was demonstrated by analyzing human urine samples.

  16. 顶空固相微萃取-气相色谱-质谱联用分析费约果叶片挥发性香气成分条件优化%Optimization of headspace solid phase micro-extraction combined with gas chromatography-mass spectrometry conditions of volatile flavor from Feijoa sellowiana leaves

    Institute of Scientific and Technical Information of China (English)

    白俊英; 黄仁华; 陆云梅; 余游; 王丹

    2016-01-01

    To establish the appropriate extraction conditions for the analysis of volatile constit-uents from Feijoa sellowiana leaves by headspace solid phase micro-extraction( HS-SPME ) combined with gas chromatography-mass spectrometry( GC-MS),the extraction conditions were investigated by orthogonal tests. The sum of the peak areas and total peak numbers of the volatile constituents were used as indices to optimize the extraction conditions by using L9(34) orthogonal array design. The results showed that the influence of temperature was larger and that of the sample amount was smaller for total peak numbers and peak areas. The optimum HS-SPME parameters were selected as follows:0. 6 g sample,extracted for 50 min at 50 ℃, and then desorbed for 6 min. Under these conditions,a total of 88 substances were detected. These substances can reflect the fragrant chemical components of Feijoa sellowiana leaves, and provide some references for the development and utilization of the leaves.%为了建立适合费约果叶片香气成分检测的顶空固相微萃取-气相色谱-质谱( HS-SPME-GC-MS)分析方法,考察HS-SPME中不同萃取条件对香气萃取效果的影响,采用L9(34)正交试验,以出峰个数和总峰面积为考察指标确定最佳萃取条件。结果表明,萃取温度对出峰个数和总峰面积的影响较大,而加样量的影响较小。实验得出的较优萃取条件为:加样量0.6 g,萃取温度50℃,萃取时间50 min,解吸时间6 min。在此萃取条件下能够得到88种物质,这些物质能更真实地反映费约果叶片香气成分的化学构成,为费约果叶片的开发利用提供有价值的数据。

  17. Headspace solid-phase microextraction for wine volatile analysis.

    Science.gov (United States)

    Azzi-Achkouty, Samar; Estephan, Nathalie; Ouaini, Naïm; Rutledge, Douglas N

    2017-07-03

    The most commonly used technique to prepare samples for the analysis of wine volatile is the headspace solid-phase microextraction (HS-SPME). This method has gained popularity in last few years, as it is a unique solventless preparation technique. In this paper, a summary of recently published studies using HS-SPME for the analysis of wine aromas, with special emphasis on the method developed, has been compiled. Several papers are discussed in detail, mainly with respect to the SPME conditions used. A brief summary of the reviews related to HS-SPME analysis is given and discussed. Several parameters affecting the HS-SPME, such as the salt concentration and the agitation conditions, are used in the same way as used in several papers. The HS-SPME extraction proved to be sufficiently sensitive to satisfy legislative requirements related to low detection and quantification limits as well as method accuracy and precision requirements. However, in order to achieve the best performance and precision, the protocol needs to be optimized for each case. The effect of different parameters must be well characterized to ensure correct extraction and desorption to ensure the transfer of extracted compounds into the analytical system. The operating parameters, such as time, temperature, and agitation, must then be kept constant for all the samples.

  18. Simultaneous Determination of Alkoxyalcohols in Wet Wipes Using Static Headspace Gas Chromatography and Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lee, So Jin; Pyo, Hee Soo; Chung, Bong Chul; Lee, Jeon Gae [KIST, Seoul (Korea, Republic of); Kim, Hai Dong [Kyung Hee University, Seoul (Korea, Republic of)

    2014-09-15

    Alkoxyalcohols are used as solvents or preservatives in various consumer products such as wet wipes. The metabolites of alkoxyalcohols are known to be chronically toxic and carcinogenic to animals. Thus, an analytical method is needed to monitor alkoxyalcohols in wet wipes. The aim of this study was to develop a simultaneous analytical method for 14 alkoxyalcohols using headspace gas chromatography coupled with mass spectrometry to analyze the wet wipes. This method was developed by comparing with various headspace extraction parameters. The linear calibration curves were obtained for the method (r2 > 0.995). The limit of detection of alkoxyalcohols ranged from 2 to 200 ng mL-1. The precision of the determinative method was less than 18.20% coefficient of variation both intra and inter days. The accuracy of the method ranged from 82.86% to 119.83%. (2-Methoxymethylethoxy)propanol, 2-phenoxyethanol, and 1-phenoxy-2-propanol were mainly detected in wet wipes.

  19. GNS Castor V/21 Headspace Gas Sampling 2014

    Energy Technology Data Exchange (ETDEWEB)

    Winston, Philip Lon [Idaho National Lab. (INL), Idaho Falls, ID (United States)

    2016-01-01

    Prior to performing an internal visual inspection, samples of the headspace gas of the GNS Castor V/21 cask were taken on June 12, 2014. These samples were taken in support of the CREIPI/Japanese nuclear industry effort to validate fuel integrity without visual inspection by measuring the 85Kr content of the cask headspace

  20. Furanic compounds and furfural in different coffee products by headspace liquid-phase micro-extraction followed by gas chromatography-mass spectrometry: survey and effect of brewing procedures.

    Science.gov (United States)

    Chaichi, Maryam; Ghasemzadeh-Mohammadi, Vahid; Hashemi, Maryam; Mohammadi, Abdorreza

    2015-01-01

    In this study, the levels of furan, 2-methylfuran, 2,5-dimethylfuran, vinyl furan, 2-methoxymethyl-furan and furfural in different coffee products were evaluated. Simultaneous determination of these six furanic compounds was performed by a head space liquid-phase micro-extraction (HS-LPME) method. A total of 67 coffee powder samples were analysed. The effects of boiling and espresso-making procedures on the levels of furanic compounds were investigated. The results showed that different types of coffee samples contained different concentrations of furanic compounds, due to the various processing conditions such as temperature, degree of roasting and fineness of grind. Among the different coffee samples, the highest level of furan (6320 µg kg⁻¹) was detected in ground coffee, while coffee-mix samples showed the lowest furan concentration (10 µg kg⁻¹). Levels in brewed coffees indicated that, except for furfural, brewing by an espresso machine caused significant loss of furanic compounds.

  1. Headspace analysis of foams and fixatives

    Energy Technology Data Exchange (ETDEWEB)

    Harper, Kyle [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Truong, Thanh-Tam [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Magwood, Leroy [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Peters, Brent [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Nicholson, James [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Washington, II, Aaron L. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2017-07-27

    In the process of decontaminating and decommissioning (D&D) older nuclear facilities, special precautions must be taken with removable or airborne contamination. One possible strategy utilizes foams and fixatives to affix these loose contaminants. Many foams and fixatives are already commercially available, either generically or sold specifically for D&D. However, due to a lack of revelant testing in a radioactive environment, additional verification is needed to confirm that these products not only affix contamination to their surfaces, but also will function in a D&D environment. Several significant safety factors, including flammability and worker safety, can be analyzed through the process of headspace analysis, a technique that analyzes the off gas formed before or during the curing process of the foam/fixative, usually using gas chromatography-mass spectrometry (GC-MS). This process focuses on the volatile components of a chemical, which move freely between the solid/liquid form within the sample and the gaseous form in the area above the sample (the headspace). Between possibly hot conditions in a D&D situation and heat created in a foaming reaction, the volatility of many chemicals can change, and thus different gasses can be released at different times throughout the reaction. This project focused on analysis of volatile chemicals involved in the process of using foams and fixatives to identify any potential hazardous or flammable compounds.

  2. Analysis of Volatile Components in Mulberry Fruit Vinegar by Headspace Solid-phase Micro-extraction Coupled with GC-MS%顶空固相微萃取与气相色谱-质谱联用分析桑椹果醋挥发性成分

    Institute of Scientific and Technical Information of China (English)

    梁贵秋; 李全; 吴婧婧; 陆飞; 肖更生; 周晓玲; 陆春霞

    2012-01-01

    In order to evaluate the aroma characteristics of mulberry fruit vinegar, the method of headspace solid-phase micro-extraction was used to extract volatile components in mulberry fruit vinegar, and the technique of gas chromatogra-phy-mass spectrometry (GC-MS) was adopted to analyze these compounds. After search and comparison in NIST 05 spectrum database, 40 kinds of compounds were detected in mulberry fruit vinegar. The relative contents of some compounds were determined with peak area normalization method. The results showed that organic acids, alcohols, esters and aldehydes were the major aroma compounds in mulberry fruit vinegar. It was preliminarily identified that the unique aroma of mulberry fruit vinegar came from phenethyl alcohol, phenethyl cinnamate, ethyl caprylate, hexanoic acid ethyl ester, benzaldehyde, phenylacetaldehyde, and pelargonic aldehyde. These different kinds of aroma compounds give off sweet honey rose aroma, fruity aroma, flowery aroma, fatty acid taste, almond flavor, sweet flavor and fragrance of rose flower respectively, and their synergistic effect attributes to the special fragrance of mulberry vinegar.%为了评价桑椹果醋的香气特征,利用顶空固相微萃取法提取桑椹果醋中的挥发性成分,并采用气相色谱-质谱(GC-MS)技术进行分析.经过NIST05谱库检索对比,在桑椹果醋中共检测出40种化合物.利用峰面积归一法测定部分化合物的相对含量,其中有机酸类、醇类、酯类和醛类是桑椹果醋中含量最高的气味化合物.初步得出构成桑椹果醋特有香气的化合物为苯乙醇、肉桂酸苯乙酯、辛酸乙酯、癸酸乙酯、苯甲醛、苯乙醛、壬醛等.这些不同种类香味化合物分别具有的蜜香玫瑰味、水果香气、花香气、脂肪酸味、杏仁味、甜香味和玫瑰花香,共同作用构成了桑椹果醋的特有香气.

  3. Comparison of Three Methods for Extraction of Volatile Lipid Oxidation Products from Food Matrices for GC-MS Analysis

    DEFF Research Database (Denmark)

    Jacobsen, Charlotte; Yesiltas, B.; Berner, Lis

    GC based methods are often used for determination of volatile oxidation products such as pentanal and hexanal. Different extraction methods for extracting volatiles before GC analysis can be used, e.g static headspace, dynamic headspace and solid phase microextraction (SPME). Traditionally, dynamic...... headspace extraction has been performed manually. Recently, automated dynamic headspace methods have become available. This presentation will summarize the principles of the different extraction methods. Moreover, results from fish oil, oil-in-water emulsion and milk obtained with SPME, manual dynamic...... headspace or automated dynamic headspace (TDU/DHS) extraction followed by GC-MS analysis will be compared. In all cases, concentrations of volatiles were quantified by calibration curves by addition of selected standards to oil, emulsion or milk. The results show that the linearity of calibration curves...

  4. Development of a syringe pump assisted dynamic headspace sampling technique for needle trap device.

    Science.gov (United States)

    Eom, In-Yong; Niri, Vadoud H; Pawliszyn, Janusz

    2008-07-04

    This paper describes a new approach that combines needle trap devices (NTDs) with a dynamic headspace sampling technique (purge and trap) using a bidirectional syringe pump. The needle trap device is a 22-G stainless steel needle 3.5-in. long packed with divinylbenzene sorbent particles. The same sized needle, without packing, was used for purging purposes. We chose an aqueous mixture of benzene, toluene, ethylbenzene, and p-xylene (BTEX) and developed a sequential purge and trap (SPNT) method, in which sampling (trapping) and purging cycles were performed sequentially by the use of syringe pump with different distribution channels. In this technique, a certain volume (1 mL) of headspace was sequentially sampled using the needle trap; afterwards, the same volume of air was purged into the solution at a high flow rate. The proposed technique showed an effective extraction compared to the continuous purge and trap technique, with a minimal dilution effect. Method evaluation was also performed by obtaining the calibration graphs for aqueous BTEX solutions in the concentration range of 1-250 ng/mL. The developed technique was compared to the headspace solid-phase microextraction method for the analysis of aqueous BTEX samples. Detection limits as low as 1 ng/mL were obtained for BTEX by NTD-SPNT.

  5. Volatile Constituents from leaves of Piper betle L by Head-space Solid Micro-extraction Coupled with GC-MS%HS-SPME-GC-MS分析蒟酱叶挥发性成分

    Institute of Scientific and Technical Information of China (English)

    尹震花; 王微; 顾海鹏; 康文艺

    2012-01-01

    To study the volatile constituents from leaves of Piper betle L. ,the volatiles were analyzed by head- space solid micro-extraction,coupled with GC-MS and Kovats indices for the first time. A quantitative analysis in percent was performed by peak area normalization measurements. The results showed that 27 compounds were identified from the leaves, accounting for 97.53% of the total essential constituents. The structure types of volatiles compounds included aldehyde, acids,esters,phenols,alkenes,aromatic hydrocarbons,and alkanes. 2-Methoxy-5-methylbenzaldehyde (42. 89% ) ,4-(2-propenyl)-phenol acetate ( 12. 49% ) ,2-methoxy-4-( 1-propenyl)-phenol ( 13. 42% ) ,4-allyl-l, 2-diace-toxybenzene (9.47% ) ,4-(2-propenyl)-phenol (2. 89% ) ,y-cadinene (2. 74% ) .eugenol (2. 66% ) and 2-methoxy-4-( 1-propenyl)-phenol acetate (2.06% ) were the main volatile constituents.%首次采用顶空固相微萃取和气质联用技术(HS-SPME-GCMS),结合保留指数法,用峰面积归一化法测定蒟酱叶中挥发性成分及相对百分含量.结果表明,从蒟酱叶中鉴别出27个化学成分,占峰面积的97.53%,化合物结构类型包括醛、酸、酯、酚、烯烃、芳香烃和(环)烷烃.2-甲氧基-5-甲基苯甲醛(42.89%)、胡椒酚醋酸酯(12.49%)、异丁香酚(13.42%)、4-烯丙基-1,2-二乙酰氧基苯(9.47%)、胡椒酚(2.89%)、γ-毕橙茄烯(2.74%)、丁香酚(2.66%)和乙酸异丁香酚酯(2.06%)是蒟酱叶的主要挥发性成分.

  6. Permeable sorptive walls for treatment of hydrophobic organic contaminant plumes in groundwater

    Energy Technology Data Exchange (ETDEWEB)

    Grathwohl, P.; Peschik, G. [Univ. of Tuebingen (Germany)

    1997-12-31

    Highly hydrophobic contaminants are easily adsorbed from aqueous solutions. Since for many of these compounds sorption increases with increasing organic carbon content natural materials such as bituminous shales and coals may be used in permeable sorptive walls. This, however, only applies if sorption is at equilibrium, which may not always be the case in groundwater treatment using a funnel-and-gate system. In contrast to the natural solids, granular activated carbons (GACs) have very high sorption capacities and reasonably fast sorption kinetics. The laboratory results show that application of GACs (e.g. F100) is economically feasible for in situ removal of polycyclic aromatic hydrocarbons (PAH) from groundwater at a former manufactured gas plant site (MGP). For less sorbing compounds (such as benzene, toluene, xylenes) a combination of adsorption and biodegradation is necessary (i.e. sorptive + reactive treatment).

  7. Determination of 11 quinolones in bovine milk using immunoaffinity stir bar sorptive microextraction and liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Yao, Kai; Zhang, Wei; Yang, Linyan; Gong, Jianfang; Li, Liuan; Jin, Tianming; Li, Cun

    2015-10-15

    A sensitive, selective and reproducible immunoaffinity stir bar sorptive microextraction (SBSME) coupled with liquid chromatography-fluorescence method for determination of 11 quinolones (QNs) in bovine milk was developed and validated. It is first report of a broad-specificity monoclonal antibody to QNs that has been immobilized to glass bar for preparation of a re-usable immunoaffinity stir bar. Analytes were extracted by placing stir bar in milk and shaking on a rotary shaker for 30min at 30rpm, followed by liquid chromatography and fluorescence detection. The newly developed method has limits of detection for each QN from 0.05 to 0.1ng/g with intra-day and inter-day precision ranging from 3.2 to 11.9% and from 5.2 to 12.5%, respectively. This allowed us to quantitatively analyze drugs in bovine milk with the advantage of significantly simplified sample preparation. The proposed method was successfully applied to the bovine milk samples analyses with QNs, demonstrating its rare application in animal food safety analysis.

  8. An Analytical Method for Relationship Between Hydraulic Diffusivity and Soil Sorptivity

    Institute of Scientific and Technical Information of China (English)

    WANG Quan-Jiu; ZHANG Jiang-Hui; FAN Jun

    2006-01-01

    A simple method was developed to relate soil sorptivity to hydraulic diffusivity and water absorption experiments were conducted utilizing one-dimensional horizontal soil columns to validate the relationship. In addition, an estimation method for hydraulic diffusivity with disc infiltrometer was developed. The results indicated a favorable fit of the theoretical relation to the experimental data. Also, the experiment with disc infiltrometer for estimating the diffusivity showed that the new method was feasible.

  9. Headspace chromatographic determination of water pollutants

    Energy Technology Data Exchange (ETDEWEB)

    Otson, R.; Williams, D.T.

    1982-05-01

    A readily constructed, automated purging assembly, on-column trapping, and simultaneous use of flame ionization and electrolytic conductivity detectors were applied to develop a dynamic headspace gas chromatographic technique which was evaluated for the determination of 42 organic polluants in water. Detection limits of <1 ..mu..g/L and linear plots of peak area against concentration in the range 0.25-16 ..mu..g/L were obtained for 32 compounds. At aqueous concentrations of 4 and 16 ..mu..g/L, peak area precision of <10% relative standard deviation (RSD) for triplicate sample analysis and purging efficiencies of >75% were generally obtained. Storage of aqueous composite standard solutions at 4 and 16 ..mu..g/L for 6 weeks at 4/sup 0/C did not usually affect analytical results by more than +/- 15%.

  10. Volatile Constituents from Three Parts of Cucurbita Moschata Duch. (Miben) by Head-Space Solid Phase Micro-Extraction Coupled with GC-MS%HS-SPME-GC-MS分析蜜本南瓜3个部位的挥发性成分

    Institute of Scientific and Technical Information of China (English)

    张伟; 彭涛; 卢引; 顾雪竹; 李昌勤; 康文艺

    2013-01-01

    This study was aimed to analyze the volatile constituents from flower, stem tip and seed of Cucurbita moschata Duch.(Miben). The volatiles were analyzed by head-space solid micro-extraction, coupled with GC-MS and Kovats indices for the first time . The results showed that 22 compounds were identified from the flower , 20 from the stem tip and 21 from the seed of the C. moschata (Miben). The total essential constituents from each part were 91 . 89%, 89 . 24% and 96 . 26%, respectively . A total of 10 compounds in the flower and stem tip were mutual. And 3 compounds in the flower, stem tip and seed were mutual. It was concluded that the β-bourbonene (17.57%) and heneicosane (11.90%) were the highest components of the total essential constituents of the flower of C. moschata (Miben). Decanal (28.77%) was the highest components of the stem tip and hexadecanoic acid ethyl ester (29.12%), 2,3-butanediol (16.90%) and linoleic acid ethyl ester (16.52%) were the highest compo-nents of seed of C. moschata (Miben).%目的:对蜜本南瓜花、茎尖和籽的挥发性成分进行分析。方法:采用顶空固相微萃取和气质联用技术(HS-SPME-GC-MS),结合保留指数法,首次分析蜜本南瓜3个部位的挥发性成分。结果:从蜜本南瓜花、茎尖、籽中分别鉴定出22、20和21个挥发性成分,占总峰面积的91.89%、89.24%和96.26%。其中花和茎尖共有10个共有成分,花、茎尖和籽有3个共有成分。结论:蜜本南瓜花中茁-波旁烯(17.57%)和二十一烷(11.90%)含量较高;蜜本南瓜茎尖中癸醛(28.77%)含量最高;籽中棕榈酸乙酯(29.12%)、2,3-丁二醇(16.90%)和亚油酸乙酯(16.52%)含量较高。

  11. 顶空萃取-气相色谱-质谱法测定一种儿童专用防痱止痒水的挥发性成分%Analysis of Volatile Flavor Components in One Type of Remove Philippine and Itching Water by Headspace Extraction-GC/MS

    Institute of Scientific and Technical Information of China (English)

    李红; 熊爽; 田福林; 赵海波

    2011-01-01

    采用顶空萃取-气相色谱/质谱法分析鉴定防痱止痒水的挥发性成分。结果表明:共检测出35种挥发性成分,主要成分为乙醇和酞酸二乙酯,其它成分主要包括醇、烯、酯、甘菊环等。检出的物质中,α-蒎烯、β-蒎烯、莰烯、桉叶醇、樟脑、α-萜品醇、龙脑、醋酸异龙脑酯、石竹烯为野菊花挥发油的有效成分;苯甲酸甲酯、苯甲酸苄酯、丁香酚为金银花挥发油的有效成分;广藿香醇为广藿香提取物的主要成分。α-蒎烯、β-月桂烯、β-蒎烯、莰烯、薄荷醇、丁香酚等成分都具有较强的驱避蚊虫的作用。%The volatile components in one type of remove philippine and itching water were analyzed by headspace extraction-gas chromatography-mass spectrometry(HS-GC/MS).The results showed that HS-GC/MS is effective in the analysis of remove philippine and itching water.35 components are separated and identified.The main components are ethyl alcohol and diethyl phthalate acid,the others are alcohols,terpenes,esters and azulenes.alpha.-Pinene,beta.-pinene,camphene,eucalyptol,camphor,p-menth-1-en-8-ol,borneol,isobornyl acetate,caryophyllene are the effective components of the volatile oil in chrysanthemum indicum L.Benzoic acid methyl ester,benzyl benzoate,eugenol are the effective components of the volatile oil in flos lonicerae.Patchouli alcohol is the effective components of the volatile oil in pogostemon cablin(blanco) benth.alpha.-Pinene,beta.-myrcene,beta.-pinene,camphene,menthol,eugenol are all effictive repellent.

  12. Detection of Pyrazine Compounds in Cocoa Wort by Gas Chromatography with Headspace Solid Phase Micro-Extraction%顶空-固相微萃取-气相色谱法检测可可麦汁中吡嗪类化合物

    Institute of Scientific and Technical Information of China (English)

    肖天鹏; 郑晓峰; 吕吉鸿; 郭泽峰; 高峰; 刘春凤; 李崎

    2012-01-01

    A headspace solid phase microextraction (HS-SPME), followed by gas chromatographic method was established for the detection of three pyrazine compounds (2,5-dimethyl pyrazine, 2,3,5-trimethyl pyrazine and 2,3, 5, 6-tetramethyl pyrazine) in cocoa wort. Equilibrium temperature and equilibrium time were optimized by using different SPME heads. According to the results of the optimization experiments, the following conclusion can be drawn: The cocoa wort sample was efficiently extracted under 40 ℃ for 40 min with 75 urn CAR/PDMS SPME head. The method had linear response within 1 - 500 mg/L, and the detection limits (S/N=3) were below 0. 023 礸/L. The relative standard deviations were from 3. 6%-6. 4% and the recoveries were from 95. A% to 102. 7%. This method is characterized by rapidly, high sensitivity, good linearity and repeatability for the analysis of cocoa wort samples.%建立了顶空-固相微萃取(HS-SPME)-气相色谱快速测定可可麦汁中3种吡嗪类物质(2,5-二甲基吡嗪、2,3,5-三甲基吡嗪和2,3,5,6-四甲基吡嗪)的方法.选择不同的固相微萃取头对萃取温度和时间进行优化,所得最佳萃取条件为:在60℃下,采用75 μm CAR/PDMS萃取头对麦汁样品萃取40 min.本方法的检出限(S/N=3)为0.023~ 0.056 μg/L,线性范围1~500 mg/L;相对标准偏差为3.6%~6.4%;回收率为95.4%~102.7%.本方法应用于样品检测,发现可可麦汁中吡嗪的浓度与原料中可可粉的添加量正相关,显示了很好灵敏性.

  13. Analysis of Volatile Constituents from the Fresh Leaves of Pelargonium odoratissimum(L.)L Her.ex Ait.by Headspace Solid-Phase Micro Extraction and Gas Chromatography-Mass Spectrometry%豆蔻天竺葵鲜叶挥发性成分的HS-SPME/GC-MS分析

    Institute of Scientific and Technical Information of China (English)

    王建刚

    2011-01-01

    [目的]研究豆蔻天竺葵鲜叶中的挥发性成分.[方法]采用顶空固相微萃取(HS-SPME)和气相色谱质谱联用(GC-MS)技术对豆蔻天竺葵鲜叶挥发性化学成分进行分离鉴定,用色语峰面积归一化法确定各组分的相对含量.[结果]从豆蔻天竺葵叶挥发性物质中分离出了68个组分,鉴定出了61个组分,并测定了各组分相对含量,包括D-柠檬烯(61.18%),芳樟醇(4.09%),大牻牛儿烯(3.38%),4-蒈烯(2.92%),按叶醇(1.31%),α-蒎烯(2.19%),桧烯(2.15%),异松油烯(2.86%),1,7,7-三甲基双环[2.2.1]庚-2-乙酸酯(1.98%)等.[结论]通过对豆蔻天竺葵挥发性成分的研究,为豆蔻天竺葵资源的进一步开发利用提供了试验依据.%[Objective] To analyze volatile constituents from the fresh leaves of Pelargonium odoratissimum (L. ) L Her. Ex Ait.. [ Method] Volatile constituents were isolated from fresh leaves of Pelargonium odoratissimum (L. ) L Her. Ex Ait. And identified by headspace solid-phase micro extraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS), contents of which were determined by area normalization method. [ Result ] 68 constituents were isolated, 61 of which were identified including D-limonene (61.18%), linalool (4.09% ) , germacrene (3.38%), 4-carene (2.92%), eucalyptol (1.31%), alpha-pinene (2.19%), sabinene (2.15%), terpinolene (2.86%) and 1, 7, 7-trime-thylbicyclo [2.2.1] hept-2-yl acetate(1.98% ). [Conclusion] The study on the volatile constituents could provide a test basis for further development and utilization of Pelargonium odoratissimum ( L. ) L Her. Ex Ait. Resources.

  14. Application of headspace solid phase microextraction for study of noncovalent interaction of borneol with human serum albumin

    Institute of Scientific and Technical Information of China (English)

    Liang HU; Dong-ying CHEN

    2009-01-01

    Aim: To investigate noncovalent interactions between borneol and human serum albumin (HSA) under near-physiological conditions. Methods: A 65-um polydimethylsiloxane (PDMS) fiber was selected for sampling. The extraction temperature was kept at 37 ℃, and the extraction time was optimized at 10 min. Borneol solutions of different concentrations were equilibrated in 600 umol/L HSA and 67 mmol/L phosphate buffer solution (pH 7.4,37 ℃) for 24 h prior to solid phase microextraction (SPME) using headspace mode. The binding properties were obtained based on the calculation of extracted borneol amount using gas chromatography (GC) determination. Results: The headspace SPME extraction method avoided disturbance from the HSA binding matrix. The recovery showed good linearity for the borneol concentrations over the range of 0.4-16.3 μmol/L with a regression coefficient (R~2) of 0.9998. The limit of detection and lower limit of quantitation were determined to be 0.01 umol/L and 0.4 umol/L, respectively. The binding constant and the percentage binding rate were estimated to be 2.4×10~3(mol/L)~(-1) and 59.5%, respectively.Conclusion: Headspace SPME coupled to GC is a simple, sensitive and rapid method for the study of borneol binding to HSA. The method may be applied in the determination of other protein binding properties in human plasma.

  15. Microwave-assisted headspace single-drop microextration of chlorobenzenes from water samples.

    Science.gov (United States)

    Vidal, Lorena; Domini, Claudia E; Grané, Nuria; Psillakis, Elefteria; Canals, Antonio

    2007-05-29

    A one-step and in-situ sample preparation method used for quantifying chlorobenzene compounds in water samples has been developed, coupling microwave and headspace single-drop microextraction (MW-HS-SDME). The chlorobenzenes in water samples were extracted directly onto an ionic liquid single-drop in headspace mode under the aid of microwave radiation. For optimization, a Plackett-Burman screening design was initially used, followed by a mixed-level factorial design. The factors considered were: drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time, ionic liquid type, microwave power and length of the Y-shaped glass-tube. The optimum experimental conditions found from this statistical evaluation were: a 5 microL microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate exposed for 20 min to the headspace of a 30 mL aqueous sample, irradiated by microwaves at 200 W and placed in a 50 mL spherical flask connected to a 25 cm Y-shaped glass-tube. Under the optimised experimental conditions, the response of a high performance liquid chromatographic system was found to be linear over the range studied and with correlation coefficients ranging between 0.9995 and 0.9999. The method showed a good level of repeatability, with relative standard deviations varying between 2.3 and 8.3% (n=5). Detection limits were found in the low microg L(-1) range varying between 0.016 and 0.039 microg L(-1). Overall, the performance of the proposed method demonstrated the favourable effect of microwave sample irradiation upon HS-SDME. Finally, recovery studies from different types of environmental water samples revealed that matrix had little effect upon extraction.

  16. Microwave-assisted headspace single-drop microextration of chlorobenzenes from water samples

    Energy Technology Data Exchange (ETDEWEB)

    Vidal, Lorena [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Domini, Claudia E. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Grane, Nuria [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Psillakis, Elefteria [Department of Environmental Engineering, Technical University of Crete, Polytechneioupolis, GR-73100 Chania, Crete (Greece); Canals, Antonio [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain)]. E-mail: a.canals@ua.es

    2007-05-29

    A one-step and in-situ sample preparation method used for quantifying chlorobenzene compounds in water samples has been developed, coupling microwave and headspace single-drop microextraction (MW-HS-SDME). The chlorobenzenes in water samples were extracted directly onto an ionic liquid single-drop in headspace mode under the aid of microwave radiation. For optimization, a Plackett-Burman screening design was initially used, followed by a mixed-level factorial design. The factors considered were: drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time, ionic liquid type, microwave power and length of the Y-shaped glass-tube. The optimum experimental conditions found from this statistical evaluation were: a 5 {mu}L microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate exposed for 20 min to the headspace of a 30 mL aqueous sample, irradiated by microwaves at 200 W and placed in a 50 mL spherical flask connected to a 25 cm Y-shaped glass-tube. Under the optimised experimental conditions, the response of a high performance liquid chromatographic system was found to be linear over the range studied and with correlation coefficients ranging between 0.9995 and 0.9999. The method showed a good level of repeatability, with relative standard deviations varying between 2.3 and 8.3% (n = 5). Detection limits were found in the low {mu}g L{sup -1} range varying between 0.016 and 0.039 {mu}g L{sup -1}. Overall, the performance of the proposed method demonstrated the favourable effect of microwave sample irradiation upon HS-SDME. Finally, recovery studies from different types of environmental water samples revealed that matrix had little effect upon extraction.

  17. "Aqua-space", a new headspace method for isolation of natural floral aromas using humidified air as a carrier gas.

    Science.gov (United States)

    Ishikawa, Masashi; Honda, Tsutomu; Fujita, Akira; Kurobayashi, Yoshiko; Kitahara, Takeshi

    2004-02-01

    A new method called "Aqua-space" was developed for the isolation of the natural fragrances of plants. Living flowers were enclosed in a space under simulated natural conditions, and humidified air was pumped into the space as a fragrance carrier. In a comparison among three isolation methods, i.e., Aqua-space, headspace, and solvent extraction, the Aqua-space method proved to be the most effective in retaining natural fragrances with abundant oxygenated components key to floral fragrances.

  18. Modelling infiltration and geostatistical analysis of spatial variability of sorptivity and transmissivity in a flood spreading area

    Energy Technology Data Exchange (ETDEWEB)

    Haghighi-Fashi, F.; Sharifi, F.; Kamali, K.

    2014-06-01

    Knowledge of infiltration characteristics is useful in hydrological studies of agricultural soils. Soil hydraulic parameters such as steady infiltration rate, sorptivity, and transmissivity can exhibit appreciable spatial variability. The main objectives of this study were to examine several mathematical models of infiltration and to analyze the spatial variability of observed final infiltration rate, estimated sorptivity and estimated transmissivity in flood spreading and control areas in Ilam province, Iran. The suitability of geostatistics to describe such spatial variability was assessed using data from 30 infiltration measurements sampled along three lines. The Horton model provided the most accurate simulation of infiltration considering all measurements and the Philips two-term model provided less accurate simulation. A comparison of the measured values and the estimated final infiltration rates showed that the Kostiakov- Lewis, Kostiakov, and SCS models could not estimate the final infiltration rate as well as Horton model. Estimated sorptivity and transmissivity parameters of the Philips two-term model and final infiltration rate had spatial structure, and were considered to be structural variables over the transect pattern. The Gaussian model provided the best-fit theoretical variogram for these three parameters. Variogram values ranged from 99 and 88 m for sorptivity and final infiltration rate to 686 (spherical) and 384 m (Gaussian) for transmissivity. Sorptivity, transmissivity and final infiltration attributes showed a high degree of spatial dependence, being 0.99, 0.81 and 1, respectively. Results showed that kriging could be used to predict the studied parameters in the study area. (Author)

  19. Use of volatile organic solvents in headspace liquid-phase microextraction by direct cooling of the organic drop using a simple cooling capsule.

    Science.gov (United States)

    Ghiasvand, Ali Reza; Yazdankhah, Fatemeh; Hajipour, Somayeh

    2016-08-01

    A low-cost and simple cooling-assisted headspace liquid-phase microextraction device for the extraction and determination of 2,6,6-trimethyl-1,3 cyclohexadiene-1-carboxaldehyde (safranal) in Saffron samples, using volatile organic solvents, was fabricated and evaluated. The main part of the cooling-assisted headspace liquid-phase microextraction system was a cooling capsule, with a Teflon microcup to hold the extracting organic solvent, which is able to directly cool down the extraction phase while the sample matrix is simultaneously heated. Different experimental factors such as type of organic extraction solvent, sample temperature, extraction solvent temperature, and extraction time were optimized. The optimal conditions were obtained as: extraction solvent, methanol (10 μL); extraction temperature, 60°C; extraction solvent temperature, 0°C; and extraction time, 20 min. Good linearity of the calibration curve (R(2) = 0.995) was obtained in the concentration range of 0.01-50.0 μg/mL. The limit of detection was 0.001 μg/mL. The relative standard deviation for 1.0 μg/mL of safranal was 10.7% (n = 6). The proposed cooling-assisted headspace liquid-phase microextraction device was coupled (off-line) to high-performance liquid chromatography and used for the determination of safranal in Saffron samples. Reasonable agreement was observed between the results of the cooling-assisted headspace liquid-phase microextraction high-performance liquid chromatography method and those obtained by a validated ultrasound-assisted solvent extraction procedure.

  20. Comparison of Methanol and Tetraglyme as Extraction Solvents for Determination of Volatile Organics in Soil

    Science.gov (United States)

    1987-11-01

    determining volatile organics in soil can be classified into thefollowing groups: 1. Static or dynamic headspace analysis 2. Solvent extraction-direct...methods based on the dynamic headspace method whereby the volatiles are stripped from a soil/water slurry using a conventional purge-and-trap instrument...651. Brazell, R.S. and MP. Maskarinec (1981) Dynamic headspace analysis of solid waste materials. Journal of High Resolution Chromatography and

  1. Systematic comparison of static and dynamic headspace sampling techniques for gas chromatography.

    Science.gov (United States)

    Kremser, Andreas; Jochmann, Maik A; Schmidt, Torsten C

    2016-09-01

    Six automated, headspace-based sample preparation techniques were used to extract volatile analytes from water with the goal of establishing a systematic comparison between commonly available instrumental alternatives. To that end, these six techniques were used in conjunction with the same gas chromatography instrument for analysis of a common set of volatile organic carbon (VOC) analytes. The methods were thereby divided into three classes: static sampling (by syringe or loop), static enrichment (SPME and PAL SPME Arrow), and dynamic enrichment (ITEX and trap sampling). For PAL SPME Arrow, different sorption phase materials were also included in the evaluation. To enable an effective comparison, method detection limits (MDLs), relative standard deviations (RSDs), and extraction yields were determined and are discussed for all techniques. While static sampling techniques exhibited sufficient extraction yields (approx. 10-20 %) to be reliably used down to approx. 100 ng L(-1), enrichment techniques displayed extraction yields of up to 80 %, resulting in MDLs down to the picogram per liter range. RSDs for all techniques were below 27 %. The choice on one of the different instrumental modes of operation (aforementioned classes) was thereby the most influential parameter in terms of extraction yields and MDLs. Individual methods inside each class showed smaller deviations, and the least influences were observed when evaluating different sorption phase materials for the individual enrichment techniques. The option of selecting specialized sorption phase materials may, however, be more important when analyzing analytes with different properties such as high polarity or the capability of specific molecular interactions. Graphical Abstract PAL SPME Arrow during the extraction of volatile analytes from the headspace of an aqueous sample.

  2. Solid phase microextraction (SPME) for extraction of volatile oxidation products from complex food systems – Pros and cons

    DEFF Research Database (Denmark)

    Jacobsen, Charlotte; Horn, Anna Frisenfeldt; Lu, Henna Fung Sieng

    Volatile secondary lipid oxidation products can be identified and quantified by GC-FID or GC-MS. An extraction step is, however, needed before GC analysis. A range of different extraction methods are available such as static headspace, dynamic headspace and SPME. Each of these methods has its adv...

  3. Is Solid Phase Microextraction (SPME) an appropriate method for extraction of volatile oxidation products from complex food systems

    DEFF Research Database (Denmark)

    Jacobsen, Charlotte; Horn, Anna Frisenfeldt; Lu, Henna Fung Sieng

    Volatile secondary lipid oxidation products can be identified and quantified by GC-FID or GC-MS. An extraction step is, however, needed before GC analysis. A range of different extraction methods are available such as static headspace, dynamic headspace and SPME. Each of these methods has its adv...

  4. Study about the capillary absorption and the sorptivity of concretes with Cuban limestone aggregates

    OpenAIRE

    Howland, J. J.; Martín, A. R.

    2013-01-01

    The objective of this study was to demonstrate the possibility to obtain concretes in Cuba with values of effective porosity below of 10%, using limestone aggregates with high levels of absorption (higher than 1% in many cases), and values of Sorptivity below of 5 x 10-5 m/s1/2 as is established in the document prepared by the DURAR Latin Working Group, for structures exposed to very aggressive environments. The experimental results showed that the use of the trial method of capillary absorpt...

  5. 顶空固相微萃取-气相色谱-质谱法测定苦杏仁中苦杏仁苷含量%GC-MS Determination of Amygdalins in Bitter Almond with Sample Treatment by Head-space Solid Phase Micro-extraction

    Institute of Scientific and Technical Information of China (English)

    韩素芳; 丁明; 刘亚群; 陈顺伟

    2011-01-01

    采用顶空固相微萃取-气相色谱-质谱法对苦杏仁中苦杏仁苷进行了测定。0.1g苦杏仁样品及4mol·L^-1硫酸4mL置于25mL顶空瓶中,于沸水浴水解15min。PDMS/DVB萃取头顶空萃取20min,萃取头于气相色谱进样口解析1min。采用HP-5MS色谱柱在程序升温条件下进行分离。用氦气为载气,流量为1.0mL·min^-1,质谱分析中采用电子轰击电离源(230℃,70eV),并在40-600amu质量数范围内进行全扫描。结果表明:方法在100μg·g^-1以内呈线性。采用此法对市售苦杏仁中苦杏仁苷含量测定结果为60.43μg·g^-1,与分光光度法结果相符。样品5次测定结果相对标准偏差为1.8%;60μg·g^-1。及20μg·g^-1两个水平添加回收率均在90%以上。%The sample of bitter almond (0. 1 g) was hydrolyzed with 4 mol · L^-1 H2SO4 in a 25 mL headspace bottle heated in a boiling water bath for 15 min, and then extracted by SPME with the PDMS/DVB extractor for 20 min. The extractor was desorbed for 1 min at the inlet of the gas chromatograph, and separation of amygdalin was carried out on the HP-5MS chromatographic column with programmed temperature elevation. Helium with flow-rate of 1.0 mL · min ^-1 was used as carrier gas. Electron bombardment ionization (230 ℃, 70 eV) and whole scanning in the mass range of 40-600 ainu were adopted in MS analysis. Linearity was obtained in the range within 100μg · g^-1 . A sample of bitter almond was analyzed by this method, value of amygdalin content of 60. 43μg · g^-1 was found, which is in consistency with the value determined by spectrophotometry. Value of RSD (n=5) found by analyzing the same sample was 1. 8%. Values of recovery over 90% were obtained in the recovery tests at 2 concentration levels of 60μg · g^-1 and 20 μg · g^-1 .

  6. Dynamic headspace generation and quantitation of triacetone triperoxide vapor.

    Science.gov (United States)

    Giordano, Braden C; Lubrano, Adam L; Field, Christopher R; Collins, Greg E

    2014-02-28

    Two methods for quantitation of triacetone triperoxide (TATP) vapor using a programmable temperature vaporization (PTV) inlet coupled to a gas chromatography/mass spectrometer (GC/MS) have been demonstrated. The dynamic headspace of bulk TATP was mixed with clean humid air to produce a TATP vapor stream. Sampling via a heated transfer line to a PTV inlet with a Tenax-TA™ filled liner allowed for direct injection of the vapor stream to a GC/MS for vapor quantitation. TATP was extracted from the vapor stream and subsequently desorbed from the PTV liner for splitless injection on the GC column. Calibration curves were prepared using solution standards with a standard split/splitless GC inlet for quantitation of the TATP vapor. Alternatively, vapor was sampled onto a Tenax-TA™ sample tube and placed into a thermal desorption system. In this instance, vapor was desorbed from the tube and subsequently trapped on a liquid nitrogen cooled PTV inlet. Calibration curves for this method were prepared from direct liquid injection of standards onto samples tube with the caveat that a vacuum is applied to the tube during deposition to ensure that the volatile TATP penetrates into the tube. Vapor concentration measurements, as determined by either GC/MS analysis or mass gravimetry of the bulk TATP, were statistically indistinguishable. Different approaches to broaden the TATP vapor dynamic range, including diluent air flow, sample chamber temperature, sample vial orifice size, and sample size are discussed. Vapor concentrations between 50 and 5400ngL(-1) are reported, with stable vapor generation observed for as long as 60 consecutive hours.

  7. AMMONIA CONCENTRATION IN SALTSTONE HEADSPACE SUMMARY REPORT

    Energy Technology Data Exchange (ETDEWEB)

    Zamecnik, J; Alex Cozzi, A

    2008-09-26

    The Saltstone Facility Documented Safety Analysis (DSA) is under revision to accommodate changes in the Composite Lower Flammability Limit (CLFL) from the introduction of Isopar into Tank 50. Saltstone samples were prepared with an 'MCU' type salt solution spiked with ammonia. The ammonia released from the saltstone was captured and analyzed. The ammonia concentration found in the headspace of samples maintained at 95 C and 1 atm was, to 95% confidence, less than or equal to 3.9 mg/L. Tank 50 is fed by several influent streams. The salt solution from Tank 50 is pumped to the salt feed tank (SFT) in the Saltstone Production Facility (SPF). The premix materials cement, slag and fly ash are blended together prior to transfer to the grout mixer. The premix is fed to the grout mixer in the SPF and the salt solution is incorporated into the premix in the grout mixer, yielding saltstone slurry. The saltstone slurry drops into a hopper and then is pumped to the vault. The Saltstone Facility Documented Safety Analysis (DSA) is under revision to accommodate changes in the Composite Lower Flammability Limit (CLFL) from the introduction of Isopar{reg_sign} L into Tank 50. Waste Solidification-Engineering requested that the Savannah River National Laboratory (SRNL) perform testing to characterize the release of ammonia in curing saltstone at 95 C. The test temperature represents the maximum allowable temperature in the Saltstone Disposal Facility (SDF). Ammonia may be present in the salt solution and premix materials, or may be produced by chemical reactions when the premix and salt solution are combined. A final report (SRNS-STI-2008-00120, Rev. 0) will be issued that will cover in more depth the information presented in this report.

  8. Determination of 2-methylisoborneol and geosmin in drinking water using headspace solid phase micro-extraction coupled with gas chromatography-mass spectrometry%顶空固相微萃取-气相色谱-质谱联用测定饮用水中的2-甲基异莰醇和土臭素

    Institute of Scientific and Technical Information of China (English)

    成建国; 刘开颖; 白敏冬; 程超; 余忆玄; 周新颖

    2015-01-01

    2-甲基异莰醇(2-methylisoborneol,2-MIB)和土臭素(geosmin,GSM)在水源水中大量分泌排放是造成饮用水土霉异味突发事件、引发居民用水恐慌的重用因素之一。使用顶空固相微萃取( HS-SPME)与气相色谱-质谱联用技术( GC-MS)建立了水库水、水库附近土壤、居民自来水中2-MIB 和 GSM 的测定方法。结合正交分析优化了加盐量、萃取温度、萃取时间条件,在电子轰击( EI)-选择离子扫描( SIM)模式下进行了目标物的定性定量分析。结果表明:在5~1000 ng/L 范围内,2-MIB 和 GSM 的色谱峰面积与其质量浓度的线性关系良好( r2≥0.998),2-MIB与 GSM的检出限分别为0.72 ng/L和0.34 ng/L,定量限分别为2.40 ng/L 和1.13 ng/L;目标物加标水平为10~600 ng/L时,平均回收率为93.6%~107.7%,相对标准偏差( RSD)≤6.1%( n=6)。基于上述方法,对辽宁省某地区水库水、水库附近土壤、居民自来水中的目标物进行检测,结果表明:水库水目标物质量浓度范围为3.0~3.6 ng/L,水库附近土壤中提取的2-MIB为8.1 ng/L、提取的GSM为17.8 ng/L,居民自来水中的目标物未检出。该方法操作简便、准确可靠,灵敏度高,无需有机溶剂,适合于饮用水中2-MIB和 GSM的分析检测。%The odorous compounds of 2-methylisoborneol(2-MIB)and geosmin(GSM)heavi-ly produced and released in water source are one of the most important factors leading to off-flavor emergencies and resident water consumption panic in drinking water. A headspace solid phase micro-extraction ( HS-SPME ) combined with gas chromatography-mass spectrometry ( GC-MS)method was established for the simultaneous determination of these two trace earthy and musty compounds in reservoir water,reservoir soil and tap water. The conditions of HS-SPME,such as salt amount,extraction time and extraction temperature,were optimized based on

  9. [Analysis of headspace constituents of Gardenia flower by GC/MS with solid-phase microextraction and dynamic headspace sampling].

    Science.gov (United States)

    Liu, B Z; Gao, Y

    2000-09-01

    The headspace constituents of fresh Gardenia flower were investigated by GC/MS. The headspace volatiles were sampled by solid-phase microextraction (SPME) and dynamic headspace sampling (DHS). SPME sampling was conducted with 100 microns PDMS fiber at 28 degrees C for 60 min. In DHS sampling, purified nitrogen was used as purging gas with a flow rate at 80 mL/min for 120 min. Tenax GR(20 mesh-40 mesh) was used as adsorbent and the volatiles were eluted by ether, and concentrated to 0.5 mL for GC/MS analysis. A Supelco-wax capillary column (30 m x 0.25 mm i.d. x 0.25 micron df) was employed in GC/MS analysis. Initial oven temperature was kept at 45 degrees C for 2 min, then raised to 250 degrees C at 4 degrees C/min, and kept at 250 degrees C for 10 min. According to SPME-GC/MS analysis, the main compounds in headspace of fresh Gardenia flower included farnesene(64.86%), cis-ocimene(29.33%), linalool(2.74%), cis-3-hexenyl tiglate(1.34%), methyl benzoate(0.25%). Results obtained from SPME and DHS sampling were also compared. In this study, SPME afforded a simpler and more sensitive sampling method, and much more accurate information about headspace volatiles of Gardenia flower.

  10. Performance Demonstration Program Plan for Analysis of Simulated Headspace Gases

    Energy Technology Data Exchange (ETDEWEB)

    Carlsbad Field Office

    2007-11-13

    The Performance Demonstration Program (PDP) for headspace gases distributes blind audit samples in a gas matrix for analysis of volatile organic compounds (VOCs). Participating measurement facilities (i.e., fixed laboratories, mobile analysis systems, and on-line analytical systems) are located across the United States. Each sample distribution is termed a PDP cycle. These evaluation cycles provide an objective measure of the reliability of measurements performed for transuranic (TRU) waste characterization. The primary documents governing the conduct of the PDP are the Quality Assurance Program Document (QAPD) (DOE/CBFO-94-1012) and the Waste Isolation Pilot Plant (WIPP) Waste Analysis Plan (WAP) contained in the Hazardous Waste Facility Permit (NM4890139088-TSDF) issued by the New Mexico Environment Department (NMED). The WAP requires participation in the PDP; the PDP must comply with the QAPD and the WAP. This plan implements the general requirements of the QAPD and the applicable requirements of the WAP for the Headspace Gas (HSG) PDP. Participating measurement facilities analyze blind audit samples of simulated TRU waste package headspace gases according to the criteria set by this PDP Plan. Blind audit samples (hereafter referred to as PDP samples) are used as an independent means to assess each measurement facility’s compliance with the WAP quality assurance objectives (QAOs). To the extent possible, the concentrations of VOC analytes in the PDP samples encompass the range of concentrations anticipated in actual TRU waste package headspace gas samples. Analyses of headspace gases are required by the WIPP to demonstrate compliance with regulatory requirements. These analyses must be performed by measurement facilities that have demonstrated acceptable performance in this PDP. These analyses are referred to as WIPP analyses and the TRU waste package headspace gas samples on which they are performed are referred to as WIPP samples in this document

  11. Performance Demonstration Program Plan for Analysis of Simulated Headspace Gases

    Energy Technology Data Exchange (ETDEWEB)

    Carlsbad Field Office

    2007-11-19

    The Performance Demonstration Program (PDP) for headspace gases distributes blind audit samples in a gas matrix for analysis of volatile organic compounds (VOCs). Participating measurement facilities (i.e., fixed laboratories, mobile analysis systems, and on-line analytical systems) are located across the United States. Each sample distribution is termed a PDP cycle. These evaluation cycles provide an objective measure of the reliability of measurements performed for transuranic (TRU) waste characterization. The primary documents governing the conduct of the PDP are the Quality Assurance Program Document (QAPD) (DOE/CBFO-94-1012) and the Waste Isolation Pilot Plant (WIPP) Waste Analysis Plan (WAP) contained in the Hazardous Waste Facility Permit (NM4890139088-TSDF) issued by the New Mexico Environment Department (NMED). The WAP requires participation in the PDP; the PDP must comply with the QAPD and the WAP. This plan implements the general requirements of the QAPD and the applicable requirements of the WAP for the Headspace Gas (HSG) PDP. Participating measurement facilities analyze blind audit samples of simulated TRU waste package headspace gases according to the criteria set by this PDP Plan. Blind audit samples (hereafter referred to as PDP samples) are used as an independent means to assess each measurement facility’s compliance with the WAP quality assurance objectives (QAOs). To the extent possible, the concentrations of VOC analytes in the PDP samples encompass the range of concentrations anticipated in actual TRU waste package headspace gas samples. Analyses of headspace gases are required by the WIPP to demonstrate compliance with regulatory requirements. These analyses must be performed by measurement facilities that have demonstrated acceptable performance in this PDP. These analyses are referred to as WIPP analyses and the TRU waste package headspace gas samples on which they are performed are referred to as WIPP samples in this document

  12. Field Performance of Dieldrin/Resin Wettable Powders on Sorptive Mud Surface

    Science.gov (United States)

    Van Tiel, N.

    1961-01-01

    Recent field experiments on the relative performance of dieldrin and dieldrin/resin wettable powders on sorptive mud surface have not confirmed the promising results obtained with the latter products in earlier laboratory tests. In view of this a renewed investigation into the possible factors governing the performance of such products was considered desirable, and further laboratory and field experiments were carried out in co-operation with the Colonial Pesticides Research Unit at Arusha, Tanganyika. The results of these experiments have given a better understanding of the factors involved, and a coherent interpretation of the differences in performance shown by various products under different conditions. The main factors to be taken into account appear to be: mobility of the insects during exposure, as influenced by insect species and exposure conditions; inherent toxicity of the dieldrin/resin particles; and the average relative humidity inside the experimental huts. The sorption phenomenon can be demonstrated in the field, but in view of the humidity conditions it does not seem likely that it will interfere seriously with practical mosquito control. A potential critical condition might be prevalent only in areas where the presence of sorptive mud is coupled with long periods of low humidity inside the huts, but further experimental data are necessary to confirm this. PMID:13780061

  13. Sample Preparation for Headspace GC Analysis of Residual Solvents in Hyaluronic Acid Derivative Fiber

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hoon Joo; Kim, Dong Min; Yang, Jeong Soo [LG life Sciences, Ltd./R and D Park, Daejeon (Korea, Republic of); Kim, Chan Wha [Korea University, Seoul (Korea, Republic of)

    2006-02-15

    The aim of this study is to develop efficient sample preparation method for HS-GC analysis of residual solvents in HA derivative fiber. Compared to direct extraction of residual solvents from HA derivative fiber, the extraction through the hydrolysis of HA derivative fiber by HAse gave more complete and higher reproducible quantification of residual solvent. To validate HS-GC analysis method of residual solvents, specificity, limits of detection and quantification, linearity, accuracy and precision are investigated in the study. HA derivative fiber was hydrolyzed using HAse for headspace gas chromatographic analysis of residual solvents of ethanol, acetone and isopropanol in HA derivative fiber. This study showed that the developed method had specificity, linearity, accuracy and precision. In addition, it demonstrated that HS-GC coupled with matrix-breaking method such as hydrolysis was available for the determination of residual solvents in a matrix like HA derivative fiber.

  14. Microwave distillation followed by headspace single drop microextraction coupled to gas chromatography-mass spectrometry (GC-MS) for fast analysis of volatile components of Echinophora platyloba DC.

    Science.gov (United States)

    Gholivand, Mohammad Bagher; Abolghasemi, Mir Mahdi; Piryaei, Marzieh; Maassoumi, Sayed Mohammad; Papzan, Abdolhamid

    2013-05-01

    To avoid the traditional and time consuming hydrodistillation, the analyses of volatile components in aerial parts of Echinophora platyloba DC was carried out by a simple microwave distillation followed by headspace single drop microextraction (MD-HS-SDME) coupled to gas chromatography-mass spectrometry (GC-MS). The headspace volatile compounds were collected after irradiation using a single drop of n-heptadecan. The extraction conditions were optimised using the relative peak areas as index. The chemical composition of the MD-HS-SDME extracts was confirmed according to their retention indexes and mass spectra. Fifty-three components were extracted and identified by using the MD-HS-SDME method. E-β-ocimene (53.81%), R-D-decalactone (12.75%), α-pinene (6.43%), n-heptanol (6.27%), β-phellanderne (2.70%) and linalool (1.89%) were the major constituents. Copyright © 2012 Elsevier Ltd. All rights reserved.

  15. Quality control of raw cows' milk by headspace analysis

    NARCIS (Netherlands)

    Hettinga, K.A.; Valenberg, van H.J.F.; Hooijdonk, van A.C.M.

    2008-01-01

    This study investigated whether headspace analysis of volatile components can be used for monitoring the quality of raw cows¿ milk. The detection of different quality defects caused by cows¿ feed, microbiological and chemical contamination, as well as enzymatic deterioration was studied. Fresh raw m

  16. Purge-assisted headspace solid-phase microextraction combined with gas chromatography-mass spectrometry for determination of chlorophenols in aqueous samples.

    Science.gov (United States)

    Ho, Hsin-Pin; Lee, Ren-Jye; Lee, Maw-Rong

    2008-12-12

    A simple, economical and very effective method is demonstrated for simultaneous determination of 2,4-dichlorophenol, 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol and pentachlorophenol, in aqueous samples, by using purge-assisted headspace solid-phase microextraction (PA/HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). In the new method, purging the sample enhances the removal of the trace chlorophenols without derivatization from the matrices to the headspace. Extraction parameters including extraction temperature, purge gas flow rate and extraction time were systematically investigated. Under optimal conditions, the relative standard deviations (RSDs) were 4-11% at 50 pg/mL and 5-14% at 5 pg/mL, respectively. The recoveries were in the range of 83-114%. Detection limits were determined at the fg level. These results indicate that PA/HS-SPME provides a significant contribution to highly efficient extraction of semi-volatile CPs, especially for pentachlorophenol, which has the smallest Henry's constant and large octanol-water partitioning coefficient. In addition, the proposed method was successfully applied to the analysis of chlorophenols in landfill leachate. New perspectives are opened for headspace extraction of relatively low vapor pressure compounds in complex matrices.

  17. 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.

  18. Study about the capillary absorption and the sorptivity of concretes with Cuban limestone aggregates

    Directory of Open Access Journals (Sweden)

    Howland, J. J.

    2013-12-01

    Full Text Available The objective of this study was to demonstrate the possibility to obtain concretes in Cuba with values of effective porosity below of 10%, using limestone aggregates with high levels of absorption (higher than 1% in many cases, and values of Sorptivity below of 5 x 10-5 m/s1/2 as is established in the document prepared by the DURAR Latin Working Group, for structures exposed to very aggressive environments. The experimental results showed that the use of the trial method of capillary absorption of Göran Fagerlund, were obtained concretes with effective porosity below of the 10%, for water/cement ratios of 0.4 and 0.45, but the values of sorptivities were very high. Nevertheless the subsequent use of the trial method of the ASTM C1585, that use cylinders probes with bigger depth and different processing, permits to obtain the desired sorptivity values for water/cement ratios of 0.4 and 0.45 whenever would be fulfilled the Good Practices of the Construction.El objetivo del estudio fue demostrar la posibilidad de lograr en Cuba, con el empleo de áridos calizos de elevada absorción (mayores del 1% en muchos casos, hormigones con valores de porosidad efectiva inferiores al 10% y de velocidad de absorción capilar (Sorptividad inferiores a 5 x 10-5 m/s1/2, tal como establece el documento elaborado por la RED DURAR del CYTED para estructuras expuestas a ambientes muy agresivos. Los resultados experimentales mostraron que con la aplicación del método de ensayo de absorción capilar de Göran Fagerlund se obtuvieron porosidades efectivas inferiores al 10% para relaciones agua/cemento de 0,4 y 0,45, pero los valores de sorptividad fueron muy elevados. No obstante la aplicación posterior del método de ensayo de la ASTM C1585 que utiliza probetas de mayor espesor y diferente tratamiento, permitió obtener los valores indicados de sorptividad para relaciones agua/cemento de 0,4; 0,45 siempre que se cumplan las Buenas Prácticas constructivas.

  19. EXTRACT

    DEFF Research Database (Denmark)

    Pafilis, Evangelos; Buttigieg, Pier Luigi; Ferrell, Barbra

    2016-01-01

    The microbial and molecular ecology research communities have made substantial progress on developing standards for annotating samples with environment metadata. However, sample manual annotation is a highly labor intensive process and requires familiarity with the terminologies used. We have the...... and text-mining-assisted curation revealed that EXTRACT speeds up annotation by 15-25% and helps curators to detect terms that would otherwise have been missed.Database URL: https://extract.hcmr.gr/....

  20. Evaluation of sorptive flotation technique for enhanced removal of radioactive Eu(III) from aqueous solutions

    Energy Technology Data Exchange (ETDEWEB)

    Ezzat, Amir; Saad, Ebtissam A. [Ain Shams Univ., Cairo (Egypt). Chemistry Dept.; Mahmoud, Mamdoh R. [Atomic Energy Authority, Cairo (Egypt). Nuclear Chemistry Dept.; Soliman, Mohamed A. [Atomic Energy Authority, Cairo (Egypt). Egypt Second Research Reactor; Kandil, Abdelhakim [Helwan Univ., Cairo (Egypt). Chemistry Dept.

    2017-06-01

    The present study aims at the removal of Eu(III) from aqueous solutions by sorptive flotation process. This process involves adsorption of Eu(III) onto bentonite and kaolinite clays followed by floatation using sodium dodecyl sulfate (SDS) and cetyltrimethylammonium bromide (CTAB) collectors. The effect of adsorption parameters (pH, contact time, clay weight, Eu(III) concentration, ionic strength) as well as flotation parameters (collector and frother concentrations, bubbling time, concentrations of foreign cations and anions) on the removal efficiency of Eu(III) were studied. The obtained results show that Eu(III) ions are removed efficiently (R% ∝ 95%) at pH=4 after 1 h shaking with clay and 15 min floatation. The adsorption kinetics of Eu(III) onto the employed clays followed the pseudo-second-order model and the equilibrium data fitted well to the Freundlich isotherm model.

  1. Role of biofilms in sorptive removal of steroidal hormones and 4-nonylphenol compounds from streams

    Science.gov (United States)

    Writer, Jeffrey H.; Ryan, Joseph N.; Barber, Larry B.

    2011-01-01

    Stream biofilms play an important role in geochemical processing of organic matter and nutrients, however, the significance of this matrix in sorbing trace organic contaminants is less understood. This study focused on the role of stream biofilms in sorbing steroidal hormones and 4-nonylphenol compounds from surface waters using biofilms colonized in situ on artificial substrata and subsequently transferred to the laboratory for controlled batch sorption experiments. Steroidal hormones and 4-nonylphenol compounds readily sorb to stream biofilms as indicated by organic matter partition coefficients (Kom, L kg-1) for 17β-estradiol (102.5-2.8 L kg-1), 17α-ethynylestradiol (102.5-2.9 L kg-1), 4-nonylphenol (103.4-4.6 L kg-1), 4-nonylphenolmonoethoxylate (103.5-4.0 L kg-1), and 4-nonylphenoldiethoxylate (103.9-4.3 L kg-1). Experiments using water quality differences to induce changes in the relative composition of periphyton and heterotrophic bacteria in the stream biofilm did not significantly affect the sorptive properties of the stream biofilm, providing additional evidence that stream biofilms will sorb trace organic compounds under of variety of environmental conditions. Because sorption of the target compounds to stream biofilms was linearly correlated with organic matter content, hydrophobic partition into organic matter appears to be the dominant mechanism. An analysis of 17β-estradiol and 4-nonylphenol hydrophobic partition into water, biofilm, sediment, and dissolved organic matter matrices at mass/volume ratios typical of smaller rivers showed that the relative importance of the stream biofilm as a sorptive matrix was comparable to bed sediments. Therefore, stream biofilms play a primary role in attenuating these compounds in surface waters. Because the stream biofilm represents the base of the stream ecosystem, accumulation of steroidal hormones and 4-nonylphenol compounds in the stream biofilm may be an exposure pathway for organisms in higher trophic

  2. Headspace screening: A novel approach for fast quality assessment of the essential oil from culinary sage.

    Science.gov (United States)

    Cvetkovikj, Ivana; Stefkov, Gjoshe; Acevska, Jelena; Karapandzova, Marija; Dimitrovska, Aneta; Kulevanova, Svetlana

    2016-07-01

    Quality assessment of essential oil (EO) from culinary sage (Salvia officinalis L., Lamiaceae) is limited by the long pharmacopoeial procedure. The aim of this study was to employ headspace (HS) sampling in the quality assessment of sage EO. Different populations (30) of culinary sage were assessed using GC/FID/MS analysis of the hydrodistilled EO (pharmacopoeial method) and HS sampling directly from leaves. Compound profiles from both procedures were evaluated according to ISO 9909 and GDC standards for sage EO quality, revealing compliance for only 10 populations. Factors to convert HS values, for the target ISO and GDC components, into theoretical EO values were calculated. Statistical analysis revealed a significant relationship between HS and EO values for seven target components. Consequently, HS sampling could be used as a complementary extraction technique for rapid screening in quality assessment of sage EOs.

  3. Volatile release from aqueous solutions under dynamic headspace dilution conditions.

    Science.gov (United States)

    Marin, M; Baek, I; Taylor, A J

    1999-11-01

    Static equilibrium was established between the gas phase (headspace) and an unstirred aqueous phase in a sealed vessel. The headspace was then diluted with air to mimic the situation when a container of food is opened and the volatiles are diluted by the surrounding air. Because this first volatile signal can influence overall flavor perception, the parameters controlling volatile release under these conditions are of interest. A mechanistic model was developed and validated experimentally. Release of compounds depended on the air-water partition coefficient (K(aw)) and the mass transport in both phases. For compounds with K(aw) values 10(-)(3), mass transport in the gas phase became significant and the Reynolds number played a role. Because release from packaged foods occurs at low Reynolds numbers, whereas most experiments are conducted at medium to high Reynolds numbers, the experimentally defined profile may not reflect the real situation.

  4. Selective fiber used for headspace solid-phase microextraction of abused drugs in human urine

    Directory of Open Access Journals (Sweden)

    Sunanta Wangkarn

    2007-09-01

    Full Text Available A sensitive and selective fiber for simultaneous analysis of three drugs of abuse (amphetamine, methamphetamine and ephedrine in urine samples was explored using headspace solid phase microextraction and gas chromatography with flame ionization detection. Several parameters affecting extraction such as extraction time, extraction temperature, pH of solution and salt concentrations were investigated. Among five commercially available fibers, divinylbenzene/carboxen/ polydimethylsiloxane is the most sensitive and selective fiber at pH 10.0, extraction temperature at 80 C for 20 min and desorption temperature at 220 C for 2 min. Under the optimal conditions, the proposed solid phase microextraction method provided good linearity in the ranges 0.1-10 µg/ml for amphetamine and methamphetamine and 0.5-20 µg/ml for ephedrine. The detection limits for amphetamine, methamphetamine and ephedrine were 9, 3 and 30 ng/ml, respectively. The recoveries of three drugs in urine samples were exceeding 85%.

  5. Bioaccesibility Extraction of Hydrophobic Pollutants: Benefits of Separating Leaching Agent and Acceptor Medium

    DEFF Research Database (Denmark)

    Cocovi-Solberg, D. J.; Miro, M.; Loibner, A. P.

    2015-01-01

    can lead to underestimation of bioaccessibility. Therefore, several studies have proposed to add a sink to the extraction medium, including the so called contaminant trap, the silicon rod based sorptive bioaccessibility extraction and tenax beads-assisted extractions. While these methods certainly...... and highly performing format was further optimized and validated. This new configuration was characterized in terms of mass transfer kinetics, analytical performance criteria and suitability for direct analysis by high performance liquid chromatography (HPLC) and gas chromatography (GC). Finally...

  6. Design and testing of a new sampler for simplified vacuum-assisted headspace solid-phase microextraction.

    Science.gov (United States)

    Yiantzi, Evangelia; Kalogerakis, Nicolas; Psillakis, Elefteria

    2016-07-13

    The design and testing of a new and low-cost experimental setup used for vacuum-assisted headspace solid-phase microextraction (Vac-HSSPME) is reported here. The device consists of a specially designed O-ring seal screw cap offering gas-tight seal to commercially available headspace vials. The new polytetrafluoroethylene (PTFE) cap was molded by a local manufacturer and had a hole that could tightly accommodate a septum. All operations were performed through the septum: air evacuation of the sampler, sample introduction and HSSPME sampling. The analytical performance of the new sampler was evaluated using 22 mL headspace vials with 9 mL water samples spiked with polychlorinated biphenyls (PCBs). Several experimental parameters were controlled and the optimized conditions were: 1000 rpm agitation speed; 30 min extraction time; 40 °C sampling temperature; polydimethylsiloxane-divinylbenzene (PDMS-DVB) fiber. The lack of accurate Henry's law constant (KH) values and information regarding how they change with temperature was a major limitation in predicting the phase location of evaporation resistance during Vac-HSSPME. Nevertheless, the combined effects of system conditions indicated the increasing importance of gas phase resistance with increasing degree of PCBs chlorination. Stirring enhancements were not recorded for the higher chlorinated PCBs suggesting that the hyperhydrophobic gas/water interface was the preferred location for these compounds. Analytically, the developed method was found to yield linear calibration curves with limits of detection in the sub ng L(-1) level and relative standard deviations ranging between 5.8 and 14%. To compensate for the low recoveries of the higher chlorinated PCB congeners in spiked river water the standard addition methodology was applied. Overall, the compact design of the new and reusable sample container allows efficient HSSPME sampling of organic analytes in water within short extraction times and at low sampling

  7. Direct synthesis of nitrogen-doped graphene on platinum wire as a new fiber coating method for the solid-phase microextraction of BXes in water samples: Comparison of headspace and cold-fiber headspace modes.

    Science.gov (United States)

    Memarian, Elham; Hosseiny Davarani, Saied Saeed; Nojavan, Saeed; Movahed, Siyavash Kazemi

    2016-09-01

    In this work, a new solid-phase microextraction fiber was prepared based on nitrogen-doped graphene (N-doped G). Moreover, a new strategy was proposed to solve problems dealt in direct coating of N-doped G. For this purpose, first, Graphene oxide (GO) was coated on Pt wire by electrophoretic deposition method. Then, chemical reduction of coated GO to N-doped G was accomplished by hydrazine and NH3. The prepared fiber showed good mechanical and thermal stabilities. The obtained fiber was used in two different modes (conventional headspace solid-phase microextraction and cold-fiber headspace solid-phase microextraction (CF-HS-SPME)). Both modes were optimized and applied for the extraction of benzene and xylenes from different aqueous samples. All effective parameters including extraction time, salt content, stirring rate, and desorption time were optimized. The optimized CF-HS-SPME combined with GC-FID showed good limit of detections (LODs) (0.3-2.3 μg/L), limit of quantifications (LOQs) (1.0-7.0 μg/L) and linear ranges (1.0-5000 μg/L). The developed method was applied for the analysis of benzene and xylenes in rainwater and some wastewater samples.

  8. Multiple headspace-solid-phase microextraction: An application to quantification of mushroom volatiles

    Energy Technology Data Exchange (ETDEWEB)

    Costa, Rosaria; Tedone, Laura; De Grazia, Selenia [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Dugo, Paola [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy); Mondello, Luigi, E-mail: lmondello@unime.it [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy)

    2013-04-03

    Highlights: ► Multiple headspace extraction-solid phase microextraction (MHS-SPME) has been applied to the analysis of Agaricus bisporus. ► Mushroom flavor is characterized by the presence of compounds with a 8-carbon atoms skeleton. ► Formation of 8-carbon compounds involves a unique fungal biochemical pathway. ► The MHS-SPME allowed to determine quantitatively 5 target analytes of A. bisporus for the first time. -- Abstract: Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC–MS) and flame ionization detection (GC–FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033–0.078 ng), limit of quantification (LoQ, range 0.111–0.259 ng) and analyte recovery (92.3–108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented.

  9. Headspace in-tube microextraction coupled with micellar electrokinetic chromatography of neutral aromatic compounds.

    Science.gov (United States)

    Cho, Sung Min; Park, Bum Su; Jung, Woo Sung; Lee, Sang Won; Jung, Yunhwan; Chung, Doo Soo

    2016-02-01

    Headspace (HS) extraction can be carried out easily and aptly via single drop microextraction coupled with capillary electrophoresis (CE). However, one drawback is the difficulty of keeping the single drop stably at the capillary tip. To solve this problem, we have recently demonstrated HS in-tube microextraction (ITME) of acidic compounds such as chlrophenols in an acidic sample using a basic run buffer plug in the separation capillary for CE as an acceptor phase. In this report, an organic acceptor plug in a capillary was used to extract neutral organic volatile pollutants such as BTEX (benzene, toluene, ethylbenzene, and m-xylene). After extraction, the analytes enriched in the organic acceptor plug were analyzed with micellar electrokinetic chromatography (MEKC). The enrichment factors for BTEX in a standard solution were up to 350 under an optimal condition of 25°C for 20 min. As an application, BTEX spiked into bottled water were analyzed with HS-ITME-MEKC, and the enrichment factors for BTEX were up to 320. The limits of detections were 1-4 ppb, which are at least 200 times lower than the US Environmental Protection Agency guidelines for drinking water, except benzene. The entire procedure of HS-ITME-MEKC was carried out automatically using a commercial CE instrument.

  10. Sorptivity of rocks and soils of the van Genuchten-Mualem type

    Energy Technology Data Exchange (ETDEWEB)

    Zimmerman, R.W.; Bodvarsson, G.S. [Lawrence Berkeley Lab., CA (United States)

    1991-06-01

    One hydrological process that will have great relevance to the performance of the proposed underground radioactive waste repository at Yucca Mountain, Nevada, is that of the absorption of water from a water-filled fracture into the adjacent unsaturated rock formation. The rate at which water is imbibed by a rock depends on the hydrological properties of the rock and on the initial saturation (or initial capillary suction) of the formation. The hydrological properties that affect imbibition are the relative permeability function and the capillary pressure function. These functions are often collectively referred to as the `characteristic functions` of the porous medium. For one-dimensional absorption, it can be shown that, regardless of the details of the characteristic functions, the total amount of water imbibed by the formation, per unit surface area, will be proportional to the square root of the elapsed time. Hence the ability of a rock or soil to imbibe water can be quantified by a parameter known as the sorptivity S, which is defined such that the cumulative volumetric liquid influx per unit area is given by Q = S{radical}t. The paper discusses the simplification of these characteristic functions of porous medium.

  11. EFFECT OF LDPE RAW MATERIAL ON STRENGTH, CORROSION AND SORPTIVITY OF CONCRETE

    Directory of Open Access Journals (Sweden)

    R. MANIKANDRAN

    2015-04-01

    Full Text Available Many researchers focused on effect of Low Density Poly Ethylene (LDPE on bituminous pavements or concrete to modify the strength and ductility in view of reusing the abundant quantity of non-degradable LDPE material available. It also reduces the use of bituminous materials and disposal problems of such waste material. Developing countries are moving towards construction concrete pavement or converting bituminous pavements into concrete pavements. Hence in this paper an attempt has been made to study the feasibility of using LDPE raw material itself as a modifier in cement concrete with a characteristic compressive strength of 20 MPa. Present study focuses on effect of addition of LDPE raw material (3, 4 and 5% under different temperatures (70°C, 80°C and 90°C and duration of thermal curing (4, 8 and 16 hours on compressive strength, corrosion resistance and sorptivity. It was inferred from the results that, addition of LDPE raw material considerably increases the compressive strength, resistance against corrosion and permeability. Results also revealed that concrete with 3% LDPE modifier for 80°C with 4 hours of thermal curing was found to be optimum.

  12. Identification of characteristic flavor compounds in cocoa powder by gas chromatography-olfactometry-mass spectrometry with headspace solid phase micro-extraction%顶空固相微萃取结合GC-O与GC-MS技术鉴定可可粉中特征风味化合物

    Institute of Scientific and Technical Information of China (English)

    肖天鹏; 郑晓峰; 吕吉鸿; 郭泽峰; 高峰; 刘春凤; 李崎

    2012-01-01

    A method for headspace solid-phase microextraction(HS-SPME),followed by gas chromatography-olfactometry-mass spectrometry analysis was established for the identification of the characteristic flavor compounds in cocoa powder.According to the results,39 compounds which gave contribution to the flavor of cocoa powder were detected,including 7 aldehydes,3 alcohols,3 ketones,8 esters,2 acids,4 pyrazines,2 amines and any other special volatile substances.Among the flavor compounds,three compounds had key odorant(nutty,cocoa flavor),they were 2,5-dimethyl pyrazine,2,3,5-trimethyl pyrazine and 2,3,5,6-tetramethyl pyrazine.%利用顶空固相微萃取(HS-SPME)结合GC-O与GC-MS技术鉴定可可粉中的特征致香成分,鉴定出有39种化合物参与构成可可风味,分别是:7种醛、3种醇、3种酮、8种酯、2种酸、4种吡嗪、2种胺以及其他一些特殊的挥发性物质。其中具有典型可可风味(坚果,可可香)的关键化合物有3种,分别为2,5-二甲基吡嗪、2,3,5-三甲基吡嗪以及2,3,5,6-四甲基吡嗪。

  13. Characterization of volatile compounds of Daucus crinitus Desf. Headspace Solid Phase Microextraction as alternative technique to Hydrodistillation

    Directory of Open Access Journals (Sweden)

    Tabti Boufeldja

    2010-09-01

    Full Text Available Abstract Background Traditionally, the essential oil of aromatic herbs is obtained using hydrodistillation (HD. Because the emitted volatile fraction plays a fundamental role in a plant's life, various novel techniques have been developed for its extraction from plants. Among these, headspace solid phase microextraction (HS-SPME can be used to obtain a rapid fingerprint of a plant's headspace. Daucus crinitus Desf. is a wild plant that grows along the west coast of Algeria. Only a single study has dealt with the chemical composition of the aerial part oils of Algerian D. crinitus, in which isochavicol isobutyrate (39.0%, octyl acetate (12.3%, and β-caryophyllene (5.4% were identified. Using GC-RI and GC-MS analysis, the essential oils and the volatiles extracted from separated organs of D. crinitus Desf. were studied using HS-SPME. Results GC-RI and GC-MS analysis identified 72 and 79 components in oils extracted using HD and in the volatile fractions extracted using SPME, respectively. Two types of essential oils were produced by the plant: the root oils had aliphatic compounds as the main component (87.0%-90.1%, and the aerial part oils had phenylpropanoids as the main component (43.1%-88.6%. HS-SPME analysis showed a more precise distribution of compounds in the organs studied: oxygenated aliphatic compounds were well represented in the roots (44.3%-84.0%, hydrocarbon aliphatic compounds were in the leaves and stems (22.2%-87.9%, and phenylpropanoids were in the flowers and umbels (47.9%-64.2%. Moreover, HS-SPME allowed the occurrence of isochavicol (29.6 - 34.7% as main component in D. crinitus leaves, but it was not detected in the oils, probably because of its solubility in water. Conclusions This study demonstrates that HD and HS-SPME modes could be complimentary extraction techniques in order to obtain the complete characterization of plant volatiles.

  14. Dynamic headspace analysis of volatile metabolites from the reductive dehalogenation of trichloro- and tetrachloroethanes by hepatic microsomes.

    Science.gov (United States)

    Thompson, J A; Ho, B; Mastovich, S L

    1985-03-01

    A dynamic headspace technique was developed to facilitate the identification and quantitation of low levels of volatile metabolites produced in vitro by subcellular preparations. The method is complementary to commonly used static headspace and solvent-extraction techniques, and involves purging the compounds from microsomal suspensions with an inert gas, trapping them on a short column of adsorbant resin, and transferring the metabolites to a gas chromatograph. An apparatus was designed to facilitate the incubations and isolations of volatile compounds. Recoveries of several chlorinated hydrocarbons with boiling points in the range 12 to 186 degrees C were 85% or higher, and the recovery of vinyl chloride (boiling point -13 degrees C) was 25%. The quantitative precision of the method was determined and calibration curves were established for each metabolite, demonstrating that no discrimination occurred over a wide range of concentrations. This technique was employed to investigate the reductive metabolism of 1,1,1-trichloroethane, 1,1,2-trichloroethane, and 1,1,2,2-tetrachloroethane by rat liver microsomes. The metabolites from these substrates were 1,1-dichloroethane, vinyl chloride, and 1,2-dichloroethylene, respectively. These conversions were NADPH-dependent, occurred only under anaerobic conditions, and indicate that chloroethanes with relatively low electron affinities can be reduced slowly by microsomal cytochrome P-450. The rates of formation of vinyl chloride, 1,1-dichloroethane, and 1,2-dichloroethylene with 1.0 mM substrate were 12.5 +/- 2.0, 122 +/- 14, and 147 +/- 12 pmol/min/mg of protein, respectively. The results show that there are distinct advantages of the purge/trap method over the static headspace method for studying volatile metabolites when high sensitivity is required.

  15. Effects of headspace fraction and aqueous alkalinity on subcritical hydrothermal gasification of cellulose

    Energy Technology Data Exchange (ETDEWEB)

    Dolan, Ryan; Yin, Sudong; Tan, Zhongchao [Department of Mechanical and Manufacturing Engineering, Centre for Environmental Engineering Research and Education, Schulich School of Engineering, University of Calgary, 2500 University Dr. N.W. Calgary, AB (Canada)

    2010-07-15

    In order to better understand the pathways of hydrothermal gasification of cellulose, the effect of headspace fraction and alkalinity on the hydrothermal gasification of cellulose has been studied at 315 C in the presence of Pt/Al{sub 2}O{sub 3} as catalyst. It was found that regardless of alkalinity the headspace fraction had a large impact on gasification yield, with larger headspace fractions resulting in considerably more gas product. Without the addition of sodium carbonate, the effect of headspace fraction became more pronounced, with gas increasing by approximately a factor of forty from the lowest to highest headspace fraction. On the other hand, for the same residence time the addition of sodium carbonate co-catalyst dampened the magnitude of the effect, to a factor of 2.5 and 1.5, for 50 and 100 mM sodium carbonate solutions, respectively. These results indicated that the headspace fraction affected the phase behaviour, and that this altered the pathway of the cellulose decomposition. While furfural alcohol was the major product obtained with a 49% headspace fraction, it was effectively suppressed by using 78% or greater headspace fractions. Based on the effects of phase behaviour and previous literature, the reduced effect occurring upon the addition of sodium carbonate may relate to catalysis of the Lobry de-bruyn Van Eckenstein transform to produce lactic acid rather than intermediates proceeding through glycolaldehyde. (author)

  16. Bepaling van tetrachloor- en trichloorethyleen in olijfolie met behulp van headspace - gaschromatografie

    NARCIS (Netherlands)

    Roos, A.H.; Mazijk, van R.J.; Tuinstra, L.G.M.Th.

    1990-01-01

    De resultaten van de EEG headspace methode wijzen uit dat de herhaalbaarheid en nauwkeurigheid voldoende zijn om tetrachloor- en trichloorethyleen in olijfolie te bepalen tot een niveau van 0,01 mg/kg op produkt. De headspace techniek is door de eenvoudige procedure zeer geschikt voor routine analys

  17. DISSOLVED OXYGEN AND METHANE IN WATER BY A GC HEADSPACE EQUILIBRATION TECHNIQUE

    Science.gov (United States)

    An analytical procedure is described for the determination of dissolved oxygen and methane in groundwater samples. The method consists of generating a helium gas headspace in a water filled bottle, and analysis of the headspace by gas chromatography. Other permanent gases such as...

  18. Primary Polymer Aging Processes Identified from Weapon Headspace Chemicals

    Energy Technology Data Exchange (ETDEWEB)

    Chambers, D M; Bazan, J M; Ithaca, J G

    2002-03-25

    A current focus of our weapon headspace sampling work is the interpretation of the volatile chemical signatures that we are collecting. To help validate our interpretation we have been developing a laboratory-based material aging capability to simulate material decomposition chemistries identified. Key to establishing this capability has been the development of an automated approach to process, analyze, and quantify arrays of material combinations as a function of time and temperature. Our initial approach involves monitoring the formation and migration of volatile compounds produced when a material decomposes. This approach is advantageous in that it is nondestructive and provides a direct comparison with our weapon headspace surveillance initiative. Nevertheless, this approach requires us to identify volatile material residue and decomposition byproducts that are not typically monitored and reported in material aging studies. Similar to our weapon monitoring method, our principle laboratory-based method involves static headspace collection by solid phase microextraction (SPME) followed by gas chromatography/mass spectrometry (GC/MS). SPME is a sorbent collection technique that is ideally suited for preconcentration and delivery of trace gas-phase compounds for analysis by GC. When combined with MS, detection limits are routinely in the low- and sub-ppb ranges, even for semivolatile and polar compounds. To automate this process we incorporated a robotic sample processor configured for SPME collection. The completed system will thermally process, sample, and analyze a material sample. Quantification of the instrument response is another process that has been integrated into the system. The current system screens low-milligram quantities of material for the formation or outgas of small compounds as initial indicators of chemical decomposition. This emerging capability offers us a new approach to identify and non-intrusively monitor decomposition mechanisms that are

  19. Volatile constituents of Murraya koenigii fresh leaves using headspace solid phase microextraction--gas chromatography-mass spectrometry.

    Science.gov (United States)

    Sukkaew, Sayamol; Pripdeevech, Patcharee; Thongpoon, Chalermporn; Machan, Theeraphan; Wongchuphan, Rattana

    2014-12-01

    The volatile components of Murraya koenigii fresh leaves, collected from Surat Thani province, Thailand were studied by using headspace (HS) solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS). The four fibers employed to extract the volatiles were polydimethylsiloxane (PDMS), polydimethylsiloxane-divinylbenzene (PDMS-DVB), carboxane-polydimethylsiloxane (CAR-PDMS) and polydimethylsiloxane-divinylbenzene-carboxane (PDMS-DVB-CAR). The volatile constituents of M. koenigii fresh leaves were also extracted by hydrodistillation and analyzed by GC-MS. Fifty-one compounds were identified by these fibers. Five major compounds, γ-terpinene, β-caryophyllene, β-phellandrene, a-selinene and a-pinene, were detected in all fibers. The PDMS-DVB-CAR fiber was considered as the best for trapping key volatiles of M. koenigii fresh leaves.

  20. Determination of amphetamines in human urine by headspace solid-phase microextraction and gas chromatography.

    Science.gov (United States)

    Raikos, Nikolaos; Christopoulou, Klio; Theodoridis, Georgios; Tsoukali, Heleni; Psaroulis, Dimitrios

    2003-06-05

    Solid-phase microextraction (SPME) is under investigation for its usefulness in the determination of a widening variety of volatile and semivolatile analytes in biological fluids and materials. Semivolatiles are increasingly under study as analytical targets, and difficulties with small partition coefficients and long equilibration times have been identified. Amphetamines were selected as semivolatiles exhibiting these limitations and methods to optimize their determination were investigated. A 100- micro m polydimethylsiloxane (PDMS)-coated SPME fiber was used for the extraction of the amphetamines from human urine. Amphetamine determination was made using gas chromatography (GC) with flame-ionization detection (FID). Temperature, time and salt saturation were optimized to obtain consistent extraction. A simple procedure for the analysis of amphetamine (AMP) and methamphetamine (MA) in urine was developed and another for 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxy-N-methamphetamine (MDMA) and 3,4-methylenedioxy-N-ethylamphetamine (MDEA) using headspace solid-phase microextraction (HS-SPME) and GC-FID. Higher recoveries were obtained for amphetamine (19.5-47%) and methamphetamine (20-38.1%) than MDA (5.1-6.6%), MDMA (7-9.6%) and MDEA (5.4-9.6%).

  1. Application of microwave-assisted desorption/headspace solid-phase microextraction as pretreatment step in the gas chromatographic determination of 1-naphthylamine in silica gel adsorbent.

    Science.gov (United States)

    Yan, Cheing-Tong; Jen, Jen-Fon; Shih, Tung-Sheng

    2007-03-30

    Pretreatment of silica gel sample containing 1-naphthylamine by microwave-assisted desorption (MAD) coupled to in situ headspace solid phase microextraction (HS-SPME) has been investigated as a possible alternative to conventional methods prior to gas chromatographic (GC) analysis. The 1-naphthylamine desorbs from silica gel to headspace under microwave irradiation, and directly absorbs onto a SPME fiber located in a controlled-temperature headspace area. After being collected on the SPME fiber, and desorbed in the GC injection port, 1-naphthylamine is analyzed by GC-FID. Parameters that influence the extraction efficiency of the MAD/HS-SPME, such as the extraction media and its pH, the microwave irradiation power and irradiation time as well as desorption conditions of the GC injector, have been investigated. Experimental results indicate that the extraction of a 150mg silica gel sample by using 0.8ml of 1.0M NaOH solution and a PDMS/DVB fiber under high-powered irradiation (477W) for 5min maximizes the extraction efficiency. Desorption of 1-naphthylamine from the SPME fiber in GC injector is optimal at 250 degrees C held for 3min. The detection limit of method is 8.30ng. The detected quantity of 1-naphthylamine obtained by the proposed method is 33.3 times of that obtained by the conventional solvent extraction method for the silica gel sample containing 100ng of 1-naphthylamine. It provides a simple, fast, sensitive and organic-solvent-free pretreatment procedure prior to the analysis of 1-naphthylamine collected on a silica gel adsorbent.

  2. GAS ANALYSES FROM HEADSPACE OF PLUTONIUM-BEARING MATERIALS CONTAINERS

    Energy Technology Data Exchange (ETDEWEB)

    Almond, P.; Livingston, R.; Traver, L.; Arnold, M.; Bridges, N.; Kessinger, G.; Duffey, J.

    2010-02-01

    The Savannah River National Laboratory (SRNL) 3013 destructive examination program performs surveillances on 3013 containers originating from multiple sites across the DOE complex. The bases for the packaging, storage, and surveillance activities are derived from the Department of Energy's 3013 Standard (DOE-STD-3013-2004). During destructive examination, headspace gas samples are obtained from the 3013 inner container and the annulus between the outer and inner containers. To characterize gas species, the samples are analyzed by gas chromatography (GC), direct-inlet mass spectrometry (DIMS), and Fourier-transform infrared spectroscopy (FTIR). The GC results, as well as other parameters, are utilized as input into the gas evaluation software tool (GEST) program for computation of pre-puncture gas compositions and pressures. Over 30 containers from the Hanford Site and the Rocky Flats Environmental Technology Site (RFETS) have been examined in the first three years of the surveillance program. Several containers were shown to have appreciable hydrogen content (some greater than 30 mol %), yet little or no oxygen was detected in any of the containers, including those exhibiting high hydrogen concentrations. Characteristics including moisture content, surface area, and material composition, along with the headspace gas composition, are utilized in an attempt to explain the chemical behavior of the packaged materials.

  3. [Determination of dichloromethane and trichloromethane residues in ranitidine hydrochloride by headspace liquid phase microextraction coupled with gas chromatography].

    Science.gov (United States)

    Shen, Shuchang; Yun, Dan; Li, Fei

    2009-11-01

    A method for the determination of residual dichloromethane and trichloromethane in ranitidine hydrochloride by headspace liquid phase microextraction coupled with gas chromatography (GC) was developed. A homemade device was used to protect the organic drop. The effects of the nature of extraction solvent, extraction time, extraction temperature and microdrop volume on the extraction efficiency were investigated separately. The optimal experimental conditions were as follows: 2 microL of n-tridecane as extraction solvent, 30 min of extraction time, 60 degrees C of extraction temperature. The correlation coefficients of linear calibration curve were 0.9733 and 0.9724 within the concentration ranges of dichloromethane (1-10 microg/g) and trichloromethane (1-10 microg/g), respectively. The detection limits of dichlormethane and trichloromethane were 0.0273 microg/g and 0.0410 microg/g, respectively, the relative standard deviations were lower than 4.36% and 5.89%, and the recoveries of the method were 93.6%-102% and 98.1% respectively. The method is simple and reliable.

  4. Biochar characteristics produced from food-processing products and their sorptive capacity for mercury and phenanthrene

    Science.gov (United States)

    Fotopoulou, Kalliopi N.; Karapanagioti, Hrissi K.; Manariotis, Ioannis D.

    2015-04-01

    Various organic-rich wastes including wood chips, animal manure, and crop residues have been used for biochar production. Biochar is used as an additive to soils to sequester carbon and improve soil fertility but its use as a sorbent for environmental remediation processes is gaining increased attention. Surface properties such as point of zero charge, surface area and pore volume, surface topography, surface functional groups and acid-base behavior are important factors, which affect sorption efficiency. Understanding the surface alteration of biochars increases our understanding of the pollutant-sorbent interaction. The scope of the present work was to evaluate the effect of key characteristics of biochars on their sorptive properties. Raw materials for biochar production were evaluated including byproducts from brewering, coffee, wine, and olive oil industry. The charring process was performed at different temperatures under limited-oxygen conditions using specialized containers. The surface area, the pore volume, and the average pore size of the biochars were determined. Open surface area and micropore volume were determined using t-plot method and Harkins & Jura equation. Raw food-processing waste demonstrates low surface area that increases by 1 order of magnitude by thermal treatment up to 750oC. At temperatures from 750 up to 900oC, pyrolysis results to biochars with surface areas 210-700 m2/g. For the same temperature range, a high percentage (46 to73%) of the pore volume of the biochars is due to micropores. Positive results were obtained when high surface area biochars were tested for their ability to remove organic (i.e. phenanthrene) and inorganic (i.e. mercury) compounds from aqueous solutions. All these properties point to new materials that can effectively be used for environmental remediation.

  5. Sorptive Uptake Studies of an Aryl-Arsenical with Iron Oxide Composites on an Activated Carbon Support

    OpenAIRE

    2014-01-01

    Sorption uptake kinetics and equilibrium studies for 4-hydroxy-3-nitrobenzene arsonic acid (roxarsone) was evaluated with synthetic magnetite (Mag-P), commercial magnetite (Mag-C), magnetite 10%, 19%, and 32% composite material (CM-10, -19, -32) that contains granular activated carbon (GAC), and synthetic goethite at pH 7.00 in water at 21 °C for 24 h. GAC showed the highest sorptive removal of roxarsone and the relative uptake for each sorbent material with roxarsone are listed in descending...

  6. Characterization of Brazilian green propolis throughout the seasons by headspace GC/MS and ESI-MS.

    Science.gov (United States)

    Nunes, Cleiton A; Guerreiro, Mário C

    2012-01-30

    A screening of the chemical composition of eight commercial classes of raw Brazilian green propolis throughout the seasons was carried out. A multivariate exploratory analysis of chemical composition obtained by gas chromatography associated with mass spectrometry with headspace extraction (HS-GC/MS), and by mass spectrometry with electrospray ionization (ESI-MS) was carried out using principal component analysis (PCA). Differences in the volatile and polyphenolic profiles of propolis samples were verified during the seasons. Within each season, the high quality commercial classes of propolis presented similar characteristics, while the low quality classes presented distinct compositions. In spring and summer, propolis of the trimming class, commonly considered of low quality by beekeepers, presented a composition similar to the superior quality propolis. Seasonality influences the chemical composition of the commercial classes of raw Brazilian green propolis. Headspace-GC/MS and ESI-MS assisted by PCA are effective to characterize volatile and non-volatile compounds of the propolis samples, and to correlate it to the seasons. Copyright © 2011 Society of Chemical Industry.

  7. Analysis of the volatiles in the headspace above the plasmodium and sporangia of the slime mould (Physarum polycephalum) by SPME-GCMS

    CERN Document Server

    Kateb, Huda al

    2013-01-01

    Solid phase micro-extraction (SPME) coupled with Gas Chromatography Mass Spectrometry (GC-MS) was used to extract and analyse the volatiles in the headspace above the plasmodial and sporulating stages of the slime mould Physarum Polycephalum. In total 115 compounds were identified from across a broad range of chemical classes. Although more (87) volatile organic compounds (VOCs) were identified when using a higher incubation temperature of 75oC, a large number of compounds (79) were still identified at the lower extraction temperature of 30oC and where the plasmodial stage was living. Far fewer compounds were extracted after sporulation at the two extraction temperatures. There were some marked differences between the VOCs identified in the plasmodial stage and after sporulation. In particular the nitrogen containing compounds acetonitrile, pyrrole, 2, 5-dimethyl-pyrazine and trimethyl pyrazine seemed to be associated with the sporulating stage. There were many compounds associated predominantly with the plas...

  8. Innovation in youth mental health services in Australia: common characteristics across the first headspace centres.

    Science.gov (United States)

    Rickwood, Debra; Van Dyke, Nina; Telford, Nic

    2015-02-01

    headspace centres comprise a significant innovation in community-based youth mental health service delivery in Australia. This paper examines the service activity of the first headspace centres to determine common and unique practice characteristics across headspace centres in this new approach to mental health service delivery. Data come from quarterly progress reports provided by the first 30 headspace centres during the 2010-2011 financial year. The information from 120 reports was analysed qualitatively using thematic analysis techniques to determine the types of activities reported by centres against key performance indicators. The main finding was the large number and wide range of centre activity. This heterogeneity may be explained in part by the diversity of communities across Australia and the importance that headspace places on addressing the specific needs of the local community as well as drawing upon the existing capacity that is available within a community. The most common activities were community engagement, building local partnerships and providing a youth friendly environment. There was a particularly strong focus by the majority of centres on establishing and supporting a Youth Reference Group to guide centre development and implementation. The progressive upscaling of headspace centres across Australia provides a unique opportunity to observe how a significant reorientation in health service delivery is implemented in practice to meet the needs of diverse communities. Further investigation of the headspace experience will provide critical lessons for other countries investing in new approaches to youth mental health. © 2013 Wiley Publishing Asia Pty Ltd.

  9. Sorptive Uptake Studies of an Aryl-Arsenical with Iron Oxide Composites on an Activated Carbon Support

    Directory of Open Access Journals (Sweden)

    Jae H. Kwon

    2014-03-01

    Full Text Available Sorption uptake kinetics and equilibrium studies for 4-hydroxy-3-nitrobenzene arsonic acid (roxarsone was evaluated with synthetic magnetite (Mag-P, commercial magnetite (Mag-C, magnetite 10%, 19%, and 32% composite material (CM-10, -19, -32 that contains granular activated carbon (GAC, and synthetic goethite at pH 7.00 in water at 21 °C for 24 h. GAC showed the highest sorptive removal of roxarsone and the relative uptake for each sorbent material with roxarsone are listed in descending order as follows: GAC (471 mg/g > goethite (418 mg/g > CM-10 (377 mg/g CM-19 (254 mg/g > CM-32 (227 mg/g > Mag-P (132 mg/g > Mag-C (29.5 mg/g. The As (V moiety of roxarsone is adsorbed onto the surface of the iron oxide/oxyhydrate and is inferred as inner-sphere surface complexes; monodentate-mononuclear, bidentate-mononuclear, and bidentate-binuclear depending on the protolytic speciation of roxarsone. The phenyl ring of roxarsone provides the primary driving force for the sorptive interaction with the graphene surface of GAC and its composites. Thus, magnetite composites are proposed as multi-purpose adsorbents for the co-removal of inorganic and organic arsenicals due to the presence of graphenic and iron oxide active adsorption sites.

  10. Review of Mass Spectrometry Data from Waste Tank Headspace Analyses

    Energy Technology Data Exchange (ETDEWEB)

    Sklarew, Debbie S.; Mitroshkov, Alexandre V.

    2006-02-28

    Numerous analytes have been categorized as tentatively identified compounds (TICs) in air samples from the headspaces of the Hanford Site high-level radioactive waste tanks. The tentative identification of these compounds was based mainly on the agreement between the observed mass spectra and a library of published mass spectra with consideration given to the gas chromatographic conditions and retention times. Many of the TICs were found in a limited number of tanks, were identified by only one laboratory or by one method, and/or were thought to be unlikely components of the waste or its degradation products. Consequently, the mass spectra of selected analytes have been reviewed to determine if their tentative identifications were correct. From our current review of 49 TICs, we found 25 that were misidentified and recommend that 54 of the associated results be flagged as suspect and 22 of the associated results be assigned a different compound name.

  11. Solvent desorption dynamic headspace sampling of fermented dairy product volatiles.

    Science.gov (United States)

    Rankin, S A

    2001-01-01

    A method was developed based on solvent desorption dynamic headspace analysis for the identification and relative quantification of volatiles significant to the study of fermented dairy product aroma. Descriptions of applications of this method are presented including the measurement of diacetyl and acetoin in fermented milk, the evaluation of volatile-hydrocolloid interactions in dairy-based matrices, and the identification of volatiles in cheeses for canonical discriminative analysis. Advantages of this method include rapid analysis, minimal equipment investment, and the ability to analyze samples with traditional GC split/splitless inlet systems. Limitations of this method are that the sample must be in the liquid state and the inherent analytical limitation to those compounds that do not coelute with the solvent or solvent impurity peaks.

  12. Ionic-liquid-assisted microwave distillation coupled with headspace single-drop microextraction followed by GC-MS for the rapid analysis of essential oil in Dryopteris fragrans.

    Science.gov (United States)

    Jiao, Jiao; Gai, Qing-Yan; Wang, Wei; Luo, Meng; Zhao, Chun-Jian; Fu, Yu-Jie; Ma, Wei

    2013-12-01

    A rapid, green and effective miniaturized sample preparation technique, ionic-liquid-assisted microwave distillation coupled with headspace single-drop microextraction was developed for the extraction of essential oil from dried Dryopteris fragrans. 1-Ethyl-3-methylimidazolium acetate was the optimal ionic liquid as the destruction agent of plant cell walls and microwave absorption was medium. n-Heptadecane (2.0 μL) was adopted as the suspended microdrop solvent in the headspace for the extraction and concentration of essential oil. The optimal parameters of the proposed method were an irradiation power of 300 W, sample mass of 0.9 g, mass ratio of ionic liquids to sample of 2.8, extraction temperature of 79°C, and extraction time of 3.6 min. In comparison to the previous reports, the proposed technique could equally monitor all the essential oil components with no significant differences in a simple way, which was more rapid and required a much lower amount of sample. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Vacuum-assisted headspace solid phase microextraction of polycyclic aromatic hydrocarbons in solid samples.

    Science.gov (United States)

    Yiantzi, Evangelia; Kalogerakis, Nicolas; Psillakis, Elefteria

    2015-08-26

    For the first time, Vacuum Assisted Headspace Solid Phase Microextraction (Vac-HSSPME) is used for the recovery of polycyclic aromatic hydrocarbons (PAHs) from solid matrices. The procedure was investigated both theoretically and experimentally. According to the theory, reducing the total pressure increases the vapor flux of chemicals at the soil surface, and hence improves HSSPME extraction kinetics. Vac-HSSPME sampling could be further enhanced by adding water as a modifier and creating a slurry mixture. For these soil-water mixtures, reduced pressure conditions may increase the volatilization rates of compounds with a low K(H) present in the aqueous phase of the slurry mixture and result in a faster HSSPME extraction process. Nevertheless, analyte desorption from soil to water may become a rate-limiting step when significant depletion of the aqueous analyte concentration takes place during Vac-HSSPME. Sand samples spiked with PAHs were used as simple solid matrices and the effect of different experimental parameters was investigated (extraction temperature, modifiers and extraction time). Vac-HSSPME sampling of dry spiked sand samples provided the first experimental evidence of the positive combined effect of reduced pressure and temperature on HSSPME. Although adding 2 mL of water as a modifier improved Vac-HSSPME, humidity decreased the amount of naphthalene extracted at equilibrium as well as impaired extraction of all analytes at elevated sampling temperatures. Within short HSSPME sampling times and under mild sampling temperatures, Vac-HSSPME yielded linear calibration curves in the range of 1-400 ng g(-1) and, with the exception of fluorene, regression coefficients were found higher than 0.99. The limits of detection for spiked sand samples ranged from 0.003 to 0.233 ng g(-1) and repeatability from 4.3 to 10 %. Finally, the amount of PAHs extracted from spiked soil samples was smaller compared to spiked sand samples, confirming that soil could bind target

  14. An Approach for Measuring the Sorptive Behavior of Odorants Using a Multifunction Thermal Desorber Unit: Preliminary Tests on Reduced Sulfur Compounds

    Directory of Open Access Journals (Sweden)

    Sang-Woo Joo

    2008-03-01

    Full Text Available In this study, the sorptive behavior of reduced sulfur compounds (RSC was investigated using a combination of thermal desorber (TD unit and gas chromatography (GC. To examine the sorptive properties of RSC on textile materials, two types of experiments were conducted under experimental conditions favorable for sorptive processes. In all the experiments, gaseous standards of hydrogen sulfide, methanethiol, dimethyl sulfide, and dimethyl disulfide were supplied to initiate the adsorption processes on textile pieces. The textile pieces were then forced to release those adsorbed RSC under a fixed condition. It was found that the extent of adsorption, if evaluated quantitatively, occurred at approximately 1/1000 to 1/100 of the level of RSC standards supplied originally to induce adsorption. It also indicated that RSC adsorption was affected very sensitively by the initial exposure durations to induce RSC adsorption with an exponential decrease in relative recovery (RR values with increasing exposure time. The relative sorptive patterns, when compared between different RSCs, were affected most sensitively by such factors as molecular weight and/or physical contact conditions.

  15. Prediction of the wine sensory properties related to grape variety from dynamic-headspace gas chromatography-olfactometry data.

    Science.gov (United States)

    Campo, Eva; Ferreira, Vicente; Escudero, Ana; Cacho, Juan

    2005-07-13

    Wine extracts obtained by a dynamic headspace sampling technique were studied by quantitative gas chromatography-olfactometry (GC-O) to determine the aroma profiles of six young monovarietal Spanish white wines. A partial least-square regression study was carried out to look for models relating wine aroma properties with GC-O scores. Models were validated by sensory analysis. Four out of the five most important sensory descriptors were satisfactorily described by a model, and sensory tests confirmed most of the predictions. The main aroma differences between these wines are due to the ratio linalool/3-mercaptohexyl acetate. Floral, sweet, and muscat are positively related to the concentration of linalool and negatively to that of 3-mercaptohexyl acetate. Tropical fruit is related to the wine content in this last odorant. 2-Phenyl acetate, reinforced by other acetates, can also contribute to floral and sweet notes. Alkyl-methoxypyrazines lessen the tropical fruit note, and acetic acid lessens the muscat nuance.

  16. Coupled extruder-headspace, a new method for analysis of the essential oil components of Coriandrum sativum fruits.

    Science.gov (United States)

    Sriti, Jazia; Msaada, Kamel; Talou, Thierry; Faye, Mamadou; Vilarem, Gerard; Marzouk, Brahim

    2012-10-15

    A new method involving concurrent single screw extruder combined with continuous headspace dynamic for the extraction and identification of the essential oil of Coriandrum sativum L. fruit was developed. The effect of six different nozzle diameters (5, 6, 7, 8, 9 and 10 mm) on the content and chemical composition of the essential oil of coriander fruit was studied. The oils from fruit samples were obtained by OMEGA 20 extruder. The result showed that the highest yield (0.53%) was obtained by the diameter of the nozzle was 8mm. Twenty-nine components were determined in essential oils, which were mostly hydrocarbons and alcohol monoterpenes. The main components linalool, α-pinene, γ-terpinene, p-cymene and limonene showed significant variations with drying trials.

  17. Headspace solid-phase microextraction for characterization of fragrances of lemon verbena (Aloysia triphylla) by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kim, Nam-Sun; Lee, Dong-Sun

    2004-01-01

    Natural fragrances from lemon verbena (Aloysia triphylla) were studied by headspace solid phase microextraction (HS-SPME) techniques followed by gas chromatography-mass spectrometry (GC-MS), with six different fibre coatings being tested to evaluate the extraction efficiencies of several selected compounds. A total of 14 compounds were identified in the fragrances of lemon verbena. Geranial and neral were detected as major components and alpha-pinene, beta-pinene, beta-caryophyllene, and curcumene as minor components. Enantiomeric analysis of chiral compounds from lemon verbena was carried out on a chiral column. alpha-Pinene, limonene, and camphor in the fragrances emitted from lemon verbena were found in the (+), (-), and (-) forms, respectively.

  18. Headspace solvent microextraction as a simple and highly sensitive sample pretreatment technique for ultra trace determination of geosmin in aquatic media.

    Science.gov (United States)

    Bagheri, Habib; Salemi, Amir

    2006-01-01

    A headspace solvent microextraction method was developed for the trace determination of geosmin, an odorant compound, in water samples. After performing the extraction by a microdrop of an organic solvent, the microdrop was introduced directly into a GC-MS injection port. One-at-the-time optimization strategy was applied to investigate and optimize some important extraction parameters such as type of solvent, drop volume, temperature, stirring rate, ionic strength, sample volume, and extraction time. The analytical data exhibited an RSD of less than 5% (n = 5), a linear calibration range of 5-900 ng/L (r2 > 0.998), and a detection limit of 0.8 and 3.3 ng/L using two different sets of selected ions. The proposed method was successfully applied to the extraction and determination of geosmin in the spiked real water sample and reasonable recovery was achieved.

  19. [Study of volatile organic compounds of fresh allium species using headspace combined with surface-enhanced Raman scattering].

    Science.gov (United States)

    Si, Min-Zhen; Zhang, De-Qing; Liu, Ren-Ming

    2014-09-01

    In order to identify volatile organic compounds of fresh plants at room temperature and avoid sample pretreatment and extractions which can be labor intensive, garlic, Chinese chives and scallion were chopped into pieces. Then some of them were placed in the headspace vial and sealed. The gases were drawn from the vial with a syringe and were injected very slowly into Ag colloids for test using R-3000 portable Raman spectrometer. The spectra of volatile organic compounds of allium species, fresh garlic, Chinese chive and shallot plants were successfully.recorded for the first time. For garlic high intensity bands are present at 307, 399, 569, 711, 1,182, 1,287, 1,397 and 1,622 cm(-1). For Chinese chives the high intensity band is present at 672 cm(-1). Low intensity bands are present at 274, 412, 575, 1,185, 1,289, 1,396, 1,618 cm(-1). For shallot high intensity bands are present at 693 cm(-1). Lower intensity bands are present at 372, 888, 1,023 cm(-1). Low intensity bands are present at 1,088, 1,211 and 1,322 cm(-1). The SERS of diallyl disulfide, allyl methyl sulfide and 1-propanethiol in liquid state and gas state were also obtained. The main volatile organic compound of fresh garlic, Chinese chive and shallot are diallyl disulfide, allyl methyl sulfide and 1-propanethiol respectively, and the volatile organic compound of fresh onion, scallion, shallot and chive are all 1-propanethiol. The presented results illustrate that combining headspace and SERS is a powerful tool for volatile organic compound analysis in fresh plants. The volatile organic compound can be detected in fresh plant samples directly and quickly without extraction.

  20. Determination of Polybrominated Diphenyl Ethers in Water Samples by Headspace Solid-Phase Microextraction Technique with Carbon Nanotube Coated Fibers

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    A headspace solid-phase microextraction (HS-SPME) method was developed for gas chromatography with electron-capture detection (GC-ECD) of polybrominated diphenyl ethers (PBDEs) in water samples. Silicon fibers coated with multiwalled carbon nanotube (MWCNT) with a 35 μm thickness were prepared for the SPME. Various parameters affecting the efficiency for the SPME of PBDEs, such as extraction time, temperature, agitation, volume of headspace, pH of sample, addition of salt and acetone were studied and optimized. The extraction efficiencies by HS-SPME and SPME at 25 and 100℃ were compared. At room temperature (ca. 25 ℃) the response obtained with SPME was 2-10 times higher than with HS-SPME. However, at 100℃ HS-SPME gave responses 1-8 times higher than SPME. The responses obtained with SPME and HS-SPME at 100℃ were higher than those at room temperature by a factor of 0.7-1.4 for SPME and by a factor of 2-40 for HS-SPME. The linear range of the developed method was 50-1600 ng/L with the linear correlation coefficients (r) ranging from 0.995 to 0.998. The limits of detection (S/N=3) for the five PBDEs were in the range of 1.1-16.0 ng/L and the precision (RSD, n=5) for peak area was 5.0%-9.1%. The developed method was successfully applied to the analysis of real water sam-ples with recovery of 74.2%-98.7%.

  1. Improvement of a headspace solid phase microextraction-gas chromatography/mass spectrometry method for the analysis of wheat bread volatile compounds.

    Science.gov (United States)

    Raffo, Antonio; Carcea, Marina; Castagna, Claudia; Magrì, Andrea

    2015-08-07

    An improved method based on headspace solid phase microextraction combined with gas chromatography-mass spectrometry (HS-SPME/GC-MS) was proposed for the semi-quantitative determination of wheat bread volatile compounds isolated from both whole slice and crust samples. A DVB/CAR/PDMS fibre was used to extract volatiles from the headspace of a bread powdered sample dispersed in a sodium chloride (20%) aqueous solution and kept for 60min at 50°C under controlled stirring. Thirty-nine out of all the extracted volatiles were fully identified, whereas for 95 other volatiles a tentative identification was proposed, to give a complete as possible profile of wheat bread volatile compounds. The use of an array of ten structurally and physicochemically similar internal standards allowed to markedly improve method precision with respect to previous HS-SPME/GC-MS methods for bread volatiles. Good linearity of the method was verified for a selection of volatiles from several chemical groups by calibration with matrix-matched extraction solutions. This simple, rapid, precise and sensitive method could represent a valuable tool to obtain semi-quantitative information when investigating the influence of technological factors on volatiles formation in wheat bread and other bakery products.

  2. Multivariate optimization of headspace trap for furan and furfural simultaneous determination in sponge cake.

    Science.gov (United States)

    Cepeda-Vázquez, Mayela; Blumenthal, David; Camel, Valérie; Rega, Barbara

    2017-03-01

    Furan, a possibly carcinogenic compound to humans, and furfural, a naturally occurring volatile contributing to aroma, can be both found in thermally treated foods. These process-induced compounds, formed by close reaction pathways, play an important role as markers of food safety and quality. A method capable of simultaneously quantifying both molecules is thus highly relevant for developing mitigation strategies and preserving the sensory properties of food at the same time. We have developed a unique reliable and sensitive headspace trap (HS trap) extraction method coupled to GC-MS for the simultaneous quantification of furan and furfural in a solid processed food (sponge cake). HS Trap extraction has been optimized using an optimal design of experiments (O-DOE) approach, considering four instrumental and two sample preparation variables, as well as a blocking factor identified during preliminary assays. Multicriteria and multiple response optimization was performed based on a desirability function, yielding the following conditions: thermostatting temperature, 65°C; thermostatting time, 15min; number of pressurization cycles, 4; dry purge time, 0.9min; water / sample amount ratio (dry basis), 16; and total amount (water + sample amount, dry basis), 10g. The performances of the optimized method were also assessed: repeatability (RSD: ≤3.3% for furan and ≤2.6% for furfural), intermediate precision (RSD: 4.0% for furan and 4.3% for furfural), linearity (R(2): 0.9957 for furan and 0.9996 for furfural), LOD (0.50ngfuran gsample dry basis(-1) and 10.2ngfurfural gsample dry basis(-1)), LOQ (0.99ngfuran gsample dry basis(-1) and 41.1ngfurfural gsample dry basis(-1)). Matrix effect was observed mainly for furan. Finally, the optimized method was applied to other sponge cakes with different matrix characteristics and levels of analytes.

  3. Dynamic headspace analysis of the release of volatile organic compounds from ethanolic systems by direct APCI-MS.

    Science.gov (United States)

    Tsachaki, Maroussa; Linforth, Robert S T; Taylor, Andrew J

    2005-10-19

    Static equilibrium headspace was diluted with a stream of nitrogen to study the stability of the volatile headspace concentration. The headspace dilution profile of 18 volatile compounds above aqueous and ethanolic solutions was measured in real time using atmospheric pressure chemical ionization-mass spectrometry. Under dynamic conditions the volatiles headspace concentration above water solutions decreased readily upon dilution. The presence of ethanol helped to maintain the volatile headspace concentration when the ethanol solution concentration was above 50 mL/L. This effect was such that under dynamic conditions the absolute volatile concentration above an ethanolic solution was higher than that above an aqueous solution, contrary to results observed in equilibrium studies. The ratio of the headspace concentration of volatiles above ethanolic 120 mL/L and water solutions was correlated to their air/water partition coefficient.

  4. Liquid-solid sample preparation followed by headspace solid-phase microextraction determination of multiclass pesticides in soil.

    Science.gov (United States)

    Durović, Rada D; Dordević, Tijana M; Santrić, Ljiljana R

    2012-01-01

    This paper describes development and validation of a multiresidue method for the determination of five pesticides (terbufos, prochloraz, chloridazon, pendimethalin, and fluorochloridone) belonging to different pesticide groups in soil samples by GC/MS, followed by its application in the analysis of some agricultural soil samples. The method is based on a headspace solid-phase microextraction method. Microextraction conditions, namely temperature, extraction time, and NaCI content, were tested and optimized using a 100 microm polydimethylsiloxane fiber. Three extraction solvents [methanol, methanol-acetone (1 + 1, v/v), and methanol-acetone-hexane (2 + 2 + 1, v/v/v)] and the optimum number of extraction steps within the sample preparation stage were optimized for the extraction procedure. LOD values for all the studied compounds were less than 12 microg/kg. Recovery values for multiple analyses of soil samples fortified at 30 microg/kg of each pesticide were higher than 64%. The method was proven to be repeatable, with RSD lower than 15%.

  5. Headspace Hanging Drop Liquid Phase Microextraction and Gas Chromatography-Mass Spectrometry for the Analysis of Flavors from Clove Buds

    Energy Technology Data Exchange (ETDEWEB)

    Jung, Mi Jin; Shin, Yeon Jae; Oh, Se Yeon; Kim, Nam Sun; Kim, Kun; Lee, Dong Sun [Seoul Women' s University, Seoul (Korea, Republic of)

    2006-02-15

    A novel sample pretreatment technique, headspace hanging drop liquid phase microextraction (HS-LPME) was studied and applied to the determination of flavors from solid clove buds by gas chromatography-mass spectrometry (GC-MS). Several parameters affecting on HS-LPME such as organic solvent drop volume, extraction time, extraction temperature and phase ratio were investigated. 1-Octanol was selected as the extracting solvent, drop size was fixed to 0.6 μL. 60 min extraction time at 25 .deg. C was chosen. HS-LPME has the good efficiency demonstrated by the higher partition equilibrium constant (K{sub lh}) values and concentration factor (CF) values. The limits of detection (LOD) were 1.5-3.2 ng. The amounts of eugenol, β-caryophyllene and eugenol acetate from the clove bud sample were 1.90 mg/g, 1.47 mg/g and 7.0 mg/g, respectively. This hanging drop based method is a simple, fast and easy sample enrichment technique using minimal solvent. HSLPME is an alternative sample preparation method for the analysis of volatile aroma compounds by GC-MS.

  6. HS-SPME/GC/MS法测定水中土臭素和2-甲基异崁醇的条件优化%Determination of GSM and 2-MIB in natural water by headspace solid-phase micro-extraction coupled with gas chromatography/mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    彭世富; 丁震; 夏卫文; 郑浩; 夏玉婷; 陈晓东

    2013-01-01

    目的:探索顶空固相微萃取-气相色谱/质谱法(HS-SPME/GC/MS)测定水中嗅味物质土臭素(GSM)和2-甲基异嵌醇(2-MIB)的最佳实验条件.方法:应用L32(49)正交表安排顶空固相微萃取-气相色谱/质谱法测定水中嗅味物质时的萃取温度、萃取时间、搅拌子转速、盐浓度、解吸时间和解吸温度并进行实验,优化各项操作参数.结果:顶空固相微萃取-气相色谱/质谱法测定水中嗅味物质的优化后实验条件是:萃取温度和解吸温度分别为65℃和260℃,萃取时间和解吸时间分别是40 min和7 min,搅拌子转速是600 r/min,盐浓度为30%(W/V).分别测定高低加标样,回收率为91%~107%,检出限(S/N=3)为0.04 ng/L,回收率为91%~104%,检出限(S/N=3)为0.13 ng/L.结论:通过正交实验设计优化实验条件,所建立的分析方法准确、简便、可靠,符合水中嗅味物质的测定要求.%Objective:To optimize the conditions for determination of the earthy and musty odors geosmin,2-methylisoborneol (2-MIB) in natural water by hcadspace solid-phase micro-extraction (SPME) coupled with gas chromatography/mass spectrometry and to establish a proposed method for determining the typical odor compounds in water.Methods:By applying the orthogonal experiment design L32(49) to arrange the determination conditions,several parameters of the extraction and desorption were studied and optimized (such as extraction temperature,desorption temperature,extraction time,ionic strength and rotate-speed),and some other parameters (such as correlation coefficient,limits of detection,RSD and recovery) were applied to evaluate effect of this method.Results:The optimum temperature of extraction and desorption were 65℃ and 260℃,respectively;time of extraction and desorption were 40 min and 7 min,respectively ;ionic strength,30% (W/V) ; rotate-speed,600 rpm.Under the optimized experimental conditions,limits of detection (S/N=3) were 0.04 and 0.42 ng/L for

  7. Investigations on the emission of fragrance allergens from scented toys by means of headspace solid-phase microextraction gas chromatography-mass spectrometry.

    Science.gov (United States)

    Masuck, Ines; Hutzler, Christoph; Luch, Andreas

    2010-04-30

    In the revised European toy safety directive 2009/48/EC the application of fragrance allergens in children's toys is restricted. The focus of the present work lies on the instrumental analytics of 13 banned fragrance allergens, as well as on 11 fragrance allergens that require declaration when concentrations surpass 100 microg per gram material. Applying a mixture of ethyl acetate and toluene solid/liquid extraction was performed prior to quantitative analysis of mass contents of fragrances in scented toys. In addition, an easy-to-perform method for the determination of emitted fragrances at 23 degrees C (handling conditions) or at 40 degrees C (worst case scenario) has been worked out to allow for the evaluation of potential risks originating from inhalation of these compounds during handling of or playing with toys. For this purpose a headspace solid-phase microextraction (HS-SPME) technique was developed and coupled to subsequent gas chromatography-mass spectrometry (GC-MS) analysis. Fragrance allergens were adsorbed (extracted) from the gas phase onto an 85 microm polyacrylate fiber while incubating pieces of the scented toys in sealed headspace vials at 23 degrees C and 40 degrees C. Quantification of compounds was performed via external calibration. The newly developed headspace method was subsequently applied to five perfumed toys. As expected, the emission of fragrance allergens from scented toys depends on the temperature and on the content of fragrance allergens present in those samples. In particular at conditions mimicking worst case (40 degrees C), fragrance allergens in toys may pose a risk to children since considerable amounts of compound might be absorbed by lung tissue via breathing of contaminated air.

  8. Comparison of two methods for extraction of volatiles from marine PL emulsions

    DEFF Research Database (Denmark)

    Lu, Henna Fung Sieng; Nielsen, Nina Skall; Jacobsen, Charlotte

    2013-01-01

    analysis. However, the CAR/PDMS‐SPME technique was efficient for lipid oxidation analysis in emulsions of less complex headspace. The SPME method extracted volatiles of lower molecular weights more efficient than the DHS method. On the other hand, DHS Tenax GR appeared to be more efficient in extracting......The dynamic headspace (DHS) thermal desorption principle using Tenax GR tube, as well as the solid phase micro‐extraction (SPME) tool with carboxen/polydimethylsiloxane 50/30 µm CAR/PDMS SPME fiber, both coupled to GC/MS were implemented for the isolation and identification of both lipid...... and Strecker derived volatiles in marine phospholipids (PL) emulsions. Comparison of volatile extraction efficiency was made between the methods. For marine PL emulsions with a highly complex composition of volatiles headspace, a fiber saturation problem was encountered when using CAR/PDMS‐SPME for volatiles...

  9. Rapid estimation of readily leachable triazine residues in soils using automatic kinetic bioaccessibility assays followed by on-line sorptive clean-up as a front-end to liquid chromatography.

    Science.gov (United States)

    Vida, Ana C F; Cocovi-Solberg, David J; Zagatto, Elias A G; Miró, Manuel

    2016-08-15

    An automatic batchwise bioaccessibility test was proposed for on-line monitoring of readily mobile pools of ametryn and atrazine residues in agricultural soils with different physicochemical properties. A 0.01molL(-1) CaCl2 solution mimicking rainwater percolation through the soil profiles was used for the herbicide extractions. The extract aliquots were successively sampled at regular time intervals in order to investigate the extraction kinetics. For extract clean-up and retention of freely dissolved target species, 30mg of restricted-access like copolymer were used as in-line sorptive material followed by elution with methanol and on-line heart-cut injection towards a C18 silica reversed-phase monolithic column (100×4.6mm) in a liquid chromatographic system. A mathematical model emphasized that the readily available pools vs time can be in most instances described by a first-order exponential equation, thus an asymptotical value is approached. Consequently, the leaching assays can be performed without attaining chemical equilibrium. Enhancement factors and detection limits were 10.2 and 18.8, and 0.40 and 0.37mgkg(-1) for ametryn and atrazine, respectively. The automatic method features good repeatability for leaching tests (r.s.d.: 11.8-10.2% for sandy and 3.7-6.2% for clayey soil). Reliable data, demonstrated with relative recoveries in the soil leachates ranging from 86 to 104%, were achieved in less than 35min, thus avoiding the need for up to 24h as recommended by standard leaching methods.

  10. Fast quality assessment of German chamomile (Matricaria chamomilla L.) by headspace solid-phase microextraction: influence of flower development stage.

    Science.gov (United States)

    Rafieiolhossaini, Mohammad; Adams, An; Sodaeizadeh, Hamid; Van Damme, Patrick; De Kimpe, Norbert

    2012-01-01

    For an adequate quality evaluation of aromatic plants grown under different conditions, a rapid, simple and sensitive method for the analysis of volatile constituents is indispensable. The main objective of the present study was to compare fast screening of German chamomile (Matricaria chamomilla L.) by means of headspace solid-phase microextraction (HS-SPME) with conventional isolation of the essential oil (steam distillation-solvent extraction (SDSE)) for the differentiation of chamomile essential oil constituents. Flowers were harvested at two distinct development stages: stage I, when ligulate flowers start to develop and tubular flowers are still closed, and stage II, when tubular flowers are partially to completely opened. Dried chamomile flowers at two development stages were extracted by means of both SDSE and HS-SPME, followed by GC-MS analysis. Among 30 compounds detected, (E)-beta-farnesene (49%), artemisia ketone (10%) and germacrene D (9%) were the predominant volatile components in the HS-SPME-extract, while alpha-bisabolol oxide A (42%), chamazulene (21%) and (Z)-spiroether (8%) were the main essential oil constituents among the 13 compounds obtained by SDSE. After statistical analysis of the data, both techniques enabled the same conclusion: (E)-beta-farnesene was the only compound which showed significant differences between the two flower development stages. These results suggest that HS-SPME-GC-MS can be used as a sensitive technique for the rapid screening and quality assessment of M. chamomilla.

  11. Quantification of 13 priority polycyclic aromatic hydrocarbons in human urine by headspace solid-phase microextraction gas chromatography-isotope dilution mass spectrometry.

    Science.gov (United States)

    Campo, Laura; Mercadante, Rosa; Rossella, Federica; Fustinoni, Silvia

    2009-01-12

    Polycyclic aromatic hydrocarbons (PAHs) are common environmental pollutants in both living and working environments. The aim of this study was the development of a headspace solid-phase microextraction gas chromatography-isotope dilution mass spectrometry (HS-SPME/GC-IDMS) method for the simultaneous quantification of 13 PAHs in urine samples. Different parameters affecting PAHs extraction by HS-SPME were considered and optimized: type/thickness of fiber coatings, extraction temperature/time, desorption temperature/time, ionic strength and sample agitation. The stability of spiked PAHs solutions and of real urine samples stored up to 90 days in containers of different materials was evaluated. In the optimized method, analytes were absorbed for 60min at 80 degrees C in the sample headspace with a 100mum polydimethylsiloxane fiber. The method is very specific, with linear range from the limit of quantification to 8.67 x 10(3)ngL(-1), a within-run precision of <20% and a between-run precision of <20% for 2-, 3- and 4-ring compounds and of <30% for 5-ring compounds, trueness within 20% of the spiked concentration, and limit of quantification in the 2.28-2.28 x 10(1)ngL(-1) range. An application of the proposed method using 15 urine samples from subjects exposed to PAHs at different environmental levels is shown.

  12. Quantification of 13 priority polycyclic aromatic hydrocarbons in human urine by headspace solid-phase microextraction gas chromatography-isotope dilution mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Campo, Laura [Department of Occupational and Environmental Health, University of Milan and Fondazione IRCCS Ospedale Maggiore Policlinico, Mangiagalli e Regina Elena, Milan (Italy)], E-mail: laura.campo@unimi.it; Mercadante, Rosa; Rossella, Federica; Fustinoni, Silvia [Department of Occupational and Environmental Health, University of Milan and Fondazione IRCCS Ospedale Maggiore Policlinico, Mangiagalli e Regina Elena, Milan (Italy)

    2009-01-12

    Polycyclic aromatic hydrocarbons (PAHs) are common environmental pollutants in both living and working environments. The aim of this study was the development of a headspace solid-phase microextraction gas chromatography-isotope dilution mass spectrometry (HS-SPME/GC-IDMS) method for the simultaneous quantification of 13 PAHs in urine samples. Different parameters affecting PAHs extraction by HS-SPME were considered and optimized: type/thickness of fiber coatings, extraction temperature/time, desorption temperature/time, ionic strength and sample agitation. The stability of spiked PAHs solutions and of real urine samples stored up to 90 days in containers of different materials was evaluated. In the optimized method, analytes were absorbed for 60 min at 80 deg. C in the sample headspace with a 100 {mu}m polydimethylsiloxane fiber. The method is very specific, with linear range from the limit of quantification to 8.67 x 10{sup 3} ng L{sup -1}, a within-run precision of <20% and a between-run precision of <20% for 2-, 3- and 4-ring compounds and of <30% for 5-ring compounds, trueness within 20% of the spiked concentration, and limit of quantification in the 2.28-2.28 x 10{sup 1} ng L{sup -1} range. An application of the proposed method using 15 urine samples from subjects exposed to PAHs at different environmental levels is shown.

  13. Seasonal changes in the composition of passively ventilated waste tank headspaces

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, J.L.; Hayes, J.C.; Buckley, L.L.; Jensen, L.; Pennington, L.D.; Wilmarth, S.R.

    1997-08-01

    The headspaces of four passively ventilated high-level radioactive waste tanks were sampled five times over a one-year period to evaluate seasonal changes in composition. Tanks BX-104, BY-108, C-107, and SX-102 were selected for the study on the bases of their widely varying headspace compositions, waste types, and physical headspace conditions. Samples were collected and analyzed for inorganic vapors, permanent gases, and organic vapors. Data from the 20 sampling events were compiled and reviewed. Raw mass spectral data for organic vapors were reprocessed by a single analyst. Measurement precision for results within individual sampling events, which includes both sampling and analytical random errors, was generally within the requirement of a 25% relative standard deviation. Data were fit to an analysis of variance (ANOVA) model and tested for correlation with headspace temperature. The ANOVA results indicate that the majority of headspace constituents studied were at relatively constant levels during the year-long study. The percent relative standard deviation (RSD{sub TIME}) of analyte means obtained for the five sampling events were generally low; only 15 of the 152 analytes had RSD{sub TIME} values above 60%. These highest RSD{sub TIME} values were obtained for 13 organic vapors in Tank BX-104 and two permanent gases in Tank C-107.

  14. Influence of headspace pressure on methane production in Biochemical Methane Potential (BMP) tests.

    Science.gov (United States)

    Valero, David; Montes, Jesús A; Rico, José Luis; Rico, Carlos

    2016-02-01

    The biochemical methane potential test is the most commonly applied method to determine methane production from organic wastes. One of the parameters measured is the volume of biogas produced which can be determined manometrically by keeping the volume constant and measuring increases in pressure. In the present study, the effect of pressure accumulation in the headspace of the reactors has been studied. Triplicate batch trials employing cocoa shell, waste coffee grounds and dairy manure as substrates have been performed under two headspace pressure conditions. The results obtained in the study showed that headspace overpressures higher than 600mbar affected methane production for waste coffee grounds. On the contrary, headspace overpressures within a range of 600-1000mbar did not affect methane production for cocoa shell and dairy manure. With the analyses performed in the present work it has not been possible to determine the reasons for the lower methane yield value obtained for the waste coffee grounds under high headspace pressures. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. Evaluation of headspace equilibration methods for quantifying greenhouse gases in groundwater.

    Science.gov (United States)

    Jahangir, M M R; Johnston, P; Khalil, M I; Grant, J; Somers, C; Richards, K G

    2012-11-30

    The objective of the study was to evaluate the different headspace equilibration methods for the quantification of dissolved greenhouse gases in groundwater. Groundwater samples were collected from wells with contrasting hydrogeochemical properties and degassed using the headspace equilibration method. One hundred samples from each well were randomly selected, treatments were applied and headspace gases analysed by gas chromatography. Headspace equilibration treatments varied helium (He):water ratio, shaking time and standing time. Mean groundwater N(2)O, CO(2) and CH(4) concentrations were 0.024 mg N L(-1), 13.71 mg C L(-1) and 1.63 μg C L(-1), respectively. All treatments were found to significantly influence dissolved gas concentrations. Considerable differences in the optimal He:water ratio and standing time were observed between the three gases. For N(2)O, CO(2) and CH(4) the optimum operating points for He:water ratio was 4.4:1, 3:1 and 3.4:1; shaking time was 13, 12 and 13 min; and standing time was 63, 17 and 108 min, respectively. The headspace equilibration method needs to be harmonised to ensure comparability between studies. The experiment reveals that He:water ratio 3:1 and shaking time 13 min give better estimation of dissolved gases than any lower or higher ratios and shaking times. The standing time 63, 17 and 108 min should be applied for N(2)O, CO(2) and CH(4), respectively.

  16. Monitoring of PAHs in air by collection on XAD-2 adsorbent then microwave-assisted thermal desorption coupled with headspace solid-phase microextraction and gas chromatography with mass spectrometric detection.

    Science.gov (United States)

    Wei, Ming-Chi; Chang, Wan-Ting; Jen, Jen-Fon

    2007-02-01

    Microwave-assisted thermal desorption (MAD) coupled to headspace solid-phase microextraction (HS-SPME) has been studied for in-situ, one-step, sample preparation for PAHs collected on XAD-2 adsorbent, before gas chromatography with mass spectrometric detection. The PAHs on XAD-2 were desorbed into the extraction solution, evaporated into the headspace by use of microwave irradiation, and absorbed directly on a solid-phase microextraction fiber in the headspace. After desorption from the SPME fiber in the hot GC injection port, PAHs were analyzed by GC-MS. Conditions affecting extraction efficiency, for example extraction solution, addition of salt, stirring speed, SPME fiber coating, sampling temperature, microwave power and irradiation time, and desorption conditions were investigated. Experimental results indicated that extraction of 275 mg XAD-2, containing 10-200 ng PAHs, with 10-mL ethylene glycol-1 mol L(-1) NaCl solution, 7:3, by irradiation with 120 W for 40 min (the same as the extraction time), and collection with a PDMS-DVB fiber at 35 degrees C, resulted in the best extraction efficiency. Recovery was more than 80% and RSD was less than 14%. Optimum desorption was achieved by heating at 290 degrees C for 5 min. Detection limits varied from 0.02 to 1.0 ng for different PAHs. A real sample was obtained by using XAD-2 to collect smoke from indoor burning of joss sticks. The amounts of PAHs measured varied from 0.795 to 2.53 ng. The method is a simple and rapid procedure for determination of PAHs on XAD-2 absorbent, and is free from toxic organic solvents.

  17. 超声波辅助-顶空固相微萃取-气相色谱法测定软木塞中痕量2,4,6-三氯苯甲醚%Determination of 2,4,6-trichloroanisole(TCA)in corks by ultrasonic oscillation assisted headspace solid-phase micro-extraction and gas chromatography

    Institute of Scientific and Technical Information of China (English)

    张素娟

    2015-01-01

    Through the optimization of the extraction process of Wine corks, a method for determining 2,4,6-trichloroanisole (TCA) in wine corks has been estabilished by using Ultrasonic Oscillation assisted HS-SPME-GC .The correlation coefficient for linearity (R2), limit of detection (LOD) and limit of quantification (LOQ) of this method were 0.999 8, 0.2 ng/g, and 0.5 ng/g, respectively. The precision expressed as relative standard deviation (RSD) was between 1.35%~5.47%, and recoveries ranged from 81.5%to 97.8%. The method is simple, quick, easy op-erating, high accuracy, good reproducibility and suitable for general laboratory to detect trace TCA residues in wine corks.%通过对软木塞样品提取过程的优化,建立了超声波法辅助顶空固相微萃取-气相色谱仪检测软木塞中痕量2,4,6-三氯苯甲醚(TCA)的方法。试验结果表明,该方法的线性范围0.5 ng/L~80.0 ng/L,R2为0.9998,线性关系良好。方法检出限为0.2 ng/g,方法定量限为0.5 ng/g,精密度(RSD)在1.35%~5.47%之间,加标回收率为81.5%~97.8%。该方法操作简便、快速、易操作、准确度高、重现性好,适用于普通实验室对软木塞中痕量2,4,6-三氯苯甲醚残留的检测。

  18. A novel approach to Lab-In-Syringe Head-Space Single-Drop Microextraction and on-drop sensing of ammonia.

    Science.gov (United States)

    Šrámková, Ivana; Horstkotte, Burkhard; Sklenářová, Hana; Solich, Petr; Kolev, Spas D

    2016-08-31

    A novel approach to the automation technique Lab-In-Syringe, also known as In-Syringe Analysis, is proposed which utilizes a secondary inlet into the syringe void, used as a size-adaptable reaction chamber, via a channel passing through the syringe piston. This innovative approach allows straightforward automation of head-space single-drop microextraction, involving accurately controlled drop formation and handling, and the possibility of on-drop analyte quantification. The syringe was used in upside-down orientation and in-syringe magnetic stirring was carried out, which allowed homogenous mixing of solutions, promotion of head-space analyte enrichment, and efficient syringe cleaning. The superior performance of the newly developed system was illustrated with the development of a sensitive method for total ammonia determination in surface waters. It is based on head-space extraction of ammonia into a single drop of bromothymol blue indicator created inside the syringe at the orifice of the syringe piston channel and on-drop sensing of the color change via fiber optics. The slope of the linear relationship between absorbance and time was used as the analytical signal. Drop formation and performance of on-drop monitoring was further studied with rhodamine B solution to give a better understanding of the system's performance. A repeatability of 6% RSD at 10 μmol L(-1) NH3, a linear range of up to 25 μmol L(-1) NH3, and a limit of detection of 1.8 μmol L(-1) NH3 were achieved. Study of interferences proved the high robustness of the method towards humic acids, high sample salinity, and the presence of detergents, thus demonstrating the method superiority compared to the state-of-the-art gas-diffusion methods. A mean analyte recovery of 101.8% was found in analyzing spiked environmental water samples.

  19. Development of a dynamic headspace gas chromatography-mass spectrometry method for on-site analysis of sulfur mustard degradation products in sediments.

    Science.gov (United States)

    Magnusson, R; Nordlander, T; Östin, A

    2016-01-15

    Sampling teams performing work at sea in areas where chemical munitions may have been dumped require rapid and reliable analytical methods for verifying sulfur mustard leakage from suspected objects. Here we present such an on-site analysis method based on dynamic headspace GC-MS for analysis of five cyclic sulfur mustard degradation products that have previously been detected in sediments from chemical weapon dumping sites: 1,4-oxathiane, 1,3-dithiolane, 1,4-dithiane, 1,4,5-oxadithiephane, and 1,2,5-trithiephane. An experimental design involving authentic Baltic Sea sediments spiked with the target analytes was used to develop an optimized protocol for sample preparation, headspace extraction and analysis that afforded recoveries of up to 60-90%. The optimized method needs no organic solvents, uses only two grams of sediment on a dry weight basis and involves a unique sample presentation whereby sediment is spread uniformly as a thin layer inside the walls of a glass headspace vial. The method showed good linearity for analyte concentrations of 5-200 ng/g dw, good repeatability, and acceptable carry-over. The method's limits of detection for spiked sediment samples ranged from 2.5 to 11 μg/kg dw, with matrix interference being the main limiting factor. The instrumental detection limits were one to two orders of magnitude lower. Full-scan GC-MS analysis enabled the use of automated mass spectral deconvolution for rapid identification of target analytes. Using this approach, analytes could be identified in spiked sediment samples at concentrations down to 13-65 μg/kg dw. On-site validation experiments conducted aboard the research vessel R/V Oceania demonstrated the method's practical applicability, enabling the successful identification of four cyclic sulfur mustard degradation products at concentrations of 15-308μg/kg in sediments immediately after being collected near a wreck at the Bornholm Deep dumpsite in the Baltic Sea.

  20. Development of the headspace Family and Friends Satisfaction Scale: Findings from a pilot study.

    Science.gov (United States)

    Nicholas, Angela; Holloway, Erin; Telford, Nic; Rickwood, Debra

    2017-04-19

    The primary aim of this pilot study was to determine the psychometric properties of the 18-item headspace Family and Friends Satisfaction Scale (hFAFSS). During August 2015, staff from 22 headspace centres approached family members and friends of young people attending headspace to complete the hFAFSS. Principal components analysis with oblique Promin rotation and polychoric correlations were used to assess the factor structure of the hFAFSS. There were 277 usable responses. Satisfaction was high, resulting in little variance. Parallel analyses suggested that the scale items tapped a single factor (68% of variance). This study is one of the first attempts to measure the satisfaction of family and friends with primary care-based youth mental health services. Satisfaction of family members and friends was shown to be high, but limited variance restricts the usability of the hFAFSS as an evaluation measure, and revision and further testing is needed. © 2017 John Wiley & Sons Australia, Ltd.

  1. Development of a sensory test method for odor measurement in a package headspace

    DEFF Research Database (Denmark)

    Reinbach, Helene Christine; Allesen-Holm, Bodil Helene; Kristoffersson, Lars

    2011-01-01

    The aim of the present study was to develop a sensory method to evaluate off-odors in a package headspace relative to a reference scale. Selection of panelists was performed with a questionnaire and with the Sniffin' stick test. A 1-butanol reference scale and three types of scales (a 15-cm line...... of the sensory panel to evaluation of different scaling techniques. Finally, a reliable and overtime fairly reproducible method for the evaluation of off-odors in the headspace of packages is presented....... to a physical intensity scale of 1-butanol and thus provides a valuable reference for comparing different package assessments over time. PRACTICAL APPLICATIONS A method for assessing off-odors in a package headspace is developed. The method development includes everything from selection and monitoring...

  2. Evidence That Certain Waste Tank Headspace Vapor Samples Were Contaminated by Semivolatile Polymer Additives

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, James L.

    2006-02-09

    Vapor samples collected from the headspaces of the Hanford Site high-level radioactive waste tanks in 1994 and 1995 using the Vapor Sampling System (VSS) were reported to contain trace levels of phthalates, antioxidants, and certain other industrial chemicals that did not have a logical origin in the waste. This report examines the evidence these chemicals were sampling artifacts (contamination) and identifies the chemicals reported as headspace constituents that may instead have been contaminants. Specific recommendations are given regarding the marking of certain chemicals as suspect on the basis they were sampling manifold contaminants.

  3. Headspace solid phase microextraction (HSSPME) for the determination of volatile and semivolatile pollutants in soils

    Energy Technology Data Exchange (ETDEWEB)

    Llompart, Maria [Departamento de Quimica Analitica Nutricion y Bromatologia, Facultad de Quimica, Universidad de Santiago de Compostela, E-15706 Santiago de Compostela (Spain); Li, Ken; Fingas, Merv [Emergencies Science Division, Environment Canada, Environmental Technology Centre, 3439 River Road, Ottawa, ON (Canada)

    1999-02-08

    We have investigated the use of headspace solid phase microextraction (HSSPME) as a sample concentration and preparation technique for the analysis of volatile and semivolatile pollutants in soil samples. Soil samples were suspended in solvent and the SPME fibre suspended in the headspace above the slurry. Finally, the fibre was desorbed in the Gas Chromatograph (GC) injection port and the analysis of the samples was carried out. Since the transfer of contaminants from the soil to the SPME fibre involves four separate phases (soil-solvent-headspace and fibre coating), parameters affecting the distribution of the analytes were investigated. Using a well-aged artificially spiked garden soil, different solvents (both organic and aqueous) were used to enhance the release of the contaminants from the solid matrix to the headspace. It was found that simple addition of water is adequate for the purpose of analysing the target volatile organic chemicals (VOCs) in soil. The addition of 1 ml of water to 1 g of soil yielded maximum response. Without water addition, the target VOCs were almost not released from the matrix and a poor response was observed. The effect of headspace volume on response as well as the addition of salt were also investigated. Comparison studies between conventional static headspace (HS) at high temperature (95C) and the new technology HSSPME at room temperature (=20C) were performed. The results obtained with both techniques were in good agreement. HSSPME precision and linearity were found to be better than automated headspace method and HSSPME also produced a significant enhancement in response. The detection and quantification limits for the target VOCs in soils were in the sub-ng g{sup -1} level. Finally, we tried to extend the applicability of the method to the analysis of semivolatiles. For these studies, two natural soils contaminated with diesel fuel and wood preservative, as well as a standard urban dust contaminated with polyaromatic

  4. COMPARISON OF VOLATILE COMPOUNDS IN TEUCRIUM POLIUM L. BY HEADSPACE AND HYDRODISTILLATION TECHNIQUES

    OpenAIRE

    2012-01-01

    Aerial parts of Teucrium polium were subjected to headspace (HS) and hydro-distillation (HD) techniques after drying, then headspace volatiles and the essential oil were analyzed by GC/MS. Forty-eight and Thirty-nine constituents were identified in hydro-distillation and CombiPAL system which represented 99.7% and 99.8% of the oils, respectively. hydro-distillation method were α-pinene (30.8%), β- pinene (12.0%), myrcene (8.9%), limonene (7.9%), (E)-caryophyllene (5.6%), Germacrene D (6.9%), ...

  5. Speciation of mercury compounds by gas chromatography with atomic emission detection. Simultaneous optimization of a headspace solid-phase microextraction and derivatization procedure by use of chemometric techniques

    Energy Technology Data Exchange (ETDEWEB)

    Carro, A.M.; Neira, I.; Rodil, R.; Lorenzo, R. A. [Univ. Santiago de Compostela (Spain). Dpto. Quimica Analitica, Nutricion y Bromatologia

    2003-06-01

    A method is proposed for the extraction and determination of organomercury compounds and Hg(II) in seawater samples by headspace solid-phase microextraction (HS-SPME) combined with capillary gas chromatography-microwave-induced plasma atomic emission spectrometry. The mercury species were derivatized with sodium tetraphenylborate, sorbed on a polydimethylsiloxane-coated fused-silica fibre, and desorbed in the injection port of the GC, in splitless mode. Experimental design methodology was used to evaluate the effect of six HS-SPME-derivatization variables: sample volume, NaBPh{sub 4} volume, pH, sorption time, extraction-derivatization temperature, and rate of stirring. Use of a multicriterion decision-making approach, with the desirability function, enabled determination of the optimum working conditions of the procedure for simultaneous analysis of three mercury species. (orig.)

  6. Analysis of Volatile Components of Adenosma indianum (Lour. Merr. by Steam Distillation and Headspace Solid-Phase Microextraction

    Directory of Open Access Journals (Sweden)

    Zhi Zeng

    2013-01-01

    Full Text Available The essential oil of Adenosma indianum (Lour. Merr. plays an important role in its antibacterial and antiphlogistic activities. In this work, the volatile components were extracted by steam distillation (SD and headspace solid-phase microextraction (HS-SPME and analysed by gas chromatography-mass spectrometry (GC-MS. A total of 49 volatile components were identified by GC-MS, and the major volatile components were α-limonene (20.59–35.07%, fenchone (15.79–31.81%, α-caryophyllene (6.98–10.32%, β-caryophyllene (6.98–10.19%, and piperitenone oxide (1.96–11.63%. The comparison of the volatile components from A. indianum (Lour. Merr. grown in two regions of China was reported. Also, the comparison of the volatile components by SD and HS-SPME was discussed. The results showed that the major volatile components of A. indianum (Lour. Merr. from two regions of China were similar but varied with different extraction methods. These results were indicative of the suitability of HS-SPME method for simple, rapid, and solvent-free analysis of the volatile components of the medicinal plants.

  7. Determination of acrylamide formed in asparagine/D-glucose maillard model systems by using gas chromatography with headspace solid-phase microextraction.

    Science.gov (United States)

    El-Ghorab, Ahmed H; Fujioka, Kazutoshi; Shibamoto, Takayuki

    2006-01-01

    A gas chromatographic method, along with a headspace solid-phase microextraction (HS-SPME), was developed for the determination of acrylamide formed in Maillard reaction model systems. The developed method was validated by liquid chromatography/mass spectrometry. A headspace sample was collected from an aqueous acrylamide solution (100 microg/mL) by SPME and directly injected into a gas chromatograph equipped with a nitrogen-phosphorus detector. The recovery of acrylamide from an aqueous solution was satisfactory, i.e, >93% under the conditions used. Acrylamide formed in an asparagine/D-glucose (molar ratio, 1/2) Maillard reaction model system heated at 150 and 170 degrees C for 20 min was collected and analyzed by the newly developed method using gas chromatography with nitrogen-phosphorus detection and HS-SPME. The amounts of acrylamide were 318 +/- 33 microg/g asparagine from a sample heated at 150 degrees C and 3329 +/- 176 microg/g asparagine from a sample heated at 170 degrees C. Addition of cysteamine or glutathione to the above model system reduced acrylamide formation. Acrylamide formation was not observed when cysteamine or glutathione was added to asparagine in the above model systems to obtain equimolar concentrations of both compounds. This newly developed method is simple and sensitive, and requires no solvent extraction.

  8. Determination of organotin compounds by headspace solid-phase microextraction-gas chromatography-pulsed flame-photometric detection (HS-SPME-GC-PFPD)

    Energy Technology Data Exchange (ETDEWEB)

    Bravo, Manuel [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique, LCABIE, UMR CNRS 5034, Pau (France); Pontificia Universidad Catolica de Valparaiso, Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Valparaiso (Chile); Lespes, Gaetane; Gautier, Martine Potin [Pontificia Universidad Catolica de Valparaiso, Laboratorio de Quimica Analitica y Ambiental, Instituto de Quimica, Valparaiso (Chile); Gregori, Ida de; Pinochet, Hugo [Universite de Pau et des Pays de L' Adour, Laboratoire de Chimie Analytique, LCABIE, UMR CNRS 5034, Pau (France)

    2005-12-01

    A method based on Headspace solid-phase microextraction (HS-SPME, with a 100 {mu}m PDMS-fiber) in combination with gas-chromatography and pulsed flame-photometric detection (GC-PFPD) has been investigated for simultaneous determination of eight organotin compounds. Monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), and the semi-volatile diphenyltin (DPhT), triphenyltin (TPhT), monooctyltin (MOcT), and dioctyltin (DOcT) were determined after derivatization with sodium tetraethylborate. The conditions used for the extraction and preconcentration step were optimised by experimental design methodology. Tripropyltin (TPrT) and diheptyltin (DHepT) were used as internal standards for quantification of volatile and semi-volatile organotin compounds, respectively. The analytical precision (RSD) for ten successive injections of a standard mixture containing all the organic tin compounds ranged between 2 and 11%. The limits of detection for all the organotin compounds were sub ng (Sn) L{sup -1} in water and close to ng (Sn) kg{sup -1} in sediments. The accuracy of the method was evaluated by analysis of two certified reference material (CRM) sediment samples. The HS-SPME-GC-PFPD was then applied to the analysis of three harbour sediment samples. The results showed that headspace SPME is an attractive tool for analysis of organotin compounds in solid environmental matrices. (orig.)

  9. Full evaporation dynamic headspace in combination with selectable one-dimensional/two-dimensional gas chromatography-mass spectrometry for the determination of suspected fragrance allergens in cosmetic products.

    Science.gov (United States)

    Devos, Christophe; Ochiai, Nobuo; Sasamoto, Kikuo; Sandra, Pat; David, Frank

    2012-09-14

    Suspected fragrance allergens were determined in cosmetic products using a combination of full evaporation-dynamic headspace (FEDHS) with selectable one-dimensional/two-dimensional GC-MS. The full evaporation dynamic headspace approach allows the non-discriminating extraction and injection of both apolar and polar fragrance compounds, without contamination of the analytical system by high molecular weight non-volatile matrix compounds. The method can be applied to all classes of cosmetic samples, including water containing matrices such as shower gels or body creams. In combination with selectable (1)D/(2)D GC-MS, consisting of a dedicated heart-cutting GC-MS configuration using capillary flow technology (CFT) and low thermal mass GC (LTM-GC), a highly flexible and easy-to-use analytical solution is offered. Depending on the complexity of the perfume fraction, analyses can be performed in one-dimensional GC-MS mode or in heart-cutting two-dimensional GC-MS mode, without the need of hardware reconfiguration. The two-dimensional mode with independent temperature control of the first and second dimension column is especially useful to confirm the presence of detected allergen compounds when mass spectral deconvolution is not possible.

  10. Simple and sensitive analysis of nereistoxin and its metabolites in human serum using headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Namera, A; Watanabe, T; Yashiki, M; Kojima, T; Urabe, T

    1999-03-01

    A simple method for the analysis of nereistoxin and its metabolites in human serum using headspace solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) is developed. A vial containing a serum sample, 5M sodium hydroxide, and benzylacetone (internal standard) is heated to 70 degrees C, and an SPME fiber is exposed for 30 min in the headspace of the vial. The compounds extracted by the fiber are desorbed by exposing the fiber in the injection port of the GC-MS. The calibration curves show linearity in the range of 0.05-5.0 micrograms/mL for nereistoxin and N-methyl-N-(2-methylthio-1-methylthiomethyl)ethylamine, 0.01-5.0 micrograms/mL for S,S'-dimethyl dihydronereistoxin, and 0.5-10 micrograms/mL for 2-methylthio-1-methylthiomethylethylamine in serum. No interferences are found, and the analysis time is 50 min for one sample. In addition, this proposed method is applied to a patient who attempted suicide by ingesting Padan 4R, a herbicide. Padan 4R contains 4% cartap hydrochloride, which is an analogue of nereistoxin. Nereistoxin and its metabolites are detected in the serum samples collected from the patient during hospitalization. The concentration ranges of nereistoxin in the serum are 0.09-2.69 micrograms/mL.

  11. Dispersion in oscillatory electro-osmotic flow through a parallel-plate channel with kinetic sorptive exchange at walls

    Institute of Scientific and Technical Information of China (English)

    吴朝安

    2014-01-01

    Dispersion in time-oscillatory electro-osmotic flows in a slit micro-channel under the effect of kinetic sorptive exchange at walls is theoretically investigated using the homogenization method. The two walls of the channel are considered to be made up of different materials, and therefore have different zeta potentials and sorption coefficients. A general expression for the Taylor disper-sion coefficient under different zeta potentials as well as various sorption conditions at the walls is derived analytically. The disper-sion coefficient is found to be dependent on the oscillation frequency, the Debye parameter, the species partition coefficient, the rea-ction kinetics and the ratio of the wall potentials. The results demonstrate that the presence of wall sorption tends to enhance the dispersion when the oscillation frequency is low, but the effect is negligible in high-frequency oscillatory flows. Moreover, it is found that the dispersion coefficient could be significantly changed by adjusting the relative wall potentials for low-frequency flows.

  12. Novel proton-type ionic liquid doped polyaniline for the headspace solid-phase microextraction of amines

    Energy Technology Data Exchange (ETDEWEB)

    Ai, Youhong [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072 (China); Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials & Key Laboratory for the Synthesis and Application of Organic Functional Molecules (Ministry of Education), College of Chemistry & Chemical Engineering, Hubei University, Wuhan 430062 (China); Zhao, Faqiong [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072 (China); Zeng, Baizhao, E-mail: bzzeng@whu.edu.cn [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072 (China)

    2015-06-23

    Graphical abstract: The novel proton-type ionic liquid (1-sulfobutyl-3-methylimidazolium hydrosulfate) doped polyaniline coating showed granular porous nanostructure and it had high self-EF values and extraction efficiency for amines. - Highlights: • A proton-type ionic liquid-doped polyaniline was fabricated by electrodeposition. • It showed porous granular nanostructure and had large specific surface. • It had high extraction capacity to aromatic amines. • A reasonable self-enrichment factor of SPME fiber has been proposed. - Abstract: A novel proton-type ionic liquid doped polyaniline (HIL-doped PANI) coating was presented, which was prepared on a stainless steel wire by electrodeposition in an aqueous solution containing aniline and 1-sulfobutyl-3-methylimidazolium hydrosulfate. The HIL-doped PANI coating showed granular nanostructure and had large specific surface. When it was applied to the headspace solid-phase microextraction of several amines (i.e., aniline, N-methylaniline, 3-methylaniline, 2-chloroaniline and 3-chloroaniline), it showed high extraction efficiency. The enrichment factors were 191.8–343.9 for different amines, much higher than those of common PANI and commercial polydimethylsiloxane/divinylbenzene coatings. Coupled with gas chromatographic analysis, the linear ranges were 0.097–100 μg/L with correlation coefficients above 0.9942, and the detection limits were 0.012–0.048 μg/L (S/N = 3) for different amines. The relative standard deviations (RSD) were smaller than 8.1% for five successive measurements with single fiber and the fiber-to-fiber RSDs were 8.6–13.8% (n = 5) for these amines. The proposed method was successfully applied to the extraction and determination of amines in organic waste water samples, and the recoveries were 78.3–112.8% for different analytes.

  13. Tank 241-C-106 headspace gas and vapor characterization results for samples collected in February 1994

    Energy Technology Data Exchange (ETDEWEB)

    Hackaby, J.L. [Pacific Northwest Lab., Washington, DC (United States); Bratzel, D.R. [Westinghouse Hanford Co., Richland, WA (United States)

    1995-09-26

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  14. Headspace Fourier transform infrared spectroscopy for the differentiation of Pandanus species.

    Science.gov (United States)

    Aganda, Kim Christopher C; Nonato, Maribel G; Sevilla, Fortunato; Santiago, Karen S

    2017-03-01

    Headspace Fourier Transform Infrared Spectroscopy (HS-FTIR) in tandem with chemometrics was applied to differentiate several species of the genus Pandanus. The headspace was generated from each Pandanus sample after incubation in a tightly sealed sample chamber. The resulting FTIR spectra of the headspace samples were found to be almost similar, but the application of principal component analysis (PCA) effectively differentiated the species. The unique spectral features for some samples were highlighted in the second-derivative FTIR spectra. A higher variance was exhibited in the PCA bi-plot of the 2nd derivative spectral data. The principal components differentiated not only the species, but also the cultivars or varieties, which formed distinct but proximate clusters. The manner of clustering obtained in this study resembled the behavior reported in a Random Amplified Polymorphic DNA analysis conducted on the Pandanus samples. The results demonstrate the potential of headspace FTIR spectroscopy as a simple, rapid, non-destructive, and relatively inexpensive method to discriminate between plant species and varieties.

  15. Technical note: Headspace analysis of explosive compounds using a novel sampling chamber.

    Science.gov (United States)

    DeGreeff, Lauryn; Rogers, Duane A; Katilie, Christopher; Johnson, Kevin; Rose-Pehrsson, Susan

    2015-03-01

    The development of instruments and methods for explosive vapor detection is a continually evolving field of interest. A thorough understanding of the characteristic vapor signatures of explosive material is imperative for the development and testing of new and current detectors. In this research a headspace sampling chamber was designed to contain explosive materials for the controlled, reproducible sampling and characterization of vapors associated with these materials. In a detonation test, the chamber was shown to contain an explosion equivalent to three grams of trinitrotoluene (TNT) without damage to the chamber. The efficacy of the chamber in controlled headspace sampling was evaluated in laboratory tests with bulk explosive materials. Small quantities of TNT, triacetone triperoxide (TATP) and hexamethylene triperoxide diamine (HMTD) were separately placed in the sampling chamber, and the headspace of each material was analyzed by gas chromatography/mass spectrometry (GC/MS) with online cryogenic trapping to yield characteristic vapor signatures for each explosive compound. Chamber sampling conditions, temperature and sampling time, were varied to demonstrate suitability for precise headspace analysis.

  16. Flight attraction of Spodoptera littoralis (Lepidoptera, Noctuidae to cotton headspace and synthetic volatile blends

    Directory of Open Access Journals (Sweden)

    Felipe eBorrero-Echeverry

    2015-06-01

    Full Text Available The insect olfactory system discriminates odor signals of different biological relevance, which drive innate behavior. Identification of stimuli that trigger upwind flight attraction towards host plants is a current challenge, and is essential in developing new, sustainable plant protection methods, and for furthering our understanding of plant-insect interactions. Using behavioral, analytical and electrophysiological studies, we here show that both females and males of the Egyptian cotton leafworm, Spodoptera littoralis (Lepidoptera, Noctuidae, use blends of volatile compounds to locate their host plant, cotton, Gossypium hirsutum (Malvales, Malvaceae. Female S. littoralis were engaged in upwind orientation flight in a wind tunnel when headspace collected from cotton plants was delivered through a piezoelectric sprayer. Although males took off towards cotton headspace significantly fewer males than females flew upwind towards the sprayed headspace. Subsequent assays with antennally active synthetic compounds revealed that a blend of nonanal, (Z-3 hexenyl acetate, (E-β-ocimene, and (R-(+-limonene was as attractive as cotton headspace to females and more attractive to males. DMNT and (R-(--linalool, both known plant defense compounds may have reduced the flight attraction of both females and males; more moths were attracted to blends without these two compounds. Our findings provide a platform for further investigations on host plant signals mediating innate behavior, and for the development of novel insect plant protection strategies against S. littoralis.

  17. Tank 241-U-103 headspace gas and vapor characterization results for samples collected in February 1995

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, J.L. [Pacific Northwest Lab., Richland, WA (United States); Bratzel, D.R. [Westinghouse Hanford Co., Richland, WA (United States)

    1995-09-27

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories.

  18. Tank 241-U-111 headspace gas and vapor characterization results for samples collected in February 1995

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, J.L. [Pacific Northwest Lab., Richland, WA (United States); Bratzel, D.R. [Westinghouse Hanford Co., Richland, WA (United States)

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories.

  19. Tank 241-SX-106 headspace gas and vapor characterization results for samples collected in March 1995

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, J.L. [Pacific Northwest Lab., Richland, WA (United States); Bratzel, D.R. [Westinghouse Hanford Co., Richland, WA (United States)

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories.

  20. Tank 241-S-102 headspace gas and vapor characterization results for samples collected in March 1995

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, J.L. [Pacific Northwest Lab., Richland, WA (United States); Bratzel, D.R. [Westinghouse Hanford Co., Richland, WA (United States)

    1995-09-26

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

  1. Tank 241-U-107 headspace gas and vapor characterization results for samples collected in February 1995

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, J.L. [Pacific Northwest Lab., Richland, WA (United States); Bratzel, D.R. [Westinghouse Hanford Co., Richland, WA (United States)

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories.

  2. Static and dynamic headspace analysis of instant coffee blends by proton-transfer-reaction mass spectrometry.

    Science.gov (United States)

    Romano, Andrea; Gaysinsky, Sylvia; Czepa, Andreas; Del Pulgar, José Sanchez; Cappellin, Luca; Biasioli, Franco

    2015-09-01

    Instant coffee is a widespread product, generally related to a high consumer acceptability, also because of its ease of preparation. The present work addresses the characterization of the headspace of freshly brewed instant coffees resulting from different blends, during and immediately after preparation. The sample set consisted of 10 coffees, obtained by mixing three different blends in different proportions. The employment of Proton Transfer Reaction-Mass Spectrometry (PTR-MS) allowed for direct and real-time sampling from the headspace, under conditions that mimic those that are encountered above the cup during and right after brewing. Different coffee brews were separated on the basis of the respective volatile profiles, and data showed good consistency with the respective blend compositions. When the headspace evolution was monitored during preparation, similar results were obtained in terms of blend separation; moreover, different blends displayed different and reproducible 'signatures' in terms of time evolution. A straightforward method for the prediction of headspace composition is proposed, allowing to predict the volatile profiles of two-component and three-component blends on the basis of the respective parent components. Overall, the results constitute a successful example of the applicability of PTR-MS as a tool for product development in food science. Copyright © 2015 John Wiley & Sons, Ltd.

  3. Bacterial bioremediation of selenium oxyanions using a dynamic flow bioreactor and headspace analysis

    Energy Technology Data Exchange (ETDEWEB)

    McCarty, S.L.; Chasteen, T.G. [Sam Houston State Univ., Huntsville, TX (United States). Dept. of Chemistry; Stalder, V.; Bachofen, R. [Univ. of Zuerich (Switzerland). Inst. of Plant Biology

    1995-12-31

    The volatile products of the biological reduction and methylation of selenium`s most common oxyanions, selenate and selenite, were determined using capillary gas chromatography and fluorine-induced chemiluminescence detection. Dimethyl selenide and dimethyl diselenide were detected in the headspace above cultures of bacteria resistant to this metalloid using static and dynamic headspace sampling techniques. Fluorine-induced chemiluminescence detection was applied to determine the relative concentrations of the organosulfur and organoselenium species released over many days of culture growth at a controlled temperature and purge rate. A selenium-resistant bacterium, Pseudomonas fluorescens K27, and a phototrophic bacterium Rhodobacter sphaeroides 2.4.1 were exposed to SeO{sub 4}{sup 2{minus}}, and the cultures` headspaces were examined over a period of several days for volatile selenium-containing products. The results show that the relative production of the volatile species over time depicts a pattern generally independent of the growth phase in the case of the phototrophic bacterium; the concentrations of metabolic dimethyl sulfide and dimethyl selenide determined in static headspace were highest after the microbe had been in stationary phase for 4 days.

  4. Tank 241-TY-104 headspace gas and vapor characterization results for samples collected in April 1995

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, J.L. [Pacific Northwest Lab., Richland, WA (United States); Bratzel, D.R. [Westinghouse Hanford Co., Richland, WA (United States)

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories.

  5. Headspace-Single Drop Microextraction Followed by Gas Chromatographic Determination of Key Aroma Compounds in Tomato Fruits and Their Sample Products

    Directory of Open Access Journals (Sweden)

    Vinita sawaddipanich

    2016-06-01

    Full Text Available A headspace-single drop microextraction (HS-SDME is a good choice to analyze volatile and semivolatile compounds in different matrices without any interference of the sample matrix. HS-SDME spends a very little solvent consumption for the determination of volatile aroma compounds (VACs. In this study, some VACs including 2-methylbutyraldehyde, 3-methyl-1-butanol, sec-butyl acetate, 1-octen-3-one and trans,trans-2,4-decadienal were performed with hexadecane as extraction solvent. The parameters affecting the HS-SDME method were investigated in details including extraction temperature, enrichment time, extraction time and sample volume. The optimum conditions were consisted of 45oC extraction temperature, 15min enrichment, 20min extraction time and 3mL sample volume. Comparison between liquid-liquid extraction (LLE and HS-SDME for quantitative analysis was carried out using tert-butanol as an internal standard. From results revealed that the recoveries were obtained between 81.06-90.55% for LLE and 80.26-90.09% for HS-SDME. The results demonstrated that the proposed method could be successfully applied for the determination of VACs.

  6. Multivariate optimization of a headspace solid-phase microextraction method followed by gas chromatography with mass spectrometry for the determination of terpenes in Nicotiana langsdorffii.

    Science.gov (United States)

    Ardini, Francisco; Carro, Marina Di; Abelmoschi, Maria Luisa; Grotti, Marco; Magi, Emanuele

    2014-07-01

    A simple and sensitive procedure based on headspace solid-phase microextraction and gas chromatography with mass spectrometry was developed for the determination of five terpenes (α-pinene, limonene, linalool, α-terpineol, and geraniol) in the leaves of Nicotiana langsdorffii. The microextraction conditions (extraction temperature, equilibration time, and extraction time) were optimized by means of a Doehlert design. The experimental design showed that, for α-pinene and limonene, a low temperature and a long extraction time were needed for optimal extraction, while linalool, α-terpineol, and geraniol required a high temperature and a long extraction time. The chosen compromise conditions were temperature 60°C, equilibration time 15 min and extraction time 50 min. The main analytical figures of the optimized method were evaluated; LODs ranged from 0.07 ng/g (α-pinene) to 8.0 ng/g (geraniol), while intraday and interday repeatability were in the range 10-17% and 9-13%, respectively. Finally, the procedure was applied to in vitro wild-type and transgenic specimens of N. langsdorffii subjected to abiotic stresses (chemical and heat stress). With the exception of geraniol (75-374 ng/g), low concentration levels of terpenes were measured (ng/g level or lower); some interesting variations in terpene concentration induced by abiotic stress were observed.

  7. Effects of headspace and oxygen level on off-gas emissions from wood pellets in storage.

    Science.gov (United States)

    Kuang, Xingya; Shankar, Tumuluru Jaya; Sokhansanj, Shahab; Lim, C Jim; Bi, Xiaotao T; Melin, Staffan

    2009-11-01

    Few papers have been published in the open literature on the emissions from biomass fuels, including wood pellets, during the storage and transportation and their potential health impacts. The purpose of this study is to provide data on the concentrations, emission factors, and emission rate factors of CO(2), CO, and CH(4) from wood pellets stored with different headspace to container volume ratios with different initial oxygen levels, in order to develop methods to reduce the toxic off-gas emissions and accumulation in storage spaces. Metal containers (45 l, 305 mm diameter by 610 mm long) were used to study the effect of headspace and oxygen levels on the off-gas emissions from wood pellets. Concentrations of CO(2), CO, and CH(4) in the headspace were measured using a gas chromatograph as a function of storage time. The results showed that the ratio of the headspace ratios and initial oxygen levels in the storage space significantly affected the off-gas emissions from wood pellets stored in a sealed container. Higher peak emission factors and higher emission rates are associated with higher headspace ratios. Lower emissions of CO(2) and CO were generated at room temperature under lower oxygen levels, whereas CH(4) emission is insensitive to the oxygen level. Replacing oxygen with inert gases in the storage space is thus a potentially effective method to reduce the biomass degradation and toxic off-gas emissions. The proper ventilation of the storage space can also be used to maintain a high oxygen level and low concentrations of toxic off-gassing compounds in the storage space, which is especially useful during the loading and unloading operations to control the hazards associated with the storage and transportation of wood pellets.

  8. Optimization of a novel headspace-solid-phase microextraction-gas chromatographic method by means of a Doehlert uniform shell design for the analysis of trace level ethylene oxide residuals in sterilized medical devices.

    Science.gov (United States)

    DiCicco, Michael P; Lang, Bridget; Harper, Thomas I

    2009-06-01

    Medical devices sterilized by ethylene oxide (EtO) retain trace quantities of EtO residuals, which may irritate patients' tissue. Reliably quantifying trace level EtO residuals in small medical devices requires an extremely sensitive analytical method. In this research, a Doehlert uniform shell design was utilized in obtaining a response surface to optimize a novel headspace-solid-phase microextraction-gas chromatographic (HS-SPME-GC) method developed for analyzing trace levels of EtO residuals in sterilized medical devices, by evaluating sterilized, polymer-coated, drug-eluting cardiovascular stents. The effects of four independent experimental variables (HS-SPME desorption time, extraction temperature, GC inlet temperature and extraction time) on GC peak area response of EtO were investigated simultaneously and the most influential experimental variables determined were extraction temperature and GC inlet temperature, with the fitted model showing no evidence of lack-of-fit. The optimized HS-SPME-GC method demonstrated overall good linearity/linear range, accuracy, repeatability, reproducibility, absolute recovery and high sensitivity. This novel method was successfully applied to analysis of trace levels of EtO residuals in sterilized/aerated cardiovascular stents of various lengths and internal diameter, where, upon heating, trace EtO residuals fully volatilized into HS for extraction, thereby nullifying matrix effects. As an alternative, this novel HS-SPME-GC method can offer higher sensitivity compared with conventional headspace analyzer-based sampling.

  9. Changes of headspace volatile constituents of palm olein and selected oils after frying French fries.

    Science.gov (United States)

    Omar, Muhammad Nor Bin; Nor, Nor Nazuha M; Idris, Nor Aini

    2007-04-01

    Changes of aroma constituents of palm olein and selected oils after frying French fries have been studied. The aroma constituents of used oils were collected using a solid-phase microextraction (SPME) headspace technique with an absorbent of a divinylbenzene/carboxen (DVB/CAR) (50/30 microm) on polydimethylsiloxane (PDMS) fibre. The extracted volatiles were desorbed from the fibre in the injection port of the gas chromatograph at 250 degrees C and the aroma constituents were identified by GC-MS. Analytical data showed that volatile constituents of palm olein, soybean oil, corn oil and sunflower oil changed while frying continued from 2 to 40 h, respectively. In palm olein, the 2t,4t-decadienal content decreased from 14.7 to 5.5 microg g(-1) (40 h) whilst hexanal increased from 7.9 microg g(-1) (2 h) to 29.2 microg g(-1) (40 h), respectively. Similar result was also obtained from soybean oil after frying French fries. The 2t,4t-decadienal content decreased from 15.9 microg g(-1) (2 h) to 3.2 microg g(-1) after 40 h frying whilst hexanal increased from 10.2 microg g(-1) (2 h) to 34.2 microg g(-1) (40 h). Meanwhile, in corn oil, it was found that 2t,4t-decadienal decreased from 15.6 microg g(-1) (2 h) to 3.2 microg g(-1) (40 h) whilst hexanal increased from 11.3 microg g(-1) (2 h) to 33.8 microg g(-1) when frying time reached 40 h. In sunflower oil, it was found that 2t,4t-decadienal, decreased from 16.8 microg g(-1) (2 h) to 1.2 microg g(-1) (40 h) while hexanal increased from 9.5 microg g(-1) (2 h) to 32.4 microg g(-1) when frying time reached 40 h. It also showed that used oils exhibited off-odour characteristics due to the increasing amount ofhexanal while their freshness characteristics diminished due to the decreasing amount of 2t, 4t-decadienal.

  10. Determination of roasted pistachio (Pistacia vera L.) key odorants by headspace solid-phase microextraction and gas chromatography-olfactometry.

    Science.gov (United States)

    Aceña, Laura; Vera, Luciano; Guasch, Josep; Busto, Olga; Mestres, Montserrat

    2011-03-23

    Key odorants in roasted pistachio nuts have been determined for the first time. Two different pistachio varieties (Fandooghi and Kerman) have been analyzed by means of headspace solid-phase microextraction (HS-SPME) and gas chromatography-olfactometry (GCO). The aroma extract dilution analyses (AEDA) applied have revealed 46 and 41 odor-active regions with a flavor dilution (FD) factor≥64 for the Fandooghi and the Kerman varieties, respectively, and 39 of them were related to precisely identified compounds. These included esters, pyrazines, aldehydes, acids, furans, and phenols. The results show that the Fandooghi variety presents, not only more odor-active regions but also higher FD factors than the Kerman variety that can lead to the conclusion that the first variety has a richer aromatic profile than the second one. The descriptive sensory analysis (DSA) showed that the roasted, chocolate/coffee, and nutty attributes were rated significantly higher in the Fandooghi variety, whereas the green attribute was significantly higher in the Kerman one.

  11. Development of a Direct Headspace Collection Method from Arabidopsis Seedlings Using HS-SPME-GC-TOF-MS Analysis

    Directory of Open Access Journals (Sweden)

    Kazuki Saito

    2013-04-01

    Full Text Available Plants produce various volatile organic compounds (VOCs, which are thought to be a crucial factor in their interactions with harmful insects, plants and animals. Composition of VOCs may differ when plants are grown under different nutrient conditions, i.e., macronutrient-deficient conditions. However, in plants, relationships between macronutrient assimilation and VOC composition remain unclear. In order to identify the kinds of VOCs that can be emitted when plants are grown under various environmental conditions, we established a conventional method for VOC profiling in Arabidopsis thaliana (Arabidopsis involving headspace-solid-phase microextraction-gas chromatography-time-of-flight-mass spectrometry (HS-SPME-GC-TOF-MS. We grew Arabidopsis seedlings in an HS vial to directly perform HS analysis. To maximize the analytical performance of VOCs, we optimized the extraction method and the analytical conditions of HP-SPME-GC-TOF-MS. Using the optimized method, we conducted VOC profiling of Arabidopsis seedlings, which were grown under two different nutrition conditions, nutrition-rich and nutrition-deficient conditions. The VOC profiles clearly showed a distinct pattern with respect to each condition. This study suggests that HS-SPME-GC-TOF-MS analysis has immense potential to detect changes in the levels of VOCs in not only Arabidopsis, but other plants grown under various environmental conditions.

  12. Profile of volatile compounds in 11 brandies by headspace solid-phase microextraction followed by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Zhao, Y; Xu, Y; Li, J; Fan, W; Jiang, W

    2009-03-01

    A headspace solid-phase microextraction (HS-SPME) method coupled with gas chromatography-mass spectrometry (GC-MS) was applied for the qualitative or semiquantitative characterization of brandy volatiles. SPME variables (SPME fiber, extraction temperature and time, and ethanol concentration) were optimized. A total of 144 compounds were from the brandies' volatiles, tentatively identified or identified by comparing mass spectra and retention indices of the standards or from literature. Of these, 57 are common to 11 brandies. They were mainly represented by esters and alcohols, such as 2-methyl propanol, 3-methyl butanol, 1-hexanol, ethyl octanoate, and ethyl decanoate, which were quantitatively determined. Chromatographic peaks were integrated using selective ion method (SIM) and the semiquantitative data analyzed using principal component analysis (PCA) and cluster analysis (CA) to study relationships between volatile composition and brandy. Eleven brandies were differentiated into 3 groups: 1 for Hennessy VSOP and XO samples, 1 for Changyu PEGASE VSOP and XO-1, 2, 3 samples, and the other for Changyu PEGASE brandy and VO, Taro brandy, Baiyang River brandy, and Wealth XO samples. The classification of groups is consistent with the brandy samples by variety and grade.

  13. Determination of lactones in wines by headspace solid-phase microextraction and gas chromatography coupled with mass spectrometry.

    Science.gov (United States)

    Pérez-Olivero, S J; Pérez-Pont, M L; Conde, J E; Pérez-Trujillo, J P

    2014-01-01

    Application of headspace solid-phase microextraction (HS-SPME) coupled with high-resolution gas chromatographic (HRGC) analysis was studied for determining lactones in wines. Six different SPME fibers were tested, and the influence of different factors such as temperature and time of desorption, ionic strength, time of extraction, content of sugar, ethanol, tannins and anthocyanins, and pH and influence of SO2 were studied. The proposed HS-SPME-GC method is an appropriate technique for the quantitative analysis of γ-butyrolactone, γ-hexalactone, trans-whiskey lactone, γ-octalactone, cis-whiskey lactone, γ-nonalactone, γ-decalactone, δ-decalactone, and γ-undecalactone in wines. Method reproducibility and repeatability ranged between 0.6 and 5.2% for all compounds. Detection limit for γ-butyrolactone was 0.17 mg/L and a few μg/L for the rest of the compounds. The optimized method has been applied to several wine samples.

  14. Second Order Kinetic Modeling of Headspace Solid Phase Microextraction of Flavors Released from Selected Food Model Systems

    Directory of Open Access Journals (Sweden)

    Jiyuan Zhang

    2014-09-01

    Full Text Available The application of headspace-solid phase microextraction (HS-SPME has been widely used in various fields as a simple and versatile method, yet challenging in quantification. In order to improve the reproducibility in quantification, a mathematical model with its root in psychological modeling and chemical reactor modeling was developed, describing the kinetic behavior of aroma active compounds extracted by SPME from two different food model systems, i.e., a semi-solid food and a liquid food. The model accounted for both adsorption and release of the analytes from SPME fiber, which occurred simultaneously but were counter-directed. The model had four parameters and their estimated values were found to be more reproducible than the direct measurement of the compounds themselves by instrumental analysis. With the relative standard deviations (RSD of each parameter less than 5% and root mean square error (RMSE less than 0.15, the model was proved to be a robust one in estimating the release of a wide range of low molecular weight acetates at three environmental temperatures i.e., 30, 40 and 60 °C. More insights of SPME behavior regarding the small molecule analytes were also obtained through the kinetic parameters and the model itself.

  15. Determination of Lactones in Wines by Headspace Solid-Phase Microextraction and Gas Chromatography Coupled with Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    S. J. Pérez-Olivero

    2014-01-01

    Full Text Available Application of headspace solid-phase microextraction (HS-SPME coupled with high-resolution gas chromatographic (HRGC analysis was studied for determining lactones in wines. Six different SPME fibers were tested, and the influence of different factors such as temperature and time of desorption, ionic strength, time of extraction, content of sugar, ethanol, tannins and anthocyanins, and pH and influence of SO2 were studied. The proposed HS-SPME-GC method is an appropriate technique for the quantitative analysis of γ-butyrolactone, γ-hexalactone, trans-whiskey lactone, γ-octalactone, cis-whiskey lactone, γ-nonalactone, γ-decalactone, δ-decalactone, and γ-undecalactone in wines. Method reproducibility and repeatability ranged between 0.6 and 5.2% for all compounds. Detection limit for γ-butyrolactone was 0.17 mg/L and a few μg/L for the rest of the compounds. The optimized method has been applied to several wine samples.

  16. Simple determination of fluoride in biological samples by headspace solid-phase microextraction and gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Kwon, Sun-Myung; Shin, Ho-Sang

    2015-08-14

    A simple and convenient method to detect fluoride in biological samples was developed. This method was based on derivatization with 2-(bromomethyl)naphthalene, headspace solid phase microextraction (HS-SPME) in a vial, and gas chromatography-tandem mass spectrometric detection. The HS-SPME parameters were optimized as follows: selection of CAR/PDMS fiber, 0.5% 2-(bromomethyl)naphthalene, 250 mg/L 15-crown-5-ether as a phase transfer catalyst, extraction and derivatization temperature of 95 °C, heating time of 20 min and pH of 7.0. Under the established conditions, the lowest limits of detection were 9 and 11 μg/L in 1.0 ml of plasma and urine, respectively, and the intra- and inter-day relative standard deviation was less than 7.7% at concentrations of 0.1 and 1.0 mg/L. The calibration curve showed good linearity of plasma and urine with r=0.9990 and r=0.9992, respectively. This method is simple, amenable to automation and environmentally friendly.

  17. Heavy metal removal mechanisms of sorptive filter materials for road runoff treatment and remobilization under de-icing salt applications.

    Science.gov (United States)

    Huber, Maximilian; Hilbig, Harald; Badenberg, Sophia C; Fassnacht, Julius; Drewes, Jörg E; Helmreich, Brigitte

    2016-10-01

    The objective of this research study was to elucidate the removal and remobilization behaviors of five heavy metals (i.e., Cd, Cu, Ni, Pb, and Zn) that had been fixed onto sorptive filter materials used in decentralized stormwater treatment systems receiving traffic area runoff. Six filter materials (i.e., granular activated carbon, a mixture of granular activated alumina and porous concrete, granular activated lignite, half-burnt dolomite, and two granular ferric hydroxides) were evaluated in column experiments. First, a simultaneous preloading with the heavy metals was performed for each filter material. Subsequently, the remobilization effect was tested by three de-icing salt experiments in duplicate using pure NaCl, a mixture of NaCl and CaCl2, and a mixture of NaCl and MgCl2. Three layers of each column were separated to specify the attenuation of heavy metals as a function of depth. Cu and Pb were retained best by most of the selected filter materials, and Cu was often released the least of all metals by the three de-icing salts. The mixture of NaCl and CaCl2 resulted in a stronger effect upon remobilization than the other two de-icing salts. For the material with the highest retention, the effect of the preloading level upon remobilization was measured. The removal mechanisms of all filter materials were determined by advanced laboratory methods. For example, the different intrusions of heavy metals into the particles were determined. Findings of this study can result in improved filter materials used in decentralized stormwater treatment systems.

  18. All rights reserved Development of Headspace Solid-Phase ...

    African Journals Online (AJOL)

    ADOWIE PERE

    Pesticide Residues in Fruit and Vegetable Samples using OFAT Design. *. 1,2. LUKMAN BOLA ... phase microextraction parameters (fiber coating type, extraction temperature and time, pH, salt addition ... production of food (Bakırcı, et al. 2014 ...

  19. Effect of ethanol, temperature, and gas flow rate on volatile release from aqueous solutions under dynamic headspace dilution conditions.

    Science.gov (United States)

    Tsachaki, Maroussa; Gady, Anne-Laure; Kalopesas, Michalis; Linforth, Robert S T; Athès, Violaine; Marin, Michele; Taylor, Andrew J

    2008-07-09

    On the basis of a mechanistic model, the overall and liquid mass transfer coefficients of aroma compounds were estimated during aroma release when an inert gas diluted the static headspace over simple ethanol/water solutions (ethanol concentration = 120 mL x L(-1)). Studied for a range of 17 compounds, they were both increased in the ethanol/water solution compared to the water solution, showing a better mass transfer due to the presence of ethanol, additively to partition coefficient variation. Thermal imaging results showed differences in convection of the two systems (water and ethanol/water) arguing for ethanol convection enhancement inside the liquid. The effect of ethanol in the solution on mass transfer coefficients at different temperatures was minor. On the contrary, at different headspace dilution rates, the effect of ethanol in the solution helped to maintain the volatile headspace concentration close to equilibrium concentration, when the headspace was replenished 1-3 times per minute.

  20. Differentiating organically and conventionally grown oregano using ultraperformance liquid chromatography mass spectrometry (UPLC-MS), headspace gas chromatography with flame ionization detection (headspace-GC-FID), and flow injection mass spectrum (FIMS) fingerprints combined with multivariate data analysis.

    Science.gov (United States)

    Gao, Boyan; Qin, Fang; Ding, Tingting; Chen, Yineng; Lu, Weiying; Yu, Liangli Lucy

    2014-08-13

    Ultraperformance liquid chromatography mass spectrometry (UPLC-MS), flow injection mass spectrometry (FIMS), and headspace gas chromatography (headspace-GC) combined with multivariate data analysis techniques were examined and compared in differentiating organically grown oregano from that grown conventionally. It is the first time that headspace-GC fingerprinting technology is reported in differentiating organically and conventionally grown spice samples. The results also indicated that UPLC-MS, FIMS, and headspace-GC-FID fingerprints with OPLS-DA were able to effectively distinguish oreganos under different growing conditions, whereas with PCA, only FIMS fingerprint could differentiate the organically and conventionally grown oregano samples. UPLC fingerprinting provided detailed information about the chemical composition of oregano with a longer analysis time, whereas FIMS finished a sample analysis within 1 min. On the other hand, headspace GC-FID fingerprinting required no sample pretreatment, suggesting its potential as a high-throughput method in distinguishing organically and conventionally grown oregano samples. In addition, chemical components in oregano were identified by their molecular weight using QTOF-MS and headspace-GC-MS.

  1. Geochemistry of drill core headspace gases and its significance in gas hydrate drilling in Qilian Mountain permafrost

    Science.gov (United States)

    Lu, Zhengquan; Rao, Zhu; He, Jiaxiong; Zhu, Youhai; Zhang, Yongqin; Liu, Hui; Wang, Ting; Xue, Xiaohua

    2015-02-01

    Headspace gases from cores are sampled in the gas hydrate drilling well DK-8 in the Qilian Mountain permafrost. Gas components and carbon isotopes of methane from headspace gas samples are analyzed. The geochemical features of the headspace gases along the well profile are compared with occurrences of gas hydrate, and with the distribution of faults or fractures. Their geochemical significance is finally pointed out in gas hydrate occurrences and hydrocarbon migration. Results show high levels of hydrocarbon concentrations in the headspace gases at depths of 149-167 m, 228-299 m, 321-337 m and 360-380 m. Visible gas hydrate and its associated anomalies occur at 149-167 m and 228-299 m; the occurrence of high gas concentrations in core headspace gases was correlated to gas hydrate occurrences and their associated anomalies, especially in the shallow layers. Gas compositions, gas ratios of C1/ΣC1-5, C1/(C2 + C3), iC4/nC4, and iC5/nC5, and carbon isotopic compositions of methane (δ13C1, PDB‰) indicate that the headspace gases are mainly thermogenic, partly mixed with biodegraded thermogenic sources with small amounts derived from microbial sources. Faults or fracture zones are identified at intervals of 149-167 m, 228-299 m, 321-337 m, and near 360-380 m; significantly higher gas concentrations and lower dryness ratio were found in the headspace gases within the fault or fracture zones compared with areas above these zones. In the shallow zones, low dryness ratios were observed in headspace gases in zones where gas hydrate and faults or fracture zones were found, suggesting that faults or fracture zones serve as migration paths for gases in the deep layers and provide accumulation space for gas hydrate in the shallow layers of the Qilian Mountain permafrost.

  2. Purge-assisted headspace solid-phase microextraction combined with gas chromatography/mass spectrometry for the determination of trace nitrated polycyclic aromatic hydrocarbons in aqueous samples.

    Science.gov (United States)

    Hung, Cheng-Han; Ho, Hsin-Pin; Lin, Mei-Tzu; Chen, Chung-Yu; Shu, Youn-Yuen; Lee, Maw-Rong

    2012-11-23

    This study describes a new procedure, namely, purge-assisted headspace solid phase microextraction combined with gas chromatography/negative ion chemical ionization mass spectrometry (PA/HS-SPME-GC/NICI-MS), which is used to determine seven nitrated polycyclic aromatic hydrocarbons (NPAHs) in aqueous samples. High extraction efficiency was obtained with PA/HS-SPME with polydimethylsiloxane (PDMS) fiber coating. A programmable temperature vaporizing (PTV) inlet was used in the desorption process. Selected ion monitoring (SIM) was used for quantitative and qualitative purposes. The linear range of detection of the proposed method was 5-5000 pg/mL with coefficients of determination between 0.995 and 0.999. Limits of detection (LODs) for seven NPAHs were 0.01-0.06 pg/mL. The relative standard deviation was below 12.7% at a concentration of 50 pg/mL. Compared with headspace-solid phase microextraction (HS-SPME), the purge procedure enhanced the extraction efficiency for high boiling point analytes, such as 7-nitrobenz[a]anthracene (7-NBA) and 6-nitrochrysene (6-NC). The proposed method provides a sensitive method for NPAH analysis at the pg/mL level. The application of the proposed method for the determination of trace NPAHs in real samples was investigated by analyzing aqueous samples from rivers. The concentrations of NPAHs detected from the samples ranged from 5.2 to 7.5 pg/mL. This method was applied successfully in the analysis of trace NPAHs in river samples.

  3. Dynamic headspace analyses of residual volatiles in pharmaceuticals.

    Science.gov (United States)

    Wampler, T P; Bowe, W A; Levy, E J

    1985-02-01

    Pharmaceutical preparations may be assayed for volatile organic compounds by purging them with a stream of inert carrier gas and collecting the organics onto a suitable sorbent material, from which they may be backflushed to a gas chromatograph. Compared to solvent extraction, the process offers advantages of increased sensitivity, ease of automation, and elimination of the solvent peak. Examples are given of three major sources of volatiles in pharmaceuticals, with the development of a method for quantitating the volatiles using an internal standard.

  4. Biomonitoring of benzene and toluene in human blood by headspace-solid-phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Schimming, E.; Levsen, K. [Fraunhofer-Institut fuer Toxikologie und Aerosolforschung (ITA), Hannover (Germany); Koehme, C.; Schuermann, W. [Medizinische Hochschule Hannover (Germany). Abt. fuer Pneumologie

    1999-01-01

    A simple and rapid method for the determination of benzene and toluene in whole blood by headspace-solid-phase microextraction (HS-SPME) is described. Using SPME fibres coated with 65 {mu}m carboxene/polydimethylsiloxane, limits of quantification (LOQ) of 5 ng/L for benzene and 25 ng/L for toluene are achieved. As a result of its large linear range (i.e. 5-5000 ng/L for benzene) the method is suitable for biomonitoring of both occupationally and environmentally exposed people. The reproducibility of the determination of benzene is {<=} 8%. An interlaboratory comparison demonstrated that the method proposed here compares favorably with existing methods (dynamic headspace, purge and trap). (orig.) With 2 figs., 2 tabs., 10 refs.

  5. Method Development for Container Closure Integrity Evaluation via Headspace Gas Ingress by Using Frequency Modulation Spectroscopy.

    Science.gov (United States)

    Victor, Ken G; Levac, Lauren; Timmins, Michael; Veale, James

    2017-07-20

    USP Section 3.5 states that "A deterministic leak test method having the ability to detect leaks at the product's maximum allowable leakage limit is preferred when establishing the inherent integrity of a container-closure system." Ideally, container closure integrity (CCI) of parenteral packaging would be evaluated by measuring a physical property that is sensitive to the presence of any package defect that breaches package integrity by increasing its leakage above its maximum allowable leakage limit (MALL). The primary goals of the work presented herein were to demonstrate the viability of the non-destructive, deterministic method known as laser-based gas headspace analysis for evaluating CCI and to provide a physical model for predicting leak rates for a variety of container volumes, headspace conditions and defect sizes. The results demonstrate that laser-based headspace analysis provides sensitive, accurate and reproducible measurements of the gas ingress into glass vial-stopper package assemblies that are under either diffusive or effusive leak conditions. Two different types of positive controls were examined. First, laser-drilled micro-holes in thin metal disks that were crimped on top of 15R glass vials served as positive controls with a well-characterized defect geometry. For these, a strong correlation was observed between the measured ingress parameter and the size of the defect for both diffusive and effusive conditions. Second, laser-drilled holes in the wall of glass vials served as controls that more closely simulate "real world" defects. Due to their complex defect geometries, their diffusive and effusive ingress parameters did not necessarily correlate; this is an important observation that has significant implications for standardizing the characterization of container defects. Regardless, laser-based headspace analysis could readily differentiate positive and negative controls for all leak conditions and the results provide a guide for method

  6. Evaluation of noni (Morinda citrifolia) volatile profile by dynamic headspace and gas chromatography-mass spectrometry

    OpenAIRE

    Sousa, A.; M. A. SOUZA NETO; GARRUTI, D. dos S.; Sousa, J. A.; BRITO, E. S. de

    2010-01-01

    Noni is a fruit that has interested the scientific community due to its medicinal and functional activities. Different products that contain noni are already in the market, but their consumption could be impaired by their distinctive unpleasant aroma and flavor. The aim of this work was to evaluate the noni pulp volatile profile by dynamic headspace and gas chromatography-mass spectrometry. Thirty seven volatile compounds were detected, mainly alcohols (63.3%), esters (26.9%), cetones (7.4%),...

  7. TOXICITY CHARACTERISTIC LEACHING PROCEDURE APPLIED TO RADIOACTIVE SALTSTONE CONTAINING TETRAPHENYLBORATE: DEVELOPMENT OF A MODIFIED ZERO-HEADSPACE EXTRACTOR

    Energy Technology Data Exchange (ETDEWEB)

    Crapse, K.; Cozzi, A.; Crawford, C.; Jurgensen, A.

    2006-09-30

    In order to assess the effect of extended curing times at elevated temperatures on saltstone containing Tank 48H waste, saltstone samples prepared as a part of a separate study were analyzed for benzene using a modification of the United States Environmental Protection Agency (USEPA) method 1311 Toxicity Characteristic Leaching Procedure (TCLP). To carry out TCLP for volatile organic analytes (VOA), such as benzene, in the Savannah River National Laboratory (SRNL) shielded cells (SC), a modified TCLP Zero-Headspace Extractor (ZHE) was developed. The modified method was demonstrated to be acceptable in a side by side comparison with an EPA recommended ZHE using nonradioactive saltstone containing tetraphenylborate (TPB). TCLP results for all saltstone samples tested containing TPB (both simulant and actual Tank 48H waste) were below the regulatory limit for benzene (0.5 mg/L). In general, higher curing temperatures corresponded to higher concentrations of benzene in TCLP extract. The TCLP performed on the simulant samples cured under the most extreme conditions (3000 mg/L TPB in salt and cured at 95 C for at least 144 days) resulted in benzene values that were greater than half the regulatory limit. Taking into account that benzene in TCLP extract was measured on the same order of magnitude as the regulatory limit, that these experimental conditions may not be representative of actual curing profiles found in the saltstone vault and that there is significant uncertainty associated with the precision of the method, it is recommended that to increase confidence in TCLP results for benzene, the maximum curing temperature of saltstone be less than 95 C. At this time, no further benzene TCLP testing is warranted. Additional verification would be recommended, however, should future processing strategies result in significant changes to salt waste composition in saltstone as factors beyond the scope of this limited study may influence the decomposition of TPB in saltstone.

  8. Automated dynamic headspace organic solvent film microextraction for benzene, toluene, ethylbenzene and xylene. Renewable liquid film as a sampler by a programmable motor.

    Science.gov (United States)

    Mohammadi, Abdorreza; Alizadeh, Naader

    2006-02-24

    A simple, fast and efficient dynamic headspace-organic solvent film microextraction (DHS-OSFME) method using a new automatic device was developed. The renewable organic films were formed inside a microsyringe barrel using the uniform and repeated movement of the syringe plunger enabled by programmable stirring motor. The plunger speed, number of extraction cycles, and dwell time (stop time after each half round) were controlled by a computer software, which was written by C++ Builder. A theoretical treatment of the DHS-OSFME based on the consecutive first-order process is proposed in this report. A mathematical solution for the dynamic process of the mass transfer was obtained by correlating the variation of analyte concentration in the syringe volume with the plunger speed and the amount of analyte extracted to the OSF. Benzene, toluene, ethylbenzene, and o-xylene (BTEX) were employed as model compounds to assess the extraction procedure and were determined by gas chromatography-flame ionization detection. Of the three organic solvents (1-octanol, benzyl alcohol and n-dodecane) studied as extractants, n-dodecane proved to be the most sensitive solvent for the extraction of these analytes. Several parameters, including the syringe withdrawal rate, dwelling time, number of extraction cycles, sampling volume, sample temperature, and ionic strength of the solution, were investigated for their effects on the extraction performance. The calibration graphs were linear in the range of 0.5-200 ng ml(-1), with the detection limits between 0.18 and 0.35 ng ml(-1). Wastewater samples were extracted by the optimized method, and determined using the standard addition method.

  9. Simultaneous Determination of Benzene and Toluene in Pesticide Emulsifiable Concentrate by Headspace GC-MS

    Directory of Open Access Journals (Sweden)

    Lidong Cao

    2013-01-01

    Full Text Available The toxic inert ingredients in pesticide formulations are strictly regulated in many countries. In this paper, a simple and efficient headspace-gas chromatography-mass spectrometry (HSGC-MS method using fluorobenzene as an internal standard (IS for rapid simultaneous determination of benzene and toluene in pesticide emulsifiable concentrate (EC was established. The headspace and GC-MS conditions were investigated and developed. A nonpolar fused silica Rtx-5 capillary column (30 m×0.20 mm i.d. and 0.25 μm film thickness with temperature programming was used. Under optimized headspace conditions, equilibration temperature of 120°C, equilibration time of 5 min, and sample size of 50 μL, the regression of the peak area ratios of benzene and toluene to IS on the concentrations of analytes fitted a linear relationship well at the concentration levels ranging from 3.2 g/L to 16.0 g/L. Standard additions of benzene and toluene to blank different matrix solutions 1ead to recoveries of 100.1%–109.5% with a relative standard deviation (RSD of 0.3%–8.1%. The method presented here stands out as simple and easily applicable, which provides a way for the determination of toxic volatile adjuvant in liquid pesticide formulations.

  10. Effects of alpha-tocopherol on lactones in beef headspace during storage.

    Science.gov (United States)

    Watanabe, A; Imanari, M; Higuchi, M; Shiba, N; Yonai, M

    2010-01-01

    We studied the effect of alpha-tocopherol (alpha-Toc) on the production of lactones, a desirable flavor in Wagyu beef (Japanese Black Cattle), in meat headspace. Fresh beef was minced and divided into 4 groups containing different alpha-Toc levels (1.9, 2.7, 6.1, and 10.7 mg/kg) or packed with oxygen absorber. After 10 d of storage at 2 °C, these samples were cooked in distilled water and rendered fat was collected. The headspace of the fat was analyzed with solid-phase microextraction combined with gas chromatography-mass spectrometry. The DB-17MS capillary column led to good separation of aliphatic lactones. Oxygen was important for the development of all lactones during storage. The amounts of gamma-octalactone and gamma-nonalactone decreased linearly with increasing alpha-Toc levels. The effect of alpha-Toc on delta-decalactone, delta-undecalactone, and delta-tetoradecalactone was weaker, and that on delta-hexadecalactone was ambiguous. These observations suggest that oxidation was necessary to develop the flavor of Wagyu beef, and warn that an excessive increase of alpha-Toc could reduce levels of positive flavor components, gamma-octalactone and gamma-nonalactone, in the headspace of Wagyu beef. © 2010 Institute of Food Technologists®

  11. Headspace mass spectrometry methodology: application to oil spill identification in soils

    Energy Technology Data Exchange (ETDEWEB)

    Perez Pavon, J.L.; Garcia Pinto, C.; Moreno Cordero, B. [Universidad de Salamanca, Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Salamanca (Spain); Guerrero Pena, A. [Universidad de Salamanca, Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Salamanca (Spain); Laboratorio de Suelos, Plantas y Aguas, Campus Tabasco, Colegio de Postgraduados, Cardenas, Tabasco (Mexico)

    2008-05-15

    In the present work we report the results obtained with a methodology based on direct coupling of a headspace generator to a mass spectrometer for the identification of different types of petroleum crudes in polluted soils. With no prior treatment, the samples are subjected to the headspace generation process and the volatiles generated are introduced directly into the mass spectrometer, thereby obtaining a fingerprint of volatiles in the sample analysed. The mass spectrum corresponding to the mass/charge ratios (m/z) contains the information related to the composition of the headspace and is used as the analytical signal for the characterization of the samples. The signals obtained for the different samples were treated by chemometric techniques to obtain the desired information. The main advantage of the proposed methodology is that no prior chromatographic separation and no sample manipulation are required. The method is rapid, simple and, in view of the results, highly promising for the implementation of a new approach for oil spill identification in soils. (orig.)

  12. Sorptive potential of sunflower stem for Cr(III) ions from aqueous solutions and its kinetic and thermodynamic profile.

    Science.gov (United States)

    Malik, Ummat Rasul; Hasany, Syed Moosa; Subhani, Muhammad Sadiq

    2005-03-31

    The sorptive potential of sunflower stem (180-300mum) for Cr(III) ions has been investigated in detail. The maximum sorption (>/=85%) of Cr(III) ions (70.2muM) has been accomplished using 30mg of high density sunflower stem in 10min from 0.001M nitric and 0.0001M hydrochloric acid solutions. The accumulation of Cr(III) ions on the sorbent follows Dubinin-Radushkevich (D-R), Freundlich and Langmuir isotherms. The isotherm yields D-R saturation capacity X(m)=1.60+/-0.23mmolg(-1), beta=-0.00654+/-0.00017kJ(2)mol(-2), mean free energy E=8.74+/-0.12kJmol(-1), Freundlich sorption capacity K(F)=0.24+/-0.11molg(-1), 1/n=0.90+/-0.04 and of Langmuir constant K(L)=6800+/-600dm(3)mol(-1) and C(m)=120+/-18micromolg(-1). The variation of sorption with temperature (283-323K) gives DeltaH=-23.3+/-0.8kJmol(-1), DeltaS=-64.0+/-2.7Jmol(-1)K(-1) and DeltaG(298k)=-4.04+/-0.09kJmol(-1). The negative enthalpy and free energy envisage exothermic and spontaneous nature of sorption, respectively. Bisulphate, Fe(III), molybdate, citrate, Fe(II), Y(III) suppress the sorption significantly. The selectivity studies indicate that Cr(III), Eu(III) and Tb(III) ions can be separated from Tc(VII) and I(I). Sunflower stem can be used for the preconcentration and removal of Cr(III) ions from aqueous medium. This cheaper and novel sorbent has potential applications in analytical and environmental chemistry, in water decontamination, industrial waste treatment and in pollution abatement. A possible mechanism of biosorption of Cr(III) ions onto the sunflower stem has been proposed.

  13. Estimate of the soil water retention curve from the sorptivity and β parameter calculated from an upward infiltration experiment

    Science.gov (United States)

    Moret-Fernández, D.; Latorre, B.

    2017-01-01

    The water retention curve (θ(h)), which defines the relationship between the volumetric water content (θ) and the matric potential (h), is of paramount importance to characterize the hydraulic behaviour of soils. Because current methods to estimate θ(h) are, in general, tedious and time consuming, alternative procedures to determine θ(h) are needed. Using an upward infiltration curve, the main objective of this work is to present a method to determine the parameters of the van Genuchten (1980) water retention curve (α and n) from the sorptivity (S) and the β parameter defined in the 1D infiltration equation proposed by Haverkamp et al. (1994). The first specific objective is to present an equation, based on the Haverkamp et al. (1994) analysis, which allows describing an upward infiltration process. Secondary, assuming a known saturated hydraulic conductivity, Ks, calculated on a finite soil column by the Darcy's law, a numerical procedure to calculate S and β by the inverse analysis of an exfiltration curve is presented. Finally, the α and n values are numerically calculated from Ks, S and β. To accomplish the first specific objective, cumulative upward infiltration curves simulated with HYDRUS-1D for sand, loam, silt and clay soils were compared to those calculated with the proposed equation, after applying the corresponding β and S calculated from the theoretical Ks, α and n. The same curves were used to: (i) study the influence of the exfiltration time on S and β estimations, (ii) evaluate the limits of the inverse analysis, and (iii) validate the feasibility of the method to estimate α and n. Next, the θ(h) parameters estimated with the numerical method on experimental soils were compared to those obtained with pressure cells. The results showed that the upward infiltration curve could be correctly described by the modified Haverkamp et al. (1994) equation. While S was only affected by early-time exfiltration data, the β parameter had a

  14. Sorptive behavior of the phenylamide fungicides, mefenoxam and metalaxyl, and their acid metabolite in typical Cameroonian and German soils.

    Science.gov (United States)

    Monkiedje, Adolphe; Spiteller, Michael

    2002-11-01

    Laboratory soil sorption experiments were conducted on mefenoxam, formulated metalaxyl (F-metalaxyl), pure metalaxyl (P-metalaxyl) and metalaxyl acid metabolite to elucidate differences in their sorptive behaviour on typical Cameroonian forest soil (sand clay loam, pH 4.8 and 3.01% OC) and German soil (sandy loam, pH 7.2, 1.69% OC) using a batch equilibrium method. The data obtained on all test chemicals conformed to linear and Freundlich adsorption isotherms. The Langmuir equation failed to describe the sorption of the substances tested. All substances were adsorbed to a greater extent by the Cameroonian soil. The average percentage adsorptions for mefenoxam, F-metalaxyl, P-metalaxyl and the acid metabolite on the Cameroonian soil were 27.8%, 28.3%, 31.8% and 46.8% respectively while for the German soil they were 21.7%, 21.5%, 24.7% and 9.8% respectively. The KD and KF parameters and the Freundlich exponential term (1/n) were low, indicating that the interactions between soil particles and the fungicides were weak. The sorption parameters were lower in the German soil. P-metalaxyl exhibited a higher adsorption capacity than F-metalaxyl in both soils. Mefenoxam and F-metalaxyl exhibited similar sorption parameters in soils, whereas those of P-metalaxyl and acid metabolite differed. Differences observed in the adsorption between the two soils could be attributed to their properties. Desorption studies revealed that the adsorbed fungicides were not firmly retained by soil particles and their adsorption was reversible. Desorption of adsorbed mefenoxam, P-metalaxyl and of the acid metabolite from German soil was almost completely reversible with percentage desorption rates of more than 91.0%, whereas the rate for F-metalaxyl was 74.1%. All compounds exhibited some resistance to desorption from the Cameroonian soil, with percentage desorption rates less than 77.0%. Therefore if degradation in the soil is slow the fungicides described have a potential to leach to lower

  15. Tank 241-B-103 headspace gas and vapor characterization: Results for homogeneity samples collected on October 16, 1996. Tank vapor characterization project

    Energy Technology Data Exchange (ETDEWEB)

    Olsen, K.B.; Pool, K.H.; Evans, J.C. [and others

    1997-06-01

    This report presents the results of analyses of samples taken from the headspace of waste storage tank 241-B-103 (Tank B-103) at the Hanford Site in Washington State. Samples were collected to determine the homogeneity of selected inorganic and organic headspace constituents. Two risers (Riser 2 and Riser 7) were sampled at three different elevations (Bottom, Middle, and Top) within the tank. Tank headspace samples were collected by SGN Eurisys Service Corporation (SESC) and were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL.

  16. Complementary primary mental health programs for young people in Australia: Access to Allied Psychological Services (ATAPS) and headspace.

    Science.gov (United States)

    Bassilios, Bridget; Telford, Nicolas; Rickwood, Debra; Spittal, Matthew J; Pirkis, Jane

    2017-01-01

    Access to Allied Psychological Services (ATAPS) was introduced in 2001 by the Australian Government to provide evidence-based psychological interventions for people with high prevalence disorders. headspace, Australia's National Youth Mental Health Foundation, was established in 2006 to promote and facilitate improvements in the mental health, social wellbeing and economic participation of young people aged 12-25 years. Both programs provided free or low cost psychological services. This paper aims to describe the uptake of psychological services by people aged 12-25 years via ATAPS and headspace, the characteristics of these clients, the types of services received and preliminary client outcomes achieved. Data from 1 July 2009 to 30 June 2012 were sourced from the respective national web-based minimum datasets used for routine data collection in ATAPS and headspace. In total, 20,156 and 17,337 young people accessed two or more psychological services via ATAPS and headspace, respectively, in the 3-year analysis period. There were notable differences between the clients of, and the services delivered by, the programs. ATAPS clients were less likely to be male (31 vs 39%) and to reside in major cities (51 vs 62%) than headspace clients; ATAPS clients were also older (18-21 vs 15-17 years modal age group). There was some variation in the number and types of psychological sessions that young people received via the programs but the majority received at least one session of cognitive behavioural therapy. Based on limited available outcome data, both programs appear to have produced improvements in clients' mental health; specifically, psychological distress as assessed by the Kessler-10 (K-10) was reduced. ATAPS and headspace have delivered free or low-cost psychological services to 12-25 year olds with somewhat different characteristics. Both programs have had promising effects on mental health. ATAPS and headspace have operated in a complementary fashion to fill a

  17. Determination of N-vinyl-2-pyrrolidone and N-methyl-2-pyrrolidone in drugs using polypyrrole-based headspace solid-phase microextraction and gas chromatography-nitrogen-phosphorous detection.

    Science.gov (United States)

    Mehdinia, Ali; Ghassempour, Alireza; Rafati, Hasan; Heydari, Rouhollah

    2007-03-21

    A headspace solid-phase microextraction and gas chromatography-nitrogen-phosphorous detection (HS-SPME-GC-NPD) method using polypyrrole (PPy) fibers has been introduced to determine two derivatives of pyrrolidone; N-vinyl-2-pyrrolidone (NVP) and N-methyl-2-pyrrolidone (NMP). Two types of PPy fibers, prepared using organic and aqueous media, were compared in terms of extraction efficiency and thermal stability. It was found that PPy film prepared using organic medium (i.e. acetonitrile) had higher extraction efficiency and more thermal stability compared to the film prepared in aqueous medium. To enhance the sensitivity of HS-SPME, the effects of pH, ionic strength, extraction time, extraction temperature and the headspace volume on the extraction efficiency were optimized. Using the results of this research, high sensitivity and selectivity had been achieved due to the combination of the high extraction efficiency of PPy film prepared in organic medium and the high sensitivity and selectivity of nitrogen-phosphorous detection. Linear range of the analytes was found to be between 1.0 and 1000 microg L(-1) with regression coefficients (R(2)) of 0.998 and 0.997 for NVP and NMP, consequently. Limits of detection (LODs) were 0.074 and 0.081 microg L(-1) for NVP and NMP, respectively. Relative standard deviation (R.S.D.) for five replications of analyses was found to be less than 6.0%. In real samples the mean recoveries were 94.81% and 94.15% for NVP and NMP, respectively. The results demonstrated the suitability of the HS-SPME technique for analyzing NVP and NMP in two different pharmaceutical matrices. In addition, the method was used for simultaneous detection of NVP, 2-pyrrolidone (2-Pyr), gamma-butyrolactone (GBL) and ethanolamine (EA) compounds.

  18. Determination of N,N-dimethyltryptamine in beverages consumed in religious practices by headspace solid-phase microextraction followed by gas chromatography ion trap mass spectrometry.

    Science.gov (United States)

    Gaujac, Alain; Dempster, Nicola; Navickiene, Sandro; Brandt, Simon D; de Andrade, Jailson Bittencourt

    2013-03-15

    A novel analytical approach combining solid-phase microextraction (SPME)/gas chromatography ion trap mass spectrometry (GC-IT-MS) was developed for the detection and quantification N,N-dimethyltryptamine (DMT), a powerful psychoactive indole alkaloid present in a variety of South American indigenous beverages, such as ayahuasca and vinho da jurema. These particular plant products, often used within a religious context, are increasingly consumed throughout the world following an expansion of religious groups and the availability of plant material over the Internet and high street shops. The method described in the present study included the use of SPME in headspace mode combined GC-IT-MS and included the optimization of the SPME procedure using multivariate techniques. The method was performed with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber in headspace mode (70 min at 60 °C) which resulted in good precision (RSD<8.6%) and accuracy values (71-109%). Detection and quantification limits obtained for DMT were 0.78 and 9.5 mg L(-1), respectively and good linearity (1.56-300 mg L(-1), r(2)=0.9975) was also observed. In addition, the proposed method showed good robustness and allowed for the minimization of sample manipulation. Five jurema beverage samples were prepared in the laboratory in order to study the impact of temperature, pH and ethanol on the ability to extract DMT into solution. The developed method was then applied to the analysis of twelve real ayahuasca and vinho da jurema samples, obtained from Brazilian religious groups, which revealed DMT concentration levels between 0.10 and 1.81 g L(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Effect of destoned olive cake on the aromatic profile of cows’ milk and dairy products: comparison of two techniques for the headspace aroma profile analysis

    Directory of Open Access Journals (Sweden)

    Anna Rocchina Caputo

    2015-03-01

    Full Text Available The aim of this study, carried out within the NOVOROD project (PSR Campania 2007-2013 Misura 124 HC, was to evaluate the aromatic profile of milk and dairy products of dairy cows supplemented with destoned olive cake (DOC. Two techniques for the headspace aroma profile analysis: the thermal desorption by gas chromatography with a mass selective (GC/MS detector and the electronic nose were compared. The trial was performed into a dairy cow farm. Ten dairy cows were allotted into two homogenous groups: control and experimental. Animals received the same diet, while in the experimental group the concentrate supplementation (15% dry matter was replaced with DOC. After two weeks of adaptation, animals were fed with the experimental diet for other 15 days. During the experimental period, the milk was collected and cumulatively processed in Caciotta cheese (a soft cheese, 25 days ripened and in Semicotto cheese (hard cheese, 3 months ripened for 13 times for each group. Milk and cheese volatile organic compounds (VOCs were extracted and concentrated with dynamic headspace method and determined by GC/MS. Statistical analysis of data, expressed in arbitrary units (a.u.=peak area × 10–6 and allotted in compound classes, was carried out by ANOVA. All data collected of VOCs were processed with principal component analysis (PCA. Milk and cheese samples were comparatively analysed with the electronic nose, fitted with a tenmetal oxide sensors electronic device. PCA has been used for the evaluation of the pattern data. Our results show that the use of DOC, as an unconventional feed for livestock, has no effect on the aromatic profile of both milk and dairy products. In fact, no significant differences were found in both milk and dairy products between the two groups using the GC/MS method. Also the discriminating analysis carried out by electronic nose did not show significant differences between the two groups. The two compared techniques seem to lead to

  20. Identification and evaluation of semiochemicals for the biological control of the beetle Omorgus suberosus (F.) (Coleoptera: Trogidae), a facultative predator of eggs of the sea turtle Lepidochelys olivacea (Eschscholtz)

    OpenAIRE

    Cortez, Vieyle; José R. Verdú; Ortiz, Antonio J.; Halffter, Gonzalo

    2017-01-01

    The beetle Omorgus suberosus (F.) is a facultative predator of eggs of the olive ridley turtle Lepidochelys olivacea (Eschscholtz). Laboratory and field investigations were conducted in order to characterize volatile attractants of O. suberosus and to explore the potential for application of these volatiles in a selective mass trapping method. Headspace sorptive extraction (HSSE) coupled to thermo-desorption gas chromatography–mass spectrometry (TD-GC-MS) analysis of the volatile constituents...

  1. CODEX-compliant eleven organophosphorus pesticides screening in multiple commodities using headspace-solid phase microextraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Sang, Zi-Ye; Wang, Yu-Ting; Tsoi, Yeuk-Ki; Leung, Kelvin Sze-Yin

    2013-01-15

    A headspace-solid phase microextraction-gas chromatography-mass spectrometric (HS-SPME-GC-MS, hereafter abbreviated as "SPME") method was developed for dedicated organophosphorus (OP) pesticides assessment in multiple vegetable and fruit commodities. Specific extraction variables were optimised to achieve harmonised extraction performance of eleven OPs in a great span of seven characteristic commodities cataloged in Codex Alimentarius Commission. Comprehensive validation study confirmed analytical robustness of the SPME treatment in turnip, green cabbage, French beans, eggplant, apple, nectarine and grapes. Based on range-specific evaluation, extraction of individual OPs was characterised by sub-ppb level sensitivity and a wide 0.01-2.5 mg L(-1) dynamic range. Effective sample clean-up afforded precise quantification (0.5-10.9% R.S.D.) within a 70-120% recovery range at the MRL levels specified for individual commodities. Compared to conventional methods currently used, the SPME treatment developed here is quick, accurate, and relatively environmental friendly; it represents an attractive, practical way to deliver international standards in OP screening routines.

  2. Graphene oxide based sol-gel stainless steel fiber for the headspace solid-phase microextraction of organophosphate ester flame retardants in water samples.

    Science.gov (United States)

    Jin, Tingting; Cheng, Jing; Cai, Cuicui; Cheng, Min; Wu, Shiju; Zhou, Hongbin

    2016-07-29

    In this paper, graphene oxide was coated onto a stainless steel wire through sol-gel technique and it was used as a solid phase microextraction (SPME) fiber. The prepared fiber was characterized by scanning electron microscopy (SEM), which displayed that the fiber had crinkled surface and porous structure The application of the fiber was evaluated through the headspace SPME of nine organophosphate ester flame retardants (OPFRs) with different characteristics in water samples followed by gas chromatography and nitrogen-phosphorous detector (GC/NPD). The major factors influencing the extraction efficiency, including the extraction and desorption conditions, were studied and optimized. Under the optimum conditions, the proposed method was evaluated, and applied to the analysis of organophosphate ester flame retardants in real environmental water samples. The results demonstrated the HS-SPME method based on GO sol-gel fiber had good linearity (R>0.9928), and limits of detection (1.4-135.6ngL(-1)), high repeatability (RSDsol-gel fiber displayed bigger extraction capability than the commercial PDMS fiber and the pure sol-gel fiber for both polar and apolar organophosphate esters, especially for the OPFRs containing benzene rings.

  3. One-step microwave-assisted headspace solid-phase microextraction for the rapid determination of synthetic polycyclic musks in oyster by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Wu, Shin-Fang; Liu, Li-Lian; Ding, Wang-Hsien

    2012-07-15

    A rapid, simple and solvent-free procedure was developed for the determination of synthetic polycyclic musks in oyster samples by using one-step microwave-assisted headspace solid-phase microextraction (MA-HS-SPME) and gas chromatography-mass spectrometry (GC-MS). Two commonly used synthetic polycyclic musks, galaxolide (HHCB) and tonalide (AHTN), were selected in the method development and validation. The parameters (microwave irradiation power, extraction time, amount of water added, pH value and addition of NaCl) affecting the extraction efficiency of analytes from oyster slurry were systematically investigated and optimised. The best extraction conditions were achieved when the oyster tissue mixed with 10-mL deionised water (containing 3g of NaCl in a 40-mL sample-vial) was microwave irradiated at 80 W for 5 min. The limit of quantification (LOQ) was 0.1 ng/g in 5-g of wet tissue. The good precision and accuracy of one-step MA-HS-SPME coupled with GC-MS for the determination of trace level of AHTN in oyster samples was also demonstrated.

  4. Gas chromatography-mass spectrometry following microwave distillation and headspace solid-phase microextraction for fast analysis of essential oil in dry traditional Chinese medicine.

    Science.gov (United States)

    Li, Ning; Deng, Chunhui; Li, Yan; Ye, Hao; Zhang, Xiangmin

    2006-11-10

    In this paper, a novel method based on gas chromatography-mass spectrometry (GC-MS) following microwave distillation-headspace solid-phase microextraction (MD-HS-SPME) was developed for the determination of essential oil in dry traditional Chinese medicine (TCM). TCM is dried before being preserved and used, there is too little water to absorb microwave energy and heat the TCM samples. In the work, carbonyl iron powders (CIP) was added and mixed with the dried TCM sample, which was used as microwave absorption solid medium for dry distillation of the TCM. At the same time, SPME was used for the extraction and concentration of essential oil after MD. The dry rhizomes of Atractylodes lancea DC was used as the model TCM, and used in the study. The MD-HS-SPME parameters including fiber coating, microwave power, irradiation time, and the amount of added CIP, were studied. To demonstrate the method feasibility, the conventional HS-SPME method was also used for the analysis of essential oil in the TCM. Experimental results show that more compounds were isolated and identified by MD-HS-SPME than those by HS-SPME. Compared to conventional HS-SPME, the advantages of the proposed method are: short extraction time and high extraction efficiency. All experimental results show that the proposed method is an alternative tool for fast analysis of essential oils in dry TCMs.

  5. A review of the extraction and chromatographic determination methods for the analysis of parabens.

    Science.gov (United States)

    Piao, Chunying; Chen, Ligang; Wang, Yu

    2014-10-15

    Parabens are a family of most widely used antimicrobial preservatives in food ingredients, cosmetic consumer products and pharmaceutical preparations. But several recent studies have cautioned that exposure to parabens may have more harmful consequences on animal and human health than what we realized previously, which made the analysis of parabens necessary. In this paper, we reviewed main sample preparation methods and chromatographic analysis methods proposed in formerly published works dealing with the analysis of parabens in different matrices. The sample preparation methods included ultrasonic assisted extraction, supercritical fluid extraction, pressurized liquid extraction, solid phase extraction, solid phase microextraction, liquid phase microextraction, dispersive liquid-liquid microextraction, stir bar sorptive extraction and matrix solid phase dispersion. The chromatographic analysis methods involved liquid chromatography, gas chromatography, and capillary electrophoresis. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Novel polyamide-based nanofibers prepared by electrospinning technique for headspace solid-phase microextraction of phenol and chlorophenols from environmental samples.

    Science.gov (United States)

    Bagheri, Habib; Aghakhani, Ali; Baghernejad, Masoud; Akbarinejad, Alireza

    2012-02-24

    A novel solid phase microextraction (SPME) fiber was fabricated by electrospinning method in which a polymeric solution was converted to nanofibers using high voltages. A thin stainless steel wire was coated by the network of polymeric nanofibers. The polymeric nanofiber coating on the wire was mechanically stable due to the fine and continuous nanofibers formation around the wire with a three dimensional structure. Polyamide (nylon 6), due to its suitable characteristics was used to prepare the unbreakable SPME nanofiber. The scanning electron microscopy (SEM) images of this new coating showed a diameter range of 100-200 nm for polyamide nanofibers with a homogeneous and porous surface structure. The extraction efficiency of new coating was investigated for headspace solid-phase microextraction (HS-SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Effect of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength and polyamide amount were investigated and optimized. In order to improve the chromatographic behavior of phenolic compounds, all the analytes were derivatized prior to the extraction process using basic acetic anhydride. The detection limits of the method under optimized conditions were in the range of 2-10 ng L(-1). The relative standard deviations (RSD) (n=3) at the concentration level of 1.7-6.7 ng mL(-1) were obtained between 1 and 7.4%. The calibration curves of chlorophenols showed linearity in the range of 27-1330 ng L(-1) for phenol and monochlorophenols and 7-1000 ng L(-1) for dichloro and trichlorophenols. Also, the proposed method was successfully applied to the extraction of phenol and chlorophenols from real water samples and relative recoveries were between 84 and 98% for all the selected analytes except for 2,4,6 tricholophenol which was between 72 and 74%. Copyright © 2011

  7. Novel polyamide-based nanofibers prepared by electrospinning technique for headspace solid-phase microextraction of phenol and chlorophenols from environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Bagheri, Habib, E-mail: bagheri@sharif.edu [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of); Aghakhani, Ali; Baghernejad, Masoud; Akbarinejad, Alireza [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)

    2012-02-24

    A novel solid phase microextraction (SPME) fiber was fabricated by electrospinning method in which a polymeric solution was converted to nanofibers using high voltages. A thin stainless steel wire was coated by the network of polymeric nanofibers. The polymeric nanofiber coating on the wire was mechanically stable due to the fine and continuous nanofibers formation around the wire with a three dimensional structure. Polyamide (nylon 6), due to its suitable characteristics was used to prepare the unbreakable SPME nanofiber. The scanning electron microscopy (SEM) images of this new coating showed a diameter range of 100-200 nm for polyamide nanofibers with a homogeneous and porous surface structure. The extraction efficiency of new coating was investigated for headspace solid-phase microextraction (HS-SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Effect of different parameters influencing the extraction efficiency including extraction temperature, extraction time, ionic strength and polyamide amount were investigated and optimized. In order to improve the chromatographic behavior of phenolic compounds, all the analytes were derivatized prior to the extraction process using basic acetic anhydride. The detection limits of the method under optimized conditions were in the range of 2-10 ng L{sup -1}. The relative standard deviations (RSD) (n = 3) at the concentration level of 1.7-6.7 ng mL{sup -1} were obtained between 1 and 7.4%. The calibration curves of chlorophenols showed linearity in the range of 27-1330 ng L{sup -1} for phenol and monochlorophenols and 7-1000 ng L{sup -1} for dichloro and trichlorophenols. Also, the proposed method was successfully applied to the extraction of phenol and chlorophenols from real water samples and relative recoveries were between 84 and 98% for all the selected analytes except for 2,4,6 tricholophenol which was between 72 and 74%.

  8. Removal of copper(II) from some environmental samples by sorptive-flotation using powdered marble wastes as sorbents and oleic acid as surfactant.

    Science.gov (United States)

    Ghazy, S E; Samra, S E; Mahdy, A F M; El-Morsy, S M

    2004-11-01

    A simple and economic experimental sorptive -flotation procedure is presented for the removal of copper(II) species from aqueous solutions. It is based on using powdered marble wastes (PMW), which are widespread and inexpensive and may represent an environmental problem, as the effective inorganic sorbent and oleic (HOL) as the surfactant. The main parameters (i.e. initial solution pH, sorbent, surfactant and copper concentrations, stirring times, ionic strength, temperature and the presence of foreign ions) influencing the flotation of PMW and /or Cu(II) were examined. Nearly, 100% of PMW and Cu(II) were removed from aqueous solutions at pH7 after stirring for 10 min and at room temperature, (approximately 25 degrees C). The procedure was successfully applied to recover Cu(II) spiked to some natural water samples. A mechanism for sorption and flotation is suggested.

  9. Measurement of soil sorptivity rate under different land uses by disc infiltrometer%利用圆盘入渗仪测定不同土地利用类型土壤吸渗率

    Institute of Scientific and Technical Information of China (English)

    佘冬立; 高雪梅; 房凯

    2014-01-01

    探讨利用圆盘入渗仪测定不同利用类型土壤吸渗率的适用性,该文选用盘径分别为10和20 cm的圆盘入渗仪对3种利用土壤(菜地、草地和茶园)在0、-3、-6、-9 cm 4个压力水头下的吸渗过程进行测定。研究以Vandervaere法为参考方法,对Philip法、Haverkamp 三维吸渗法、Haverkamp 三维吸渗改进法的适用性进行比较分析。结果表明:吸渗率的不同计算公式所适应的吸渗过程时间尺度不同,且Haverkamp三维吸渗法所得吸渗率值与参考方法最接近。盘径对吸渗率测定差异的影响不显著。除0 cm压力水头外,不同利用类型土壤吸渗率差异显著,且不同压力水头下测得3种土壤吸渗率大小排序不同。当压力水头为-9和-6 cm时,菜地吸渗率(0.0104和0.0119 cm/s0.5)显著高于茶园(0.0017和0.0025 cm/s0.5)(P<0.05);当压力水头为-3 cm时,茶园吸渗率(0.0370 cm/s0.5)显著高于菜地和草地(0.0147和0.0132 cm/s0.5)(P<0.05)。该研究可为南方丘陵区土壤水力参数的测定提供理论依据。%Soil sorptivity is one of the most important soil hydraulic parameters, representing the capacity of soil to absorb and release the soil solution by capillary force. Quantifying soil sorptivity is essential for describing and modeling hydrological and biological processes, and promoting the theoretical research of the unsaturated soil water movement processes, as well as for the determination of rational irrigation and drainage technology parameters. However, obtaining sufficient and reliable soil sorptivity data is expensive and time consuming. Since the measurement is fast and good for the in-site measurement in fields, the disc infiltration method has been paid more attention gradually. The objective of this study was to assess the feasibility of using a disc infiltrometer to determine soil sorptivity in 3 soils with different land uses (vegetable field, grass land

  10. Determination of residual isobutylene oxide--a genotoxic starting material in a drug substance by static headspace gas chromatography.

    Science.gov (United States)

    Han, Jun; Yeung, David; Wang, Fang; Semin, David

    2008-08-01

    A sensitive static headspace gas chromatography (sHS-GC) method is developed and validated for the determination of residual isobutylene oxide (IBO)-a genotoxic starting material in a drug substance for Phase I clinical trial studies. The experimental parameters, such as headspace vial pressure, headspace oven temperature, vial equilibration time, column flow rate, and GC oven temperature programs are optimized. Under the optimal conditions, the recovery is between 89.3% and 102.4% for spiked samples at three levels of IBO concentration in triplicates in sample preparations. Limits of quantitation (LOQ) and detection (LOD) of the standard solutions are 0.048 and 0.018 microg/mL, respectively. Linear range from 0.018 to 6 microg/mL is obtained with a correlation coefficient of 0.9999. The method is applied to determine residual IBO in drug substance samples from different batches.

  11. Analysis of Cyanide in Blood by Headspace-Isotope-Dilution-GC-MS

    DEFF Research Database (Denmark)

    Løbger, Lise Lotte; Petersen, Henning Willads; Andersen, Jens Enevold Thaulov

    2008-01-01

    An uncomplicated, rapid, automated procedure for the analysis of low cyanide concentrations in whole blood is reported. The analysis was performed by headspace gas chromatography and mass spectrometry in the (1H12C14N) and m/z 29 (1H13C15N). Carryover from cyanide adsorption onto the surface...... of the needle was prevented by developing a new method that enabled automated flushing of the needle in between each cyanide analysis. Results were compared of ordinary calibrations and those of isotope dilutions. The total time of analysis was 18min for a single cyanide analysis....

  12. Optimizing headspace sampling temperature and time for analysis of volatile oxidation products in fish oil

    DEFF Research Database (Denmark)

    Rørbæk, Karen; Jensen, Benny

    1997-01-01

    Headspace-gas chromatography (HS-GC), based on adsorption to Tenax GR(R), thermal desorption and GC, has been used for analysis of volatiles in fish oil. To optimize sam sampling conditions, the effect of heating the fish oil at various temperatures and times was evaluated from anisidine values (......) and HS-CC. AV indicated sample degradations at 90 degrees C but only small alterations between 60 and 75 degrees C. HS-GC showed increasing response with temperature and rime. Purging at 75 degrees C for 45 min was selected as the preferred sampling condition for oxidized fish oil....

  13. Isolation and quantification of volatiles in fish by dynamic headspace sampling and mass spectrometry

    DEFF Research Database (Denmark)

    Refsgaard, Hanne; Haahr, Anne-Mette; Jensen, Benny

    1999-01-01

    determined by use of this sample preparation method and for samples chewed for 10 s. Effects of sampling time, temperature, and purge flow on level of volatiles were tested. Purging at 340 mL/min for 30 min at 45 degrees C was found to be optimal. Detection Emits for a number of aldehydes were 0.2-2.7 mu g......A dynamic headspace sampling method for isolation of volatiles in fish has been developed. The sample preparation involved freezing of fish tissue in liquid nitrogen, pulverizing the tissue, and sampling of volatiles from an aqueous slurry of the fish powder. Similar volatile patterns were...

  14. Analysis of Furaneol in tomato using dynamic headspace sampling with sodium sulfate.

    Science.gov (United States)

    Buttery, R G; Takeoka, G R; Naim, M; Rabinowitch, H; Nam, Y

    2001-09-01

    High-flow dynamic headspace sampling with excess anhydrous sodium sulfate was found to be an effective method of isolating Furaneol from fresh tomatoes. Quantitative analysis was carried out by gas chromatography using maltol as internal standard. Furaneol was found in the highest concentrations (660-1100 ppb) in the summer crop of home-grown tomatoes and in some of the greenhouse hydroponically grown tomatoes, which are ripened on the plant before being transported to the supermarkets. Furaneol was found in the lowest concentrations (38-180 ppb) in the common ethylene-ripened, field-grown, supermarket tomatoes.

  15. Specific determination of benzene in urine using dynamic headspace and mass-selective detection.

    Science.gov (United States)

    Ljungkvist, G; Lärstad, M; Mathiasson, L

    1999-01-08

    A method for the determination of benzene in urine was developed, based on dynamic headspace and preconcentration of the analyte on a solid sorbent. The subsequent analysis by thermal desorption of the sorbent, capillary gas chromatography and mass-selective detection ascertained a low limit of detection (6.5 ng/l) and a highly specific determination. The limit of detection is an order of magnitude lower than that reported earlier and allows reliable quantitation of occupational exposure and of most environmental exposures. Samples could be stored frozen for at least a month without significant loss.

  16. Polytetrafluoroethylene-jacketed stirrer modified with graphene oxide and polydopamine for the efficient extraction of polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Zhang, Zinxin; Mwadini, Mwadini Ahmada; Chen, Zilin

    2016-10-01

    Steel stirrers jacketed with polytetrafluoroethylene can be regarded as an ideal substrate for stirrer bar sorptive extraction. However, it is still a great challenge to immobilize graphene onto a polytetrafluoroethylene stirrer due to the high chemical resistance of the surface of a polytetrafluoroethylene stirrer. We describe here a method to modify the surface of polytetrafluoroethylene stirrers with graphene. In this work, graphene was used as the sorbent due to its excellent adsorption capability for aromatic compounds, such as polycyclic aromatic compounds. Graphene was successfully immobilized onto polytetrafluoroethylene-stirrer by a bio-inspired polydopamine functionalization method. The graphene-modified polytetrafluoroethylene-stirrer shows good stability and tolerance to stirring, ultrasonication, strong acidic and basic solutions, and to organic solvents. The multilayer coating was characterized by scanning electronic microscopy and Fourier transform infrared spectroscopy. After the optimization of some experimental conditions, the graphene-modified polytetrafluoroethylene stirrer was used for the stirrer bar sorptive extraction of polycyclic aromatic hydrocarbons, in which the binding between the polycyclic aromatic hydrocarbons and the graphene layer was mainly based on π-π stacking and hydrophobic interactions. The graphene-modified polytetrafluoroethylene-stirrer-based stirrer bar sorptive extraction and high-performance liquid chromatography method was developed for the determination of polycyclic aromatic hydrocarbons with great extraction efficiency, with enrichment factors from 18 to 62. The method has low limits of detection of 1-5 pg/mL, wide linear range (5-100 and 10-200 pg/mL), good linearity (R ≥ 0.9957) and good reproducibility (RSD ≤ 6.45%). The proposed method has been applied to determine polycyclic aromatic hydrocarbons in real dust samples. Good recoveries were obtained, ranging from 88.53 to 109.43%.

  17. Uncertainty of Blood Alcohol Concentration (BAC Results as Related to Instrumental Conditions: Optimization and Robustness of BAC Analysis Headspace Parameters

    Directory of Open Access Journals (Sweden)

    Haleigh A. Boswell

    2015-12-01

    Full Text Available Analysis of blood alcohol concentration is a routine analysis performed in many forensic laboratories. This analysis commonly utilizes static headspace sampling, followed by gas chromatography combined with flame ionization detection (GC-FID. Studies have shown several “optimal” methods for instrumental operating conditions, which are intended to yield accurate and precise data. Given that different instruments, sampling methods, application specific columns and parameters are often utilized, it is much less common to find information on the robustness of these reported conditions. A major problem can arise when these “optimal” conditions may not also be robust, thus producing data with higher than desired uncertainty or potentially inaccurate results. The goal of this research was to incorporate the principles of quality by design (QBD in the adjustment and determination of BAC (blood alcohol concentration instrumental headspace parameters, thereby ensuring that minor instrumental variations, which occur as a matter of normal work, do not appreciably affect the final results of this analysis. This study discusses both the QBD principles as well as the results of the experiments, which allow for determination of more favorable instrumental headspace conditions. Additionally, method detection limits will also be reported in order to determine a reporting threshold and the degree of uncertainty at the common threshold value of 0.08 g/dL. Furthermore, the comparison of two internal standards, n-propanol and t-butanol, will be investigated. The study showed that an altered parameter of 85 °C headspace oven temperature and 15 psi headspace vial pressurization produces the lowest percent relative standard deviation of 1.3% when t-butanol is implemented as an internal standard, at least for one very common platform. The study also showed that an altered parameter of 100 °C headspace oven temperature and 15-psi headspace vial pressurization

  18. Análise de pesticidas organoclorados em água usando a microextração em fase sólida por headspace com cromatografia gasosa e espectrometria de massas

    Directory of Open Access Journals (Sweden)

    Crislaine Batista Prates

    2011-01-01

    Full Text Available A method based on headspace - solid phase microextraction coupled with gas chromatography - mass spectrometry was validated for the quantitative determination of 18 organochlorine pesticides in water. For the extraction conditioning some parameters as the best type of coating fiber, time and temperature of extraction, pH and ionic strength were evaluated. The method HS-SPME/GC-MS/MS showed linear coefficient above 0.9948. The repeatability of the measurements were lower than 7.6%. Relative recoveries were between 88 and 110%. Limits of detection from 0.5 x 10-3 to 1.0 mg L-1 were obtained. A total of 31 samples were analyzed and 16 presented from 1 to 5 pesticides.

  19. The comparison of solid phase microextraction-GC and static headspace-GC for determination of solvent residues in vegetable oils.

    Science.gov (United States)

    Ligor, Magdalena; Buszewski, Bogusław

    2008-02-01

    The objective of these investigations has been the determination of volatile organic compounds including residue solvents present in vegetable oil samples. Some olive oil, rape oil, sunflower oil, soy-bean oil, pumpkin oil, grape oil, rice oil as well as hazel-nut oil samples were analysed. Among residue solvents the following compounds have been mentioned: acetone, n-hexane, benzene, and toluene. Some experiments for the solid phase microextraction (SPME)-GC-flame ionisation detection (FID) were performed to examine extraction conditions such as fiber exposure time, temperature of extraction, and temperature of desorption. Various SPME fibers such as polydimethylsiloxane, Carboxen/polydimethylsiloxane and polydimethylsiloxane/divinylbenzene coatings were used for the isolation of tested compounds from vegetable oil samples. After optimisation of SPME, real vegetable oil samples were examined using SPME-GC/MS. Based on preliminary experiments the qualitative and quantitative analyses for the determination of acetone, n-hexane, benzene and toluene were performed by SPME-GC-FID and static head-space (SHS)-GC-FID methods. The regression coefficients for calibration curves for the examined compounds were R(2) > or = 0.992. This shows that the used method is linear in the examined concentration range (0.005-0.119 mg/kg for SPME-GC-FID and 0.003-0.728 mg/kg for SHS-GC-FID). Chemical properties of analysed vegetable oils have been characterised by chemometric procedure (cluster analysis).

  20. Determination of biogenic amines in canned fish samples using head-space solid phase microextraction based on nanostructured polypyrrole fiber coupled to modified ionization region ion mobility spectrometry.

    Science.gov (United States)

    Parchami, Razieh; Kamalabadi, Mahdie; Alizadeh, Naader

    2017-01-20

    The head-space solid phase microextraction (HS-SPME) was applied to extraction and determination of histamine (HIS), putrescine (PUT), cadaverine (CAD), tyramine (TYR) in canned fish samples by ion mobility spectrometry (IMS) without any derivatization process. HIS and CAD have the same mobilities in nitrogen as buffer gas and their corresponding peaks are severely overlapped in ion mobility spectrum. Peak separation was acquired in the presence of 18-crown-6 vapor as complexation reagent into carrier gas and modified ionization region of IMS (MIR-IMS) at optimum flow rate. The interaction between 18-crown-6 and the mentioned amines forms nanocluster product ions with different cross section areas and ion mobilities. The effects of main extraction parameters on the efficiency of HS-SPME-MIR-IMS were investigated and optimized. Relative standard deviations (RSD%) of the biogenic amines determination at 50μgL(-1) concentration level were obtained in range 5.7%-6.3%. Limits of detection for analytes were in the range of 0.6-1ngg(-1). HS-SPME-MIR-IMS results indicate that the proposed method can be successfully used in biogenic amines analysis in water and food samples. Method validation was conducted by comparing our results with those obtained through GC-MS method.

  1. A powerful methodological approach combining headspace solid phase microextraction, mass spectrometry and multivariate analysis for profiling the volatile metabolomic pattern of beer starting raw materials.

    Science.gov (United States)

    Gonçalves, João L; Figueira, José A; Rodrigues, Fátima P; Ornelas, Laura P; Branco, Ricardo N; Silva, Catarina L; Câmara, José S

    2014-10-01

    The volatile metabolomic patterns from different raw materials commonly used in beer production, namely barley, corn and hop-derived products - such as hop pellets, hop essential oil from Saaz variety and tetra-hydro isomerized hop extract (tetra hop), were established using a suitable analytical procedure based on dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography-quadrupole mass spectrometry detection (GC-qMS). Some SPME extraction parameters were optimized. The best results, in terms of maximum signal recorded and number of isolated metabolites, were obtained with a 50/30 μm DVB/CAR/PDMS coating fiber at 40 °C for 30 min. A set of 152 volatile metabolites comprising ketones (27), sesquiterpenes (26), monoterpenes (19), aliphatic esters (19), higher alcohols (15), aldehydes (11), furan compounds (11), aliphatic fatty acids (9), aliphatic hydrocarbons (8), sulphur compounds (5) and nitrogen compounds (2) were positively identified. Each raw material showed a specific volatile metabolomic profile. Monoterpenes in hop essential oil and corn, sesquiterpenes in hop pellets, ketones in tetra hop and aldehydes and sulphur compounds in barley were the predominant chemical families in the targeted beer raw materials. β-Myrcene was the most dominant volatile metabolite in hop essential oil, hop pellets and corn samples while, in barley, the predominant volatile metabolites were dimethyl sulphide and 3-methylbutanal and, in tetra hop, 6-methyl-2-pentanone and 4-methyl-2-pentanone. Principal component analysis (PCA) showed natural sample grouping among beer raw materials.

  2. Rapid analysis of Fructus forsythiae essential oil by ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction followed by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Jiao, Jiao; Ma, Dan-Hui; Gai, Qing-Yan; Wang, Wei; Luo, Meng; Fu, Yu-Jie; Ma, Wei

    2013-12-04

    A rapid, green and effective miniaturized sample preparation and analytical technique, i.e. ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction (ILAMD-HS-SDME) followed by gas chromatography-mass spectrometry (GC-MS) was developed for the analysis of essential oil (EO) in Fructus forsythiae. In this work, ionic liquids (ILs) were not only used as the absorption medium of microwave irradiation but also as the destruction agent of plant cell walls. 1-Ethyl-3-methylimidazolium acetate ([C2mim]OAc) was chosen as the optimal ILs. Moreover, n-heptadecane (2.0 μL) was selected as the appropriate suspended solvent for the extraction and concentration of EO. Extraction conditions of the proposed method were optimized using the relative peak area of EO constituents as the index, and the optimal operational parameters were obtained as follows: irradiation power (300 W), sample mass (0.7 g), mass ratio of ILs to sample (2.4), temperature (78°C) and time (3.4 min). In comparison to previous reports, the proposed method was faster and required smaller sample amount but could equally monitor all EO constituents with no significant differences.

  3. Polydopamine-based immobilization of a hydrazone covalent organic framework for headspace solid-phase microextraction of pyrethroids in vegetables and fruits.

    Science.gov (United States)

    Wu, Mingxue; Chen, Gang; Liu, Ping; Zhou, Weihong; Jia, Qiong

    2016-07-22

    We designed a novel hydrazone covalent organic framework (COF) and developed a polydopamine (PDA) method to immobilize COF on a stainless steel fiber for headspace solid-phase microextraction (HS-SPME). A series of characterization studies was performed to validate the structure and property of the prepared fiber. The COF-PDA fiber was applied for the extraction of pyrethroids coupled with gas chromatography equipped with an electron capture detector (GC-ECD). Under the optimum experimental conditions, high enhancement factors of 307-2327 were achieved, indicating that the hydrazone COF possessed good extraction efficiency for pyrethroids. The detection limits ranged from 0.11 to 0.23μgkg(-1) with relative standard deviations varying in the range of 3.6-9.2% (intra-batch) and 6.9-12.1% (inter-batch), respectively. The developed method was applied to the determination of pyrethroids in fruit and vegetable samples and the accuracy was assessed through recovery experiments. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Determination of furfural and hydroxymethylfurfural from baby formula using headspace solid phase microextraction based on nanostructured polypyrrole fiber coupled with ion mobility spectrometry.

    Science.gov (United States)

    Kamalabadi, Mahdie; Ghaemi, Elham; Mohammadi, Abdorreza; Alizadeh, Naader

    2015-08-15

    Furfural (Fu) and hydroxymethylfurfural (HMFu) are extracted using a dodecylbenzenesulfonate-doped polypyrrole coating as a fiber for headspace solid phase microextraction (HS-SPME) method in baby formula samples and detected using ion mobility spectrometry (IMS). Sample pH, salt effect, extraction time and temperature were investigated and optimized as effective parameters in HS-SPME. The calibration curves were linear in the range of 20-300 ng g(-1) (R(2)>0.99). Limits of detection for Fu and HMFu were 6 ng g(-1) and 5 ng g(-1), respectively. The RSD% of Fu and HMFu for five analyses was 4.4 and 4.9, respectively. The proposed method was successfully applied to determine of Fu and HMFu in the different baby formula samples with satisfactory result. The results were in agreement with those obtained using HPLC analysis. The HS-SPME-IMS is precise, selective and sensitive analytical method for determination of Fu and HMFu in baby formula samples, without any derivatization process.

  5. headspace: National Youth Mental Health Foundation: making headway with rural young people and their mental health.

    Science.gov (United States)

    Hodges, Craig A; O'Brien, Matthew S; McGorry, Patrick D

    2007-04-01

    Mental health is the number one health issue affecting young people in Australia today, yet only one in four of these young people receive professional help. Approximately 14% of 12- to 17-year-olds and 27% of 18- to 25-year-olds experience mental health problems each year. However, many do not have ready access to treatment or are reluctant to seek that help. These issues might be exacerbated in the rural and remote regions of Australia where sociocultural barriers such as stigma, lack of anonymity and logistic difficulties including cost and availability of transport can hinder young people accessing mental health services. headspace: the National Youth Mental Health Foundation has been funded to address these issues. headspace will provide funding for the establishment of communities of youth services across Australia, provide national and local community awareness campaigns and plans, establish a centre of excellence that will identify and disseminate evidence-based practice in addressing youth mental health issues, and translate findings into education and training programs that are targeted at service providers to work with youth mental health. The communities of youth services will build the capacity of local communities to identify early, and provide effective responses to, young people aged 12-25 years with mental health and related substance use disorders. Specific approaches in rural, regional and remote areas will be developed as well as specific programs to involve young Indigenous people.

  6. Grains colonised by moulds: fungal identification and headspace analysis of produced volatile metabolites

    Directory of Open Access Journals (Sweden)

    Maria Paola Tampieri

    2010-01-01

    Full Text Available The aim of this work was to verify if the headspace analysis of fungal volatile compounds produced by some species of Fusarium can be used as a marker of mould presence on maize. Eight samples of maize (four yellow maize from North Italy and four white maize from Hungary, naturally contaminated by Fusarium and positive for the presence of fumonisins, were analyzed to detect moisture content, Aw, volatile metabolites and an enumeration of viable moulds was performed by means of a colony count technique. Headspace samples were analysed using a gas-chromatograph equipped with a capillary column TR-WAX to detect volatile metabolites of moulds. Furthermore macro and microscopic examination of the colonies was performed in order to distinguish, according to their morphology, the genera of the prevalent present moulds. Prevalent mould of eight samples was Fusarium, but other fungi, like Aspergillus, Penicillum and Mucoraceae, were observed. The metabolites produced by F.graminearum and F. moniliforme were Isobutyl-acetate, 3-Methyl-1-butanol and, only at 8 days, 3-Octanone. The incubation time can affect off flavour production in consequence of the presence of other moulds. Further studies on maize samples under different conditions are needed in order to establish the presence of moulds using the count technique and through the identification of volatile compounds.

  7. Determination of dissolved methane in natural waters using headspace analysis with cavity ring-down spectroscopy.

    Science.gov (United States)

    Roberts, Hannah M; Shiller, Alan M

    2015-01-26

    Methane (CH4) is the third most abundant greenhouse gas (GHG) but is vastly understudied in comparison to carbon dioxide. Sources and sinks to the atmosphere vary considerably in estimation, including sources such as fresh and marine water systems. A new method to determine dissolved methane concentrations in discrete water samples has been evaluated. By analyzing an equilibrated headspace using laser cavity ring-down spectroscopy (CRDS), low nanomolar dissolved methane concentrations can be determined with high reproducibility (i.e., 0.13 nM detection limit and typical 4% RSD). While CRDS instruments cost roughly twice that of gas chromatographs (GC) usually used for methane determination, the process presented herein is substantially simpler, faster, and requires fewer materials than GC methods. Typically, 70-mL water samples are equilibrated with an equivalent amount of zero air in plastic syringes. The equilibrated headspace is transferred to a clean, dry syringe and then drawn into a Picarro G2301 CRDS analyzer via the instrument's pump. We demonstrate that this instrument holds a linear calibration into the sub-ppmv methane concentration range and holds a stable calibration for at least two years. Application of the method to shipboard dissolved methane determination in the northern Gulf of Mexico as well as river water is shown. Concentrations spanning nearly six orders of magnitude have been determined with this method.

  8. River water quality analysis via headspace detection of volatile organic compounds

    Science.gov (United States)

    Tang, Johnny Jock Lee; Nishi, Phyllis Jacqueline; Chong, Gabriel Eng Wee; Wong, Martin Gideon; Chua, Hong Siang; Persaud, Krishna; Ng, Sing Muk

    2017-03-01

    Human civilization has intensified the interaction between the community and the environment. This increases the threat on the environm ent for being over exploited and contaminated with m anmade products and synthetic chemicals. Of all, clean water is one of the resources that can be easily contaminated since it is a universal solvent and of high mobility. This work reports the development and optimization of a water quality monitoring system based on metal oxide sensors. The system is intended to a ssist the detection of volatile organic compounds (VOCs) present in water sources online and onsite. The sampling mechanism was based on contactless mode, where headspace partial pressure of the VOCs formed above the water body in a close chamber was drawn for detection at the sensor platform. Pure toluene was used as standard to represent the broad spectrum of VOCs, and the sensor dynamic range was achieved from 1-1000 ppb. Several sensing parameters such as sampling time, headspace volume, and sensor recovery were s tudied and optimized. Besides direct detection of VOC contaminants in the water, the work has also been extended to detect VOCs produced by microbial communities and to c orrelate the size of the communities with the reading of V OCs recorded. This can serve to give b etter indication of water quality, not only on the conce ntration of VOCs c ontamination from chemicals, but also the content of microbes, which some can have severe effect on human health.

  9. Brain and Liver Headspace Aldehyde Concentration Following Dietary Supplementation with n-3 Polyunsaturated Fatty Acids.

    Science.gov (United States)

    Ross, Brian M; Babay, Slim; Malik, Imran

    2015-11-01

    Reactive oxygen species react with unsaturated fatty acids to form a variety of metabolites including aldehydes. Many aldehydes are volatile enough to be detected in headspace gases of blood or cultured cells and in exhaled breath, in particular propanal and hexanal which are derived from omega-3 and omega-6 polyunsaturated fatty acids, respectively. Aldehydes are therefore potential non-invasive biomarkers of oxidative stress and of various diseases in which oxidative stress is thought to play a role including cancer, cardiovascular disease and diabetes. It is unclear, however, how changes in the abundance of the fatty acid precursors, for example by altered dietary intake, affect aldehyde concentrations. We therefore fed male Wistar rats diets supplemented with either palm oil or a combination of palm oil plus an n-3 fatty acid (alpha-linolenic, eicosapentaenoic, or docosahexaenoic acids) for 4 weeks. Fatty acid analysis revealed large changes in the abundance of both n-3 and n-6 fatty acids in the liver with smaller changes observed in the brain. Despite the altered fatty acid abundance, headspace concentrations of C1-C8 aldehydes, and tissue concentrations of thiobarbituric acid reactive substances, did not differ between the 4 dietary groups. Our data suggest that tissue aldehyde concentrations are independent of fatty acid abundance, and further support their use as volatile biomarkers of oxidative stress.

  10. Quantitative analysis of total starch content in wheat flour by reaction headspace gas chromatography.

    Science.gov (United States)

    Xie, Wei-Qi; Gong, Yi-Xian; Yu, Kong-Xian

    2017-07-10

    This paper proposed a new reaction headspace gas chromatographic (HS-GC) method for efficiently quantifying the total starch content in wheat flours. A certain weight of wheat flour was oxidized by potassium dichromate in an acidic condition in a sealed headspace vial. The results show that the starch in wheat flour can be completely transferred to carbon dioxide at the given conditions (at 100 °C for 40 min) and the total starch content in wheat flour sample can be indirectly quantified by detecting the CO2 formed from the oxidation reaction. The data showed that the relative standard deviation of the reaction HS-GC method in the precision test was less than 3.06%, and the relative differences between the new method and the reference method (titration method) were no more than 8.90%. The new reaction HS-GC method is automated, accurate, and can be a reliable tool for determining the total starch content in wheat flours in both laboratory and industrial applications. Graphical abstract The total starch content in wheat flour can be indirectly quantified by the GC detection of the CO2 formed from the oxidation reaction between wheat flour and potassium dichromate in an acidic condition.

  11. Calibration of an optical condensate measurement technique using indirect static headspace gas chromatography.

    Science.gov (United States)

    Hoke, P B; Loconto, P R; McGrath, J J

    2001-12-01

    Researchers in the Department of Mechanical Engineering seek to obtain a means to measure less than 3 mg of H2O that adheres to a metal surface as condensate. The objective is to calibrate optical reflectance measurements of an aluminum surface as a function of the condensate thickness present. Collaboration with the Hazardous Substance Research Center at Michigan State University results in the development of an indirect static headspace gas chromatographic technique capable of measuring H2O in low-milligram quantities. The technique utilizes manual headspace sampling, a megabore capillary column, and a flame ionization detector. A correlation of r2 = 0.999 is obtained for the calibration of the indirect measurement technique. The calibration of the analytical instrument demonstrates adequate precision (calcium carbide to convert the H2O to acetylene. A scaled calibration technique is used to simplify handling trace water volumes. The surface reflectance measurements are found to correlate well (r2 = 0.935) with measurements of the condensate mass. This result facilitates the development of an optical mass-transfer measurement technique. This study focuses on the analytical method and its relationship with engineering research.

  12. Sensitive determination of polychlorinated biphenyls in environmental water samples by headspace solid-phase microextraction with bamboo charcoal@iron oxide black fibers prior to gas chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Liu, Yan-Long; Chen, Xiang-Feng; Wang, Xia; Zhou, Jia-Bin; Zhao, Ru-Song

    2014-06-01

    We have investigated the feasibility of bamboo charcoal@iron oxide black for the headspace solid-phase microextraction of polychlorinated biphenyls in environmental water samples. Bamboo charcoal@iron oxide black was prepared and used as a solid-phase microextraction coating material, and gas chromatography with tandem mass spectrometry was used for detection. Several important factors affecting the extraction efficiency were systematically investigated and optimized. Under the optimum conditions, the experimental data exhibited wide linear range over the range 0.2-1000 ng/L and low limits of detection in the range of 4.7-22.2 pg/L. The novel coating was successfully used for the enrichment and determination of polychlorinated biphenyls in real environmental water samples. All these results indicated that bamboo charcoal@iron oxide black-based headspace solid-phase microextraction coupled to gas chromatography with tandem mass spectrometry was an excellent alternative for the sensitive analysis of polychlorinated biphenyls at ultratrace levels in the environment.

  13. Tank 241-C-111 headspace gas and vapor characterization results for samples collected in August 1993 and September 1994

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, J.L. [Pacific Northwest Lab., Richland, WA (United States); Bratzel, D.R. [Westinghouse Hanford Co., Richland, WA (United States)

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories.

  14. Bromination of Aromatic Compounds by Residual Bromide in Sodium Chloride Matrix Modifier Salt During Heated Headspace GC/MS Analysis

    Science.gov (United States)

    Analytical artifacts attributed to the bromination of toluene, xylenes, and trimethylbenzenes were found during the heated headspace gas chromatography/mass spectrometry (GC/MS) analysis of aqueous samples. The aqueous samples were produced from Fenton-like chemical oxidation rea...

  15. Comparison of tomatillo and tomato volatile compounds in the headspace by selected ion flow tube mass spectrometry (SIFT-MS).

    Science.gov (United States)

    Xu, Yichi; Barringer, Sheryl

    2010-04-01

    The concentration of 31 volatiles were measured in the headspace of tomatillos using selected ion flow tube-mass spectrometry (SIFT-MS), and were compared with those in vine-ripened tomato, roma tomato, cherry tomato, and grape tomato. None of the volatiles were higher in the headspace of tomatillos than of tomatoes. Compounds (E)-2-octenal, (E)-2-pentenal, 2-isobutylthiazole, 6-methyl-5-hepten-2-one, and phenylacetaldehyde were significantly lower in tomatillo than in the tomato varieties in the headspace. After blending, volatiles in the headspace increased, and then decreased after reaching a maximum concentration, due to further degradation or depletion. Compounds (E)-2-pentenal and 1-penten-3-one reached a maximum concentration later than (E)-2-hexenal, (Z)-3-hexenal, and hexanal for tomatillo and tomatoes. The slope of the ratio of (E)-2-hexenal and (Z)-3-hexenal was not significantly different for any of the samples, implying that the activity of cis/trans isomerase was not different between tomatillos and tomatoes.

  16. Tank 241-BY-107 headspace gas and vapor characterization results for samples collected in March 1994 and October 1994

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, J.L. [Pacific Northwest Lab., Richland, WA (United States); Bratzel, D.R. [Westinghouse Hanford Co., Richland, WA (United States)

    1995-09-01

    Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories.

  17. Application of head-space solid-phase microextraction for the analysis of volatile metabolites emitted by Penicillium species

    DEFF Research Database (Denmark)

    Nilsson, Torben; Larsen, Thomas Ostenfeld; Montanarella, Luca

    1996-01-01

    Head-space solid-phase microextraction (HS-SPME) has been used to collect volatile organic compounds (VOCs) emitted from fungi of the genus Penicillium. Gas chromatography combined with mass spectrometry (GC-MS) was employed for the analysis of the profiles of volatile metabolites characteristic ...

  18. Dynamic headspace-gas-chromatography-olfactometry analysis of different anatomical parts of lovage (Levisticum officinale Koch.) at eight growing stages

    NARCIS (Netherlands)

    Bylaite, E.; Roozen, J.P.; Legger, A.; Venskutonis, R.P.; Posthumus, M.A.

    2000-01-01

    Volatiles of five different parts of lovage (leaves, stems, flowers, seeds, and roots) were isolated by dynamic headspace (DHS) method and analyzed by GC-FID and GC-olfactometry (GC-O) techniques. In total, 98 compounds were identified in the samples, of which 41 are reported as lovage volatiles for

  19. Headspace-free setup of in vitro bioassays for the evaluation of volatile disinfection by-products.

    Science.gov (United States)

    Stalter, Daniel; Dutt, Mriga; Escher, Beate I

    2013-11-18

    The conventional setup of in vitro bioassays in microplates does not prevent the loss of volatile compounds, which hampers the toxicological characterization of waterborne volatile disinfection by-products (DBPs). To minimize the loss of volatile test chemicals, we adapted four in vitro bioassays to a headspace-free setup using eight volatile organic compounds (four trihalomethanes, 1,1-dichloroethene, bromoethane, and two haloacetonitriles) that cover a wide range of air-water partition coefficients. The nominal effect concentrations of the test chemicals decreased by up to three orders of magnitude when the conventional setup was changed to a headspace-free setup for the bacterial cytotoxicity assay using bioluminescence inhibition of Vibrio fischeri. The increase of apparent sensitivity correlated significantly with the air-water partition coefficient. Purge and trap GC/MS analysis revealed a reduced loss of dosed volatile compounds in the headspace free setup (78-130% of nominal concentration) compared to a substantial loss in the conventional set up (2-13% of the nominal concentration). The experimental effect concentrations converged with the headspace-free setup to the effect concentrations predicted by a QSAR model, confirming the suitability of the headspace-free approach to minimize the loss of volatile test chemicals. The analogue headspace-free design of the bacterial bioassays for genotoxicity (umuC assay) and mutagenicity (Ames fluctuation assay) increased the number of compounds detected as genotoxic or mutagenic from one to four and zero to two, respectively. In a bioassay with a mammalian cell line applied for detecting the induction of the Nrf-2-mediated oxidative stress response (AREc32 assay), the headspace-free setup improved the apparent sensitivity by less than one order of magnitude, presumably due to the retaining effect of the serum components in the medium, which is also reflected in the reduced aqueous concentrations of compounds. This

  20. 静态顶空-气相色谱质谱选择性测定烟用白乳胶中7种苯系物%Selective determination of seven benzene series components in cigarette adhesives by static headspace gas chromatograph-mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    姬厚伟; 刘剑; 叶冲; 万强; 韩伟; 王芳; 杨虹杰; 杨敬国

    2012-01-01

    为选择性测定烟用白乳胶中7种苯系物,建立了静态顶空-气相色谱质谱选择离子定量的测定方法.样品经140℃、30 min静态顶空后,以2-己酮为内标,采用HP-INNOWAX柱,气相色谱-质谱选择离子模式检测,内标法定量.该方法对7种苯系物的定量检测限为0.008 ~0.01 mg/kg,加标回收率为88.9%-104.5%,RSD <5%,效果良好.%A method based on static headspace gas chromatography-mass spectrometry ( SHS-GC/MS) and internal standard was developed to selectively determine seven benzene series components contents in cigarette adhesive. Experimental conditions such as headspace temperature, headspace time and analytical conditions of GC-MS were optimized. Cigarette adhesive samples were treated at 140℃ for 30 min. Head-space vapor of final extraction was injected into a HP-INNOWAX column and detected by MS. The target compounds were quantified by internal standard method under selected ion monitoring mode. Results showed that; the recoveries ranged from 88.9% to 104.5% , with relative standard deviations ( RSDs) e less than 5%. The linear range was from 0.01 to 0.5 μg/mL with a good, linear determination coefficient (R2 >0.999) and limits of quantification were 0.008 ~0.0lmg/kg. The method is accurate, simple and rapid.

  1. Simultaneous distillation-extraction of high-value volatile compounds from Cistus ladanifer L.

    Science.gov (United States)

    Teixeira, Salomé; Mendes, Adélio; Alves, Arminda; Santos, Lúcia

    2007-02-19

    The present paper describes a procedure to isolate volatiles from rock-rose (Cistus ladanifer L.) using simultaneous distillation-extraction (SDE). High-value volatile compounds (HVVC) were selected and the influence of the extraction conditions investigated. The effect of the solvent nature and extraction time on SDE efficiency was studied. The best performance was achieved with pentane in 1 h operation. The extraction efficiencies ranged from 65% to 85% and the repeatability varied between 4% and 6% (as a CV%). The C. ladanifer SDE extracts were analysed by headspace solid phase microextraction (HS-SPME) followed by gas chromatography with flame ionization detection (GC-FID). The HS-SPME sampling conditions such as fiber coating, temperature, ionic strength and exposure time were optimized. The best results were achieved with an 85 microm polyacrylate fiber for a 60 min headspace extraction at 40 degrees C with 20% (w/v) of NaCl. For optimized conditions the recovery was in average higher than 90% for all compounds and the intermediate precision ranged from 4 to 9% (as CV %). The volatiles alpha-pinene (22.2 mg g(-1) of extract), 2,2,6-trimethylcyclohexanone (6.1 mg g(-1) of extract), borneol (3.0 mg g(-1) of extract) and bornyl acetate (3.9 mg g(-1) of extract) were identified in the SDE extracts obtained from the fresh plant material.

  2. Characterization of the most odor-active compounds of Iberian ham headspace.

    Science.gov (United States)

    Carrapiso, Ana I; Ventanas, Jesús; García, Carmen

    2002-03-27

    Gas chromatography-olfactometry (GC-O) based on detection frequency (DF) was used to characterize the most odor-active compounds from the headspace of Iberian ham. Twenty-eight odorants were identified by GC-O on two capillary columns, including aldehydes (11), sulfur-containing compounds (7), ketones (5), nitrogen-containing compounds (2), esters (2), and an alcohol. Among them, the highest odor potencies (DF values) were found for 2-methyl-3-furanthiol, 2-heptanone, 3-methylbutanal, methanethiol, hexanal, hydrogen sulfide, 1-penten-3-one, 2-methylpropanal, ethyl 2-methylbutyrate, and (E)-2-hexenal. Nine of the 28 most odor-active compounds were identified for the first time as aroma components of dry-cured ham, including hydrogen sulfide, 1-penten-3-one, (Z)-3-hexenal, 1-octen-3-one, and the meaty-smelling compounds 2-methyl-3-furanthiol, 2-furfurylthiol, 3-mercapto-2-pentanone, 2-acetyl-1-pyrroline, and 2-propionyl-1-pyrroline.

  3. Characterization of volatiles from cultured dairy spreads during storage by dynamic headspace GC/MS

    DEFF Research Database (Denmark)

    Lund, Pia; Hølmer, Gunhild Kofoed

    2001-01-01

    The effect of storage time and storage temperature on the formation of volatile compounds in dairy spreads was investigated. Dairy spreads were stored for 10 weeks at -18, 5 and 20 degreesC, respectively, and analyzed after 0, 38, 54 and 67 days of storage. By means of a dynamic headspace GC....../MS method using Tenax traps the dairy spreads were analyzed for volatile aromatic compounds. 61 components were identified and their relative content was followed during the storage period. Among these were four alcohols, 17 aldehydes, four esters, ten alkanes, 11 ketones and six lactones. A general...... increase in the concentration of most of the volatile compounds during storage was found. The content of volatile compounds in dairy spreads stored at -18 OC was nearly constant or showed a rather low increase in the content during the storage period. Storage at higher temperatures (5 and 20 degrees...

  4. Carbon monoxide analysis: a comparison of two co-oximeters and headspace gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Costantino, A.G.; Park, J.; Caplan, Y.H.

    Three methods (lL-182 Co-Oximeter, lL-282 Co-Oximeter, and headspace gas chromatography) for the analysis of carbon monoxide in postmortem blood were studied and compared using a prepared reference standard, Quantra control materials, and 62 postmortem blood specimens. The methods compared favorably with one another. The linear regression equations for the 62 postmortem blood samples (range = 1.0 to 86% saturation) were: lL-282 vs. lL-182, y = 1.11x - 3.10, r = 0.981; lL-182 vs. GC, y = 0.88x + 2.97, r = 0.973; lL-282 vs. GC, y = 1.00x - 1.24, r = 0.986.

  5. Rapid quantification of dimethyl methylphosphonate from activated carbon particles by static headspace gas chromatography mass spectrometry.

    Science.gov (United States)

    Mitchell, Brendan L; Billingsley, Brit G; Logue, Brian A

    2013-06-01

    Activated carbon (AC) particles are utilized as an adsorbent for binding hazardous vapors in protective equipment. The binding affinity and utilization of these AC particles should be known to ensure effective and efficient use. Therefore, a simple and effective method was developed for the quantification of the chemical warfare agent simulant, dimethyl methylphosphonate (DMMP), from AC particles. Static headspace gas chromatography mass-spectrometry with internal standard, DMMP-d6, was used to perform the analysis. The method produced a linear dynamic range of 2.48-620g DMMP/kg carbon and a detection limit of 1.24g DMMP/kg carbon. Furthermore, the method produced a coefficient of variation of less than 16% for all intra- and inter-assay analyses. The method provided a simple and effective procedure for quantifying DMMP from AC particles and was applied to the analysis of a DMMP-exposed AC protective respirator filter.

  6. Storage stability of crips measured by headspace and peroxide value analyses

    Directory of Open Access Journals (Sweden)

    Lahtinen, R. M.

    1996-04-01

    Full Text Available Normal sunflower oil and high oleic acid sunflower oil were tested in industrial frying of crisps against the reference oil palm olein. A protective agent, dimethyl polysiloxane (DMPS, was also tested in crisp frying. Peroxide values and volatile contents of the crisps stored in normal storage conditions (room temperature were measured during storage. From the peroxide values it could be seen that crisps fried in normal sunflower oil were the most unstable during storage. Crisps fried in high oleic sunflower oil proved to be almost as stable towards oxidation as crisps fried in reference oil palm olein. Volatile contents, measured by a static headspace - gas chromatograph - mass spectrometry system, confirmed the conclusions of peroxide analysis. Neither of the methods could find any difference between the samples which had been fried with and without DMPS.

  7. Hanford Tank Ventilation System Condensates and Headspace Vapors: An Assessment of Potential Dermal Exposures

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, James L.; Springer, David L.

    2006-04-24

    This study considers the question of whether potential dermal exposures to Hanford high-level radioactive waste tank headspace vapors and their condensates could result in significant exposure to workers. Three types of potential exposures were evaluated; dermal contact with aqueous condensate, organic condensate, and direct contact with head space vapors. The dermal absorption rates from aqueous and organic condensates were estimated for selected chemicals using a model described by EPA (1992) with a modified correlation for dermal permeability suggested by Wilschut et al. (1995). Dermal absorption rates of vapors were estimated using a model given by AIHA (2000). Results were compared to an ''equivalent inhalation dose'' calculated by multiplying the inhalation occupational exposure limit by a nominal daily inhalation rate. The results should provide guidance for industrial hygienists to prepare specific recommendations based on specific scenarios.

  8. Isolation and quantification of volatiles in fish by dynamic headspace sampling and mass spectrometry.

    Science.gov (United States)

    Refsgaard, H H; Haahr, A M; Jensen, B

    1999-03-01

    A dynamic headspace sampling method for isolation of volatiles in fish has been developed. The sample preparation involved freezing of fish tissue in liquid nitrogen, pulverizing the tissue, and sampling of volatiles from an aqueous slurry of the fish powder. Similar volatile patterns were determined by use of this sample preparation method and for samples chewed for 10 s. Effects of sampling time, temperature, and purge flow on level of volatiles were tested. Purging at 340 mL/min for 30 min at 45 degrees C was found to be optimal. Detection limits for a number of aldehydes were 0.2-2.7 microg/kg. Levels of volatiles are given for fresh salmon, cod, saithe, mackerel, and redfish.

  9. Floral scent of brazilian Passiflora: five species analised by dynamic headspace.

    Science.gov (United States)

    Montero, Daniel A V; Marques, Marcia Ortiz M; Meletti, Laura M M; Kampen, Maria H VAN; Polozzi, Sandra C

    2016-09-01

    This study describes for the first time the chemical composition and olfactive description of floral scent from Brazilian Passiflora (Passiflora edulis Sim, Passiflora alata Curtis, Passiflora cincinnata Mast., Passiflora coccinea Aubl. and Passiflora quadrangularis L.). Five species were grown in greenhouse at the Agronomic Institute (IAC), São Paulo, Brazil. Volatile compounds were collected using dynamic headspace. Analyses of scent composition were performed by gas chromatograph coupled to mass spectrometer. Identification of chemical constituents was conducted through of retention index followed by comparative analysis of mass spectra with specialized databases. The olfactive descriptions of floral scent from each species was evaluated for a professional perfumer. High interspecific diversity was found between chemical compositions of floral scent within Passiflora and different bouquets were observed amount the studied species. Mayor constituents were linalool (P. alata), geraniol (P. quadrangularis), 1,4-dimethoxybenzene (P. edulis), benzaldehyde (P. cincinnata) and 2-methyl-3-pentanone (P. coccinea).

  10. Floral scent of brazilian Passiflora: five species analised by dynamic headspace

    Directory of Open Access Journals (Sweden)

    DANIEL A.V. MONTERO

    2016-01-01

    Full Text Available ABSTRACT This study describes for the first time the chemical composition and olfactive description of floral scent from Brazilian Passiflora (Passiflora edulis Sim, Passiflora alata Curtis, Passiflora cincinnata Mast., Passiflora coccinea Aubl. and Passiflora quadrangularis L.. Five species were grown in greenhouse at the Agronomic Institute (IAC, São Paulo, Brazil. Volatile compounds were collected using dynamic headspace. Analyses of scent composition were performed by gas chromatograph coupled to mass spectrometer. Identification of chemical constituents was conducted through of retention index followed by comparative analysis of mass spectra with specialized databases. The olfactive descriptions of floral scent from each species was evaluated for a professional perfumer. High interspecific diversity was found between chemical compositions of floral scent within Passiflora and different bouquets were observed amount the studied species. Mayor constituents were linalool (P. alata, geraniol (P. quadrangularis, 1,4-dimethoxybenzene (P. edulis, benzaldehyde (P. cincinnata and 2-methyl-3-pentanone (P. coccinea.

  11. A Survey of Vapors in the Headspaces of Single-Shell Waste Tanks

    Energy Technology Data Exchange (ETDEWEB)

    Stock, Leon M.; Huckaby, James L.

    2000-10-31

    This report summarizes data on the organic vapors in the single-shell high level radioactive waste tanks at the Hanford site to support a forthcoming toxicological study. All data were obtained from the Tank Characterization Database (PNNL 1999). The TCD contains virtually all the available tank headspace characterization data from 1992 to the present, and includes data for 109 different single-shell waste tanks. Each single-shell tank farm and all major waste types are represented. Descriptions of the sampling and analysis methods have been given elsewhere (Huckaby et al. 1995, Huckaby et al. 1996), and references for specific data are available in the TCD. This is a revision of a report with the same title issued on March 1, 2000 (Stock and Huckaby 2000).

  12. [Rapid determination of ethephon residues in concentrated pineapple juice by head-space gas chromatography].

    Science.gov (United States)

    Chu, X G; Yong, W; Cai, H X; Pan, J W

    2001-05-01

    The method developed is based on the special property that ethephon can be easily decomposed into ethene in alkaline solution by heating. Certain amount of concentrated KOH solution was added to the sample and heated at 70 degrees C. Then, 1 mL of the gas above the sample was injected into a gas chromatograph by head-space sampler for the determination of the target compound with external standard quantitation method. The detection limit was 0.025 mg/kg and the fortified recoveries of ethephon in concentrated pineapple juice (60 +/- 1) Brix at the range of 0.1 mg/kg-10 mg/kg were 92%-98% (n = 8, for each level). The relative standard deviations were 3.99%-7.94%.

  13. Headspace-gas chromatographic fingerprints to discriminate and classify counterfeit medicines.

    Science.gov (United States)

    Custers, D; Canfyn, M; Courselle, P; De Beer, J O; Apers, S; Deconinck, E

    2014-06-01

    Counterfeit medicines are a global threat to public health. These pharmaceuticals are not subjected to quality control and therefore their safety, quality and efficacy cannot be guaranteed. Today, the safety evaluation of counterfeit medicines is mainly based on the identification and quantification of the active substances present. However, the analysis of potential toxic secondary components, like residual solvents, becomes more important. Assessment of residual solvent content and chemometric analysis of fingerprints might be useful in the discrimination between genuine and counterfeit pharmaceuticals. Moreover, the fingerprint approach might also contribute in the evaluation of the health risks different types of counterfeit medicines pose. In this study a number of genuine and counterfeit Viagra(®) and Cialis(®) samples were analyzed for residual solvent content using headspace-GC-MS. The obtained chromatograms were used as fingerprints and analyzed using different chemometric techniques: Principal Component Analysis, Projection Pursuit, Classification and Regression Trees and Soft Independent Modelling of Class Analogy. It was tested whether these techniques can distinguish genuine pharmaceuticals from counterfeit ones and if distinct types of counterfeits could be differentiated based on health risks. This chemometric analysis showed that for both data sets PCA clearly discriminated between genuine and counterfeit drugs, and SIMCA generated the best predictive models. This technique not only resulted in a 100% correct classification rate for the discrimination between genuine and counterfeit medicines, the classification of the counterfeit samples was also superior compared to CART. This study shows that chemometric analysis of headspace-GC impurity fingerprints allows to distinguish between genuine and counterfeit medicines and to differentiate between groups of counterfeit products based on the public health risks they pose. Copyright © 2014 Elsevier B

  14. Influence of olive oil phenolic compounds on headspace aroma release by interaction with whey proteins.

    Science.gov (United States)

    Genovese, Alessandro; Caporaso, Nicola; De Luca, Lucia; Paduano, Antonello; Sacchi, Raffaele

    2015-04-22

    The release of volatile compounds in an oil-in-water model system obtained from olive oil-whey protein (WP) pairing was investigated by considering the effect of phenolic compounds. Human saliva was used to simulate mouth conditions by retronasal aroma simulator (RAS) analysis. Twelve aroma compounds were quantified in the dynamic headspace by SPME-GC/MS. The results showed significant influences of saliva on the aroma release of virgin olive oil (VOO) volatiles also in the presence of WP. The interaction between WP and saliva leads to lower headspace release of ethyl esters and hexanal. Salivary components caused lower decrease of the release of acetates and alcohols. A lower release of volatile compounds was found in the RAS essay in comparison to that in orthonasal simulation of only refined olive oil (without addition of saliva or WP), with the exception of hexanal and 1-penten-3-one, where a significantly higher release was found. Our results suggest that the extent of retronasal odor (green, pungent) of these two volatile compounds is higher than orthonasal odor. An extra VOO was used to verify the release in model systems, indicating that WP affected aroma release more than model systems, while saliva seems to exert an opposite trend. A significant increase in aroma release was found when phenolic compounds were added to the system, probably due to the contrasting effects of binding of volatile compounds caused by WP, for the polyphenol-protein interaction phenomenon. Our study could be applied to the formulation of new functional foods to enhance flavor release and modulate the presence and concentrations of phenolics and whey proteins in food emulsions/dispersions.

  15. Analysis of ultrafine TATB by ultrasonic-assisted equilibrium headspace analysis

    Energy Technology Data Exchange (ETDEWEB)

    Chambers, D M

    2000-09-12

    The purpose of this work was to screen different lots of ultrafine 1,3,5-triamine 2,4,6-trinitrobenzene (TATB) for chemical differences, which may include synthesis and formulation byproducts, decomposition products, and contaminants. The approach used here permits analysis of trapped species as volatile and semivolatile chemicals within a solid. This procedure involves preconcentration of species from the TATB matrix into a surrounding headspace followed by a preconcentration and collection step using solid phase microextraction (SPME) collection. The sample is prepared by sealing it in a glass ampule with a few milliliters of water, ultrasonicating the solution, and then sampling the headspace using SPME collection. Water couples in the ultrasonic energy to fracture the TATB, which permits the release of nonpolar species into the gas phase. However, polar species will favor the aqueous phase and require a separate analysis procedure, which is not included here. Following SPME collection, the sample is transferred to a gas chromatography/mass spectrometer (GCMS) for analysis. In this work, we analyzed and interpreted outgas signatures from four different lots (1169-135MPS-001, 4271-135M-002, 91190-135M-003, and 98170-135M-001) of ultrafine TATB. Lot 98170-135M-001 is a reprocessing of Lot 4271-135M-002, which was washed to remove the water-soluble polysaccharides. The pedigree for these materials are found in a memo from Tom Stallings and Gordon Osborn of Mason & Hanger Co., Pantex Plant in the Appendix section. Nominally, ultrafine TATB is synthesized via the emulsion-amination method in which an emulsifier is included during the amination of the 1,3,5-trichloro-2,4,6-trinitrobenzene (TCTNB) precursor. The ultrafine TATB formulation also includes 0.2% by weight guar gum, a galactomannan polysaccharide, to enhance flow properties. Historically, this polysaccharide was added to PETN to reduce its sublimation temperature, but it was also found to enhance flow

  16. Determination of volatile organic compounds in water by headspace solid-phase microextraction gas chromatography coupled to tandem mass spectrometry with triple quadrupole analyzer.

    Science.gov (United States)

    Cervera, M I; Beltran, J; Lopez, F J; Hernandez, F

    2011-10-17

    In the present work, a rapid method with little sample handling has been developed for determination of 23 selected volatile organic compounds in environmental and wastewater samples. The method is based on headspace solid-phase microextraction (SPME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) determination using triple quadrupole analyzer (QqQ) in electron ionization mode. The best conditions for extraction were optimised with a factorial design taking into account the interaction between different parameters and not only individual effects of variables. In the optimized procedure, 4 mL of water sample were extracted using a 10 mL vial and adding 0.4 g NaCl (final NaCl content of 10%). An SPME extraction with carboxen/polydimethylsiloxane 75 μm fiber for 30 min at 50°C (with 5 min of previous equilibration time) with magnetic stirring was applied. Chromatographic determination was carried out by GC-MS/MS working in Selected Reaction Monitoring (SRM) mode. For most analytes, two MS/MS transitions were acquired, although for a few compounds it was difficult to obtain characteristic abundant fragments. In those cases, a pseudo selected reaction monitoring (pseudo-SRM) with three ions was used instead. The intensity ratio between quantitation (Q) and confirmation (q) signals was used as a confirmatory parameter. The method was validated by means of recovery experiments (n=6) spiking mineral water samples at three concentration levels (0.1, 5 and 50 μg L(-1)). Recoveries between 70% and 120% were generally obtained with relative standard deviations (RSDs) lower than 20%. The developed method was applied to surface water and wastewater from a wastewater treatment plant and from a municipal solid-waste treatment plant. Several compounds, like chloroform, benzene, trichloroethylene, toluene, tetrachloroethylene, dibromochloromethane, xylenes and bromoform were detected and confirmed in all the samples analyzed.

  17. Rapid analysis of Fructus forsythiae essential oil by ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction followed by gas chromatography–mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jiao, Jiao [State Key Laboratory of Tree Genetics and Breeding, Northeast Forestry University, Harbin 150040 (China); Ma, Dan-Hui [College of Life Sciences, Northeast Forestry University, Harbin 150040 (China); Gai, Qing-Yan; Wang, Wei; Luo, Meng [State Engineering Laboratory of Bio-Resource Eco-Utilization, Northeast Forestry University, Harbin 150040 (China); Fu, Yu-Jie, E-mail: yujie_fu2002@yahoo.com [State Engineering Laboratory of Bio-Resource Eco-Utilization, Northeast Forestry University, Harbin 150040 (China); Ma, Wei, E-mail: mawei@hljucm.net [State Key Laboratory of Tree Genetics and Breeding, Northeast Forestry University, Harbin 150040 (China); School of Pharmaceutical, Heilongjiang University of Chinese Medicine, Harbin 150040 (China)

    2013-12-04

    Graphical abstract: -- Highlights: •A new ILAMD-HS-SDME method is developed for the microextraction of essential oil. •ILs used as destruction agent of plant cell walls and microwave absorption medium. •Parameters affecting the extraction efficiency are optimized by Box–Behnken design. •Procedure benefits: similar constituents, shorter duration and smaller sample amount. •ILAMD-HS-SDME followed by GC–MS is a promising technique in analytical fields. -- Abstract: A rapid, green and effective miniaturized sample preparation and analytical technique, i.e. ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction (ILAMD-HS-SDME) followed by gas chromatography–mass spectrometry (GC–MS) was developed for the analysis of essential oil (EO) in Fructus forsythiae. In this work, ionic liquids (ILs) were not only used as the absorption medium of microwave irradiation but also as the destruction agent of plant cell walls. 1-Ethyl-3-methylimidazolium acetate ([C{sub 2}mim]OAc) was chosen as the optimal ILs. Moreover, n-heptadecane (2.0 μL) was selected as the appropriate suspended solvent for the extraction and concentration of EO. Extraction conditions of the proposed method were optimized using the relative peak area of EO constituents as the index, and the optimal operational parameters were obtained as follows: irradiation power (300 W), sample mass (0.7 g), mass ratio of ILs to sample (2.4), temperature (78 °C) and time (3.4 min). In comparison to previous reports, the proposed method was faster and required smaller sample amount but could equally monitor all EO constituents with no significant differences.

  18. 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.

  19. Analysis of biofluids for gamma-hydroxybutyrate (GHB) and gamma-butyrolactone (GBL) by headspace GC-FID and GC-MS.

    Science.gov (United States)

    LeBeau, M A; Montgomery, M A; Miller, M L; Burmeister, S G

    2000-09-01

    The past few years have seen a dramatic increase in the abuse of gamma-hydroxybutyrate (GHB) and gamma-butyrolactone (GBL) in the United States. The abuse stems primarily from their euphoric and sedative properties, but these substances are also misused by bodybuilders as steroid alternatives. Recently there has been an alarming increase in the use of GHB and GBL in crimes of drug-facilitated sexual assault. A rapid and sensitive procedure was developed for the analysis of biofluids containing GHB and GBL. Two separate aliquots of a biological specimen were spiked with an alpha-methylene-gamma-butyrolactone internal standard solution. One of the aliquots was treated with concentrated sulfuric acid for cyclization of GHB to GBL and the other remained untreated. Both aliquots were extracted with methylene chloride and concentrated. Extracts were screened using automated headspace gas chromatography-flame-ionization detection (GC-FID). Qualitative findings were quantitated and confirmed in a manner similar to the GC-FID procedure with some modifications. A calibrated solution of GHB-d6 (or GBL-d6, when warranted) was added to the aliquots at a concentration approximating the level determined by the GC-FID screen. The extraction was as described with conversion of GHB to GBL, but analysis was by full-scan gas chromatography-mass spectrometry (El). Quantitation was performed by comparison of the area of the molecular ion of the parent drug (m/z 86) to that of the calibrated deuterated analogue (m/z 92). This analytical procedure allows for the rapid detection of GHB and GBL in biofluids. Its sensitivity has proven useful for the toxicological investigation of cases of drug-facilitated sexual assault.

  20. Volatile profile of the headspace fraction of "assa-peixe" (Vernonia sp. honeys Perfil dos compostos voláteis presentes na fração "headspace" de méis de assa-peixe

    Directory of Open Access Journals (Sweden)

    Mariana Carvalho Ribeiro

    2008-03-01

    Full Text Available The volatile compounds were isolated from the headspace fraction of "assa-peixe" honeys by adsorptive column chromatography, eluted with acetone and analysed by GC-FID and GC-MS. Volatile compounds were separated using a polar phase column. Low- and medium-boiling point volatile compounds predominated in the headspace. A large proportion of 3-penten-2-one (80.5 ± 13.9 µg.kg-1 and benzaldehyde (25.9 ± 4.2 µg.kg-1 was found in the headspace fraction, while 2-penten-1-ol, 3-hexenyl butanoate, octadecane and hexanoic acid (Os compostos voláteis da fração "Headspace" de méis de assa-peixe foram adsorvidos pela técnica de cromatografia de adsorção, eluídos com acetona e analisados através da CG/DIC e CG/EM usando coluna polar de sílica fundida. Os compostos voláteis de baixo e médio ponto de ebulição predominaram na fração "headspace". Foi achada uma grande proporção de 3-penten-2-ona (80,5 ± 13,9 µg.kg-1 e benzaldeído (25,9 ± 4,2 µg.kg-1, enquanto o 2-penten-1-ol, o hexanoato de 3-hexenila, o octadecano e o ácido hexanóico (<0,01 µg.kg-1 foram compostos minoritários. Um total de doze compostos voláteis foi identificado, sendo cinco descritos pela primeira vez no mel de assa-peixe. Destes cinco, a 3-penten-2-ona, o dodecano, o tridecano e o benzaldeído foram definitivamente identificados na fração "headspace" dos méis de assa-peixe brasileiro.

  1. Identification of volatile organic compounds (VOCs in different colour carrot (Daucus carota L. cultivars using static headspace/gas chromatography/mass spectrometry

    Directory of Open Access Journals (Sweden)

    Zehra Güler

    2015-12-01

    Full Text Available Volatile organic compounds (VOCs as well as sugar and acid contents affect carrot flavour. This study compared VOCs in 11 carrot cultivars. Gas chromatography/mass spectrometry using static headspace technique was applied to analyse the VOCs. The number of VOCs per sample ranged from 17 to 31. The primarily VOCs identified in raw carrots with the exception of “Yellow Stone” were terpenes, ranging from 65 to 95%. The monoterpenes with values ranging from 31 to 89% were higher than those (from 2 to 15% of sesquiterpenes. Monoterpene α-terpinolene (with ranging from 23 to 63% and (--α-pinene (26%, and alcohol ethanol (35% was the main VOC in extracts from the nine carrot cultivars, “Purple” and “Yellow Stone”, respectively. As a result, among 16 identified monoterpenes, 7 monoterpenes (--α-pinene, (--β-pinene, β-myrcene, d-limonene, γ-terpinene, α-terpinolene and p-cymene constituted more than 60% of total VOCs identified in carrots including “Atomic Red”, “Nantes”, “Cosmic Purple”, “Red Samurai”, “Eregli Black”, “White Satin”, “Parmex” and “Baby Carrot”. Thus, these cultivars may advise to carrot breeders due to the beneficial effects of terpenes, especially monoterpenes on health.

  2. Quantification of 2-acetyl-1-pyrroline in rice by stable isotope dilution assay through headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Maraval, Isabelle; Sen, Kemal; Agrebi, Abdelhamid; Menut, Chantal; Morere, Alain; Boulanger, Renaud; Gay, Frédéric; Mestres, Christian; Gunata, Ziya

    2010-08-24

    A new and convenient synthesis of 2-acetyl-1-pyrroline (2AP), a potent flavor compound in rice, and its ring-deuterated analog, 2-acetyl-1-d(2)-pyrroline (2AP-d(2)), was reported. A stable isotope dilution assay (SIDA), involving headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-positive chemical ionization-ion trap-tandem mass spectrometry (GC-PCI-IT-MS-MS), was developed for 2AP quantification. A divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was used for HS-SPME procedure and parameters affecting analytes recovery, such as extraction time and temperature, pH and salt, were studied. The repeatability of the method (n=10) expressed as relative standard deviation (RSD) was 11.6%. A good linearity was observed from 5.9 to 779 ng of 2AP (r(2)=0.9989). Limits of detection (LOD) and quantification (LOQ) for 2AP were 0.1 and 0.4 ng g(-1) of rice, respectively. The recovery of spiked 2AP from rice matrix was almost complete. The developed method was applied to the quantification of 2AP in aerial parts and grains of scented and non-scented rice cultivars.

  3. Quantification of 2-acetyl-1-pyrroline in rice by stable isotope dilution assay through headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Maraval, Isabelle [UMR Qualisud, CIRAD, 73 Rue J. F. Breton, 34398 Montpellier Cedex 5 (France); UMR Qualisud, Universite Montpellier 2, place E. Bataillon, 34095 Montpellier Cedex 5 (France); Sen, Kemal [Department of Food Engineering, Faculty of Agriculture, University of Cukurova, 01330 Adana (Turkey); Agrebi, Abdelhamid; Menut, Chantal; Morere, Alain [UMR 5247, Institut des Biomolecules Max Mousseron (IBMM), CNRS, Universites Montpellier 2 et 1, Ecole Nationale Superieure de Chimie de Montpellier, 8 Rue de l' Ecole Normale, 34296 Montpellier Cedex 5 (France); Boulanger, Renaud [UMR Qualisud, CIRAD, 73 Rue J. F. Breton, 34398 Montpellier Cedex 5 (France); Gay, Frederic [CIRAD, DORAS Centre, Research and Development Building, Kasetsart University, Bangkok 10900 (Thailand); Mestres, Christian [UMR Qualisud, CIRAD, 73 Rue J. F. Breton, 34398 Montpellier Cedex 5 (France); Gunata, Ziya, E-mail: zgunata@univ-montp2.fr [UMR Qualisud, Universite Montpellier 2, place E. Bataillon, 34095 Montpellier Cedex 5 (France)

    2010-08-24

    A new and convenient synthesis of 2-acetyl-1-pyrroline (2AP), a potent flavor compound in rice, and its ring-deuterated analog, 2-acetyl-1-d{sub 2}-pyrroline (2AP-d{sub 2}), was reported. A stable isotope dilution assay (SIDA), involving headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-positive chemical ionization-ion trap-tandem mass spectrometry (GC-PCI-IT-MS-MS), was developed for 2AP quantification. A divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was used for HS-SPME procedure and parameters affecting analytes recovery, such as extraction time and temperature, pH and salt, were studied. The repeatability of the method (n = 10) expressed as relative standard deviation (RSD) was 11.6%. A good linearity was observed from 5.9 to 779 ng of 2AP (r{sup 2} = 0.9989). Limits of detection (LOD) and quantification (LOQ) for 2AP were 0.1 and 0.4 ng g{sup -1} of rice, respectively. The recovery of spiked 2AP from rice matrix was almost complete. The developed method was applied to the quantification of 2AP in aerial parts and grains of scented and non-scented rice cultivars.

  4. Determining urea levels in dialysis human serum by means of headspace solid phase microextraction coupled with ion mobility spectrometry and on the basis of nanostructured polypyrrole film.

    Science.gov (United States)

    Kalhor, Hamideh; Alizadeh, Naader

    2013-06-01

    A simple and sensitive headspace (HS) solid phase microextraction (SPME) coupled with ion mobility spectrometry (IMS) method is presented for analysis of urea in dialysis human serum samples. A dodecylbenzenesulfonate-doped polypyrrole coating was used as a fiber for SPME. The HS-SPME-IMS method exhibits good repeatability (relative standard deviation of 3% or less), simplicity, and good sensitivity. The influence of various analytical parameters such as pH, ionic strength, extraction time and temperature was investigated and the parameters were optimized. The calibration graph was linear in the range from 5 to 50 μg mL(-1), and the detection limit was 2 μg mL(-1). The method was applied successfully for determination of urea in human serum and with acceptable recovery (more than 98%). Finally, a standard addition calibration method was applied to the HS-SPME-IMS method for the analysis of human serum samples before and at the end of dialysis. The proposed method appears to be suitable for the analysis of urea in serum samples as it is not time-consuming and requires only small quantities of the sample without any derivatization process.

  5. Development of a portable mass spectrometer characterized by discontinuous sample gas introduction, a low-pressure dielectric barrier discharge ionization source, and a vacuumed headspace technique.

    Science.gov (United States)

    Kumano, Shun; Sugiyama, Masuyuki; Yamada, Masuyoshi; Nishimura, Kazushige; Hasegawa, Hideki; Morokuma, Hidetoshi; Inoue, Hiroyuki; Hashimoto, Yuichiro

    2013-05-21

    The present study has attempted to downscale a mass spectrometer in order to make it portable and enable onsite analysis with it. The development of a small mass spectrometer required the use of a compact pump whose displacement was small, decreasing the sensitivity of that spectrometer. To get high sensitivity with a small mass spectrometer, we have integrated novel techniques: a highly sensitive ionization source and efficient extraction of sample vapor. The low-pressure dielectric barrier discharge ionization (LP-DBDI) source made it possible to increase the conductance between the source and the mass analyzer, compared with ambient ionization sources, enhancing the efficiency of the ion transfer from the ionization source to the mass analyzer. We have also developed a vacuumed headspace method efficiently transporting the sample vapor to the ionization source. The sensitivity was further enhanced by also using a discontinuous sample gas introduction technique. A prototype portable mass spectrometer using those novel techniques was found to be sensitive enough to detect 0.1 ppm methamphetamine, 1 ppm amphetamine, 1 ppm 3,4-methylenedioxymethamphetamine, and 10 ppm cocaine in liquid.

  6. Storage stability studies for tributyltin determination in human urine samples using headspace solid-phase microextraction and gas chromatography mass spectrometry.

    Science.gov (United States)

    Zachariadis, G A; Tzollas, N M; Nikolaou, M; Rosenberg, E

    2013-03-01

    A headspace solid-phase micro-extraction (HS-SPME) method was employed in order to study the effect of storage conditions of human urine samples spiked with tributyltin (TBT) using gas chromatography and mass spectrometry. To render the analyte more volatile, the derivatization (ethylation) was made in situ by sodium tetraethylborate (NaBEt(4) ), which was added directly to dilute unpreserved urine samples and in buffers of similar acidity. The stability of TBT in human urine matrix was compared with the stability of TBT in buffer solutions of similar pH value. Critical parameters of storage conditions such as temperature and time, which affect the stability of TBT in this kind of matrix, were examined extensively. The tests showed that the stability of TBT remains practically satisfactory for a maximum of 2 days of storage either at +4 or 20°C. Greater variations were observed in the concentration of TBT in human urine samples at +4°C and lower ones at -20°C over a month's storage. The freeze-thaw cycles have negative effect on the stability and should be kept to a minimum. The results from spiked urine samples are also discussed in comparison to those acquired from buffer solutions of equal TBT concentration.

  7. Novel multiwalled carbon nanotubes-polyaniline composite film coated platinum wire for headspace solid-phase microextraction and gas chromatographic determination of phenolic compounds.

    Science.gov (United States)

    Du, Wei; Zhao, Faqiong; Zeng, Baizhao

    2009-05-01

    A novel multiwalled carbon nanotubes-polyaniline composite (MWCNTs-PANI) film coated platinum wire was fabricated through electrochemical deposition. The coating was characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectrophotometry and thermogravimetry. It was found that the coating was porous and had large specific area and adsorption capacity; in the composite MWCNTs and polyaniline interacted with each other and the film kept stable up to 320 degrees C. The as-made fiber was used for the headspace solid-phase microextraction (HS-SPME) of some phenolic compounds (i.e. 2-chlorophenol, 2,4-dichlorophenol, 2-methylphenol, 3-methylphenol, 2,6-dimethylphenol, 2-nitrophenol), followed by gas chromatographic analysis. The MWCNTs-PANI coating showed better analytical performance than PANI. Under the optimized conditions, the detection limits were 1.89-65.9 ng L(-1), the relative standard deviations (RSDs) were 2.7-6.5% for six successive measurements with single fiber, the RSDs for fiber-to-fiber were 5.2-12.4%, the linear ranges exceeded two magnitudes with correlation coefficient above 0.992. The fiber could be used for more than 250 times without decrease of efficiency. The proposed method was successfully applied to the extraction and determination of phenolic compounds in water sample, and the recoveries were 87.7-111.5% for different analytes. In addition, the fiber also presented advantages of easy preparation and low cost. Therefore, it is a promising SPME fiber.

  8. Molecular characterisation of birch bark tar by headspace solid-phase microextraction gas chromatography-mass spectrometry: a new way for identifying archaeological glues.

    Science.gov (United States)

    Regert, M; Alexandre, V; Thomas, N; Lattuati-Derieux, A

    2006-01-06

    To develop an analytical methodology, as non-destructive as possible, suitable for the identification of natural substances from archaeological origin, we studied the potentiality of solid-phase microextraction (SPME) for analysing birch bark tar, an adhesive commonly used during ancient times. First of all, birch bark tars were produced by a controlled heating of birch bark. The two kinds of samples obtained using different processes of fabrication, one at liquid state, the second one at solid state, were then analysed by headspace HS-SPME-GC-MS. Different conditions of sample treatment were tested (two different fibre coatings, various times and temperatures of extraction) in order to suggest optimal conditions for the analysis of birch bark tar. Both samples were shown to be rich in volatile organic components. Two main groups of constituents, namely phenolic compounds issued from lignin or tannin known to be present in bark and sesquiterpenoid hydrocarbons, secondary metabolites largely distributed in the plant kingdom, were detected for the first time in birch bark tar. HS-SPME-GC-MS appears thus to be a very efficient method for investigating the volatiles emitted by plant tars and could be further used for the study of birch bark tar samples issued from archaeological context.

  9. Multiple headspace-solid phase microextraction for the determination of migrants coming from a self-stick label in fresh sausage.

    Science.gov (United States)

    Canellas, E; Vera, P; Nerín, C

    2016-04-15

    Most fresh sausages are sold with a self-stick adhesive label stuck directly on it. Because of that, the substances in the adhesive could migrate into the fresh sausage. In this work, the multiple headspace-solid-phase microextraction technique has been optimized to quantify the migrants found in the fresh sausage. All the compounds could be analyzed by this technique since its concentration decay exponentially with the number of extractions with good correlation coefficients (0.8258-0.9987). Then, migration assays were carried out and an evaluation of the potential risk for the human health was undertaken with the conclusion that the migration of the compounds from the label does not endanger human health. The results were compared those obtained in migration to casing filled with isooctane used as fat food simulant by Canellas et al. (2014). The values obtained for isooctane (10-600 ng/g) were much higher than the migration values found in the meat stuffed in casing expressed as ng/g of fat content (ranged from 0.02 to 3.3 ng/g of fat content). This finding shows that in some scenarios, it is difficult to simulate the intended contact of materials used in food packaging with simulants.

  10. Optimization of a Dynamic Headspace-Thermal Desorption-Gas Chromatography/Mass Spectrometry procedure for the determination of furfurals in vinegars.

    Science.gov (United States)

    Manzini, Simona; Durante, Caterina; Baschieri, Carlo; Cocchi, Marina; Sighinolfi, Simona; Totaro, Sara; Marchetti, Andrea

    2011-08-15

    The use of a Dynamic Headspace System (DHS) device combined with a Thermal Desorption Unit (TDU) interfaced to a Gas Chromatography/Mass Spectrometry (GC/MS) system is proposed for the determination of furfurals in oenological products. An experimental design protocol has been employed for the optimization of the instrumental settings concerning DHS and TDU extraction and desorption steps. It has been possible to individuate the following optimized conditions: incubation temperature 40°C, purge volume 800 mL, dry volume 1500 mL, TDU hold time 5 min and incubation time 10 min. The performance of two different SPE sorbents, namely Tenax TA and Tenax GR used for the furfurals trapping, was investigated too. The developed DHS sampling procedure showed good reproducibility values with a RSD% lower than 10% for all the monitored species. The optimized experimental settings have been used to determine furfurals in several vinegar samples obtained by traditional procedure starting from cooked grape musts, i.e. in Aceto Balsamico Tradizionale di Modena (ABTM). In fact, the control of these species is extremely important for quality and safety issues.

  11. A high-throughput platform for low-volume high-temperature/pressure sealed vessel solvent extractions

    Energy Technology Data Exchange (ETDEWEB)

    Damm, Markus [Christian Doppler Laboratory for Microwave Chemistry (CDLMC) and Institute of Chemistry, Karl-Franzens-University Graz, Heinrichstrasse 28, A-8010 Graz (Austria); Kappe, C. Oliver, E-mail: oliver.kappe@uni-graz.at [Christian Doppler Laboratory for Microwave Chemistry (CDLMC) and Institute of Chemistry, Karl-Franzens-University Graz, Heinrichstrasse 28, A-8010 Graz (Austria)

    2011-11-30

    Highlights: Black-Right-Pointing-Pointer Parallel low-volume coffee extractions in sealed-vessel HPLC/GC vials. Black-Right-Pointing-Pointer Extractions are performed at high temperatures and pressures (200 Degree-Sign C/20 bar). Black-Right-Pointing-Pointer Rapid caffeine determination from the liquid phase. Black-Right-Pointing-Pointer Headspace analysis of volatiles using solid-phase microextraction (SPME). - Abstract: A high-throughput platform for performing parallel solvent extractions in sealed HPLC/GC vials inside a microwave reactor is described. The system consist of a strongly microwave-absorbing silicon carbide plate with 20 cylindrical wells of appropriate dimensions to be fitted with standard HPLC/GC autosampler vials serving as extraction vessels. Due to the possibility of heating up to four heating platforms simultaneously (80 vials), efficient parallel analytical-scale solvent extractions can be performed using volumes of 0.5-1.5 mL at a maximum temperature/pressure limit of 200 Degree-Sign C/20 bar. Since the extraction and subsequent analysis by either gas chromatography or liquid chromatography coupled with mass detection (GC-MS or LC-MS) is performed directly from the autosampler vial, errors caused by sample transfer can be minimized. The platform was evaluated for the extraction and quantification of caffeine from commercial coffee powders assessing different solvent types, extraction temperatures and times. For example, 141 {+-} 11 {mu}g caffeine (5 mg coffee powder) were extracted during a single extraction cycle using methanol as extraction solvent, whereas only 90 {+-} 11 were obtained performing the extraction in methylene chloride, applying the same reaction conditions (90 Degree-Sign C, 10 min). In multiple extraction experiments a total of {approx}150 {mu}g caffeine was extracted from 5 mg commercial coffee powder. In addition to the quantitative caffeine determination, a comparative qualitative analysis of the liquid phase coffee

  12. Tank vapor characterization project - Tank 241-U-112 headspace gas and vapor characterization: Results for homogeneity samples collected on December 6, 1996

    Energy Technology Data Exchange (ETDEWEB)

    Sklarew, D.S.; Pool, K.H.; Evans, J.C.; Hayes, J.C. [and others

    1997-09-01

    This report presents the results of analyses of samples taken from the headspace of waste storage tank 241-U-112 (Tank U-112) at the Hanford Site in Washington State. Samples were collected to determine the homogeneity of selected inorganic and organic headspace constitutents. Two risers (Riser 3 and Riser 6) were sampled at three different elevations (Bottom, Middle, and Top) within the tank. Tank headspace samples were collected by SGN Eurisys Service Corporation (SESC) and were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Ammonia was determined to be above the immediate notification limit specified by the sampling and analysis plan.

  13. Tank vapor characterization project - Tank 241-TY-103 headspace gas and vapor characterization: Results for homogeneity samples collected on November 22, 1996

    Energy Technology Data Exchange (ETDEWEB)

    Olsen, K.B.; Pool, K.H.; Evans, J.C.; Hayes, J.C. [and others

    1997-07-01

    This report presents the results of analyses of samples taken from the headspace of waste storage tank 241-TY-103 (Tank TY-103) at the Hanford Site in Washington State. Samples were collected to determine the homogeneity of selected inorganic and organic headspace constituents. Two risers (Riser 8 and Riser 18) were sampled at three different elevations (Top, Middle, and Bottom) within the tank. Tank headspace samples were collected by SGN Eurisys Service Corporation (SESC) and were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. No analytes were determined to be above immediate notification limits specified by the sampling and analysis plan (SAP).

  14. Reliable characterization of coffee bean aroma profiles by automated headspace solid phase microextraction-gas chromatography-mass spectrometry with the support of a dual-filter mass spectra library.

    Science.gov (United States)

    Mondello, Luigi; Costa, Rosaria; Tranchida, Peter Quinto; Dugo, Paola; Lo Presti, Maria; Festa, Saverio; Fazio, Alessia; Dugo, Giovanni

    2005-06-01

    This investigation is based on the automated solid phase microextraction GC-MS analysis of the volatile fraction of a variety of coffee bean matrices. Volatile analytes were extracted by headspace (HS)-SPME which was achieved with the support of automated instrumentation. The research was directed towards various important aspects relating to coffee aroma analysis: monitoring of the volatile fraction formation during roasting; chromatographic differentiation of the two main coffee species (Arabica and Robusta) and of a single species from different geographical origins; evaluation of the influence of specific industrial treatments prior to roasting. Reliable peak assignment was carried out through the use of a recently laboratory-constructed "flavour and fragrance" library and a dual-filter MS spectral search procedure. Further emphasis was placed on the automated SPME instrumentation and on its ability to supply highly repeatable chromatographic data.

  15. Dynamic headspace solid-phase microextraction combined with one-dimensional gas chromatography-mass spectrometry as a powerful tool to differentiate banana cultivars based on their volatile metabolite profile.

    Science.gov (United States)

    Pontes, Marisela; Pereira, Jorge; Câmara, José S

    2012-10-15

    In this study the effect of the cultivar on the volatile profile of five different banana varieties was evaluated and determined by dynamic headspace solid-phase microextraction (dHS-SPME) combined with one-dimensional gas chromatography-mass spectrometry (1D-GC-qMS). This approach allowed the definition of a volatile metabolite profile to each banana variety and can be used as pertinent criteria of differentiation. The investigated banana varieties (Dwarf Cavendish, Prata, Maçã, Ouro and Platano) have certified botanical origin and belong to the Musaceae family, the most common genomic group cultivated in Madeira Island (Portugal). The influence of dHS-SPME experimental factors, namely, fibre coating, extraction time and extraction temperature, on the equilibrium headspace analysis was investigated and optimised using univariate optimisation design. A total of 68 volatile organic metabolites (VOMs) were tentatively identified and used to profile the volatile composition in different banana cultivars, thus emphasising the sensitivity and applicability of SPME for establishment of the volatile metabolomic pattern of plant secondary metabolites. Ethyl esters were found to comprise the largest chemical class accounting 80.9%, 86.5%, 51.2%, 90.1% and 6.1% of total peak area for Dwarf Cavendish, Prata, Ouro, Maçã and Platano volatile fraction, respectively. Gas chromatographic peak areas were submitted to multivariate statistical analysis (principal component and stepwise linear discriminant analysis) in order to visualise clusters within samples and to detect the volatile metabolites able to differentiate banana cultivars. The application of the multivariate analysis on the VOMs data set resulted in predictive abilities of 90% as evaluated by the cross-validation procedure.

  16. Quantitative determination of wine highly volatile sulfur compounds by using automated headspace solid-phase microextraction and gas chromatography-pulsed flame photometric detection. Critical study and optimization of a new procedure.

    Science.gov (United States)

    López, Ricardo; Lapeña, Ana Cristina; Cacho, Juan; Ferreira, Vicente

    2007-03-02

    The quantitative determination of wine volatile sulfur compounds by automated headspace solid-phase microextraction (HS-SPME) with a carboxen-polydimethylsiloxane (CAR-PDMS) fiber and subsequent gas chromatography-pulsed flame photometric detection (GC-PFPD) has been evaluated. The direct extraction of the sulfur compounds in 5 ml of wine has been found to suffer from matrix effects and short linear ranges, problems which could not be solved by the use of different internal standards or by multiple headspace SPME. These problems were attributed to saturation of the fiber and to competitive effects between analytes, internal standards and other wine volatiles. Another problem was the oxidation of analytes during the procedure. The reduction in sample volume by a factor 50 (0.1 ml diluted with water or brine) brought about a reduction in the amount of sulfur compounds taken in the fiber by a factor just 3.3. Consequently, a new procedure has been proposed. In a sealed vial containing 4.9 ml of saturated NaCl brine, the air is thoroughly displaced with nitrogen, and the wine (0.1 ml) and the internal standards (0.02 ml) are further introduced with a syringe through the vial septum. This sample is extracted at 35 degrees C for 20 min. This procedure makes a satisfactory determination possible of hydrogen sulfide, methanethiol, ethanethiol, dimethyl sulfide, diethyl sulfide and dimethyl disulfide. The linear dynamic ranges cover the normal ranges of occurrence of these analytes in wine with typical r2 between 0.9823 and 0.9980. Reproducibility in real samples ranges from 10 to 20% and repeatability is better than 10% in most cases. The method accuracy is satisfactory, with errors below 20% for hydrogen sulfide and mostly below 10% for the other compounds. The proposed method has been applied to the analysis of 34 Spanish wines.

  17. Análise dos compostos voláteis da aguardente de cana por concentração dinâmica do "headspace" e cromatografia gasosa-espectrometria de massas The analysis of volatile compounds from Brazilian sugar cane spirit by dynamic headspace concentration and gas chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Ian Carneiro da Cunha Nóbrega

    2003-08-01

    Full Text Available Os compostos voláteis da aguardente de cana foram extraídos por meio da concentração dinâmica do "headspace" em armadilhas contendo Tenax-TA e analisados por cromatografia gasosa-espectrometria de massas. Cerca de 100 compostos voláteis, com número de carbonos que variavam de 5 a 18, foram detectados. Destes, 22 foram selecionados, sendo 18 ésteres, com base nas suas quantidades no extrato ou nas suas características sensoriais obtidas na literatura. Os compostos presentes em maiores quantidades foram o 3-metil-1-butanol (álcool isoamílico, 1,1-dietoxi-etano (acetaldeído dietil acetal e os ésteres acetato de 3-metilbutila, hexanoato de etila, octanoato de etila, decanoato de etila e dodecanoato de etila. Dentre os compostos identificados em menor quantidade, destacou-se, devido a sua natureza química, o composto sulfurado 4,5-de-hidro-2-metil-3(2H-tiofenona. Esta é a primeira vez que este e outros compostos voláteis são reportados em aguardente de cana. Conclui-se que a metodologia empregada neste trabalho permitiu a identificação de compostos voláteis da fração C5-C18, que potencialmente contribuem para o aroma da aguardente de cana.The volatile compounds of Brazilian sugar cane spirit, the fermented and distilled juice of sugar cane, were extracted by dynamic headspace concentration on Tenax-TA trap and analyzed by gas chromatography-mass spectrometry. Approximately 100 volatile compounds with carbon number ranging from 5 to 18 were detected. Among these, 18 esters and 4 compounds from other chemical classes were selected for this work on the basis of their quantity in the extract or their sensory qualities obtained from literature. The major compounds identified were 3-methyl-1-butanol (isoamyl alcohol, 1,1-diethoxy-ethane (acetaldehyde diethyl acetal and the esters 3-methylbutyl acetate, ethyl hexanoate, ethyl octanoate, ethyl decanoate and ethyl dodecanoate. In minor quantities, potentially important aroma compounds

  18. Tank Vapor Characterization Project: Tank 241-S-102 fourth temporal study: Headspace gas and vapor characterization results from samples collected on December 19, 1996

    Energy Technology Data Exchange (ETDEWEB)

    Pool, K.H.; Evans, J.C.; Olsen, K.B.; Hayes, J.C. [and others

    1997-08-01

    This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-S-102 (Tank S-102) at the Hanford Site in Washington State. Tank headspace samples collected by SGN Eurisys Service Corporation (SESC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by SESC. Ammonia was determined to be above the immediate notification limit of 150 ppm as specified by the sampling and analysis plan (SAP). Hydrogen was the principal flammable constituent of the Tank S-102 headspace, determined to be present at approximately 2.410% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <2.973% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <2.973% of the LFL. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in Table S.1. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0.

  19. Potential application of microsensor technology in radioactive waste management with emphasis on headspace gas detection.

    Energy Technology Data Exchange (ETDEWEB)

    Davis, Chad Edward; Thomas, Michael Loren; Wright, Jerome L.; Pohl, Phillip Isabio; Hughes, Robert Clark; Wang, Yifeng; McGrath, Lucas K.; Ho, Clifford Kuofei; Gao, Huizhen

    2004-09-01

    Waste characterization is probably the most costly part of radioactive waste management. An important part of this characterization is the measurements of headspace gas in waste containers in order to demonstrate the compliance with Resource Conservation and Recovery Act (RCRA) or transportation requirements. The traditional chemical analysis methods, which include all steps of gas sampling, sample shipment and laboratory analysis, are expensive and time-consuming as well as increasing worker's exposure to hazardous environments. Therefore, an alternative technique that can provide quick, in-situ, and real-time detections of headspace gas compositions is highly desirable. This report summarizes the results obtained from a Laboratory Directed Research & Development (LDRD) project entitled 'Potential Application of Microsensor Technology in Radioactive Waste Management with Emphasis on Headspace Gas Detection'. The objective of this project is to bridge the technical gap between the current status of microsensor development and the intended applications of these sensors in nuclear waste management. The major results are summarized below: {sm_bullet} A literature review was conducted on the regulatory requirements for headspace gas sampling/analysis in waste characterization and monitoring. The most relevant gaseous species and the related physiochemical environments were identified. It was found that preconcentrators might be needed in order for chemiresistor sensors to meet desired detection {sm_bullet} A long-term stability test was conducted for a polymer-based chemresistor sensor array. Significant drifts were observed over the time duration of one month. Such drifts should be taken into account for long-term in-situ monitoring. {sm_bullet} Several techniques were explored to improve the performance of sensor polymers. It has been demonstrated that freeze deposition of black carbon (CB)-polymer composite can effectively eliminate the so

  20. Analytical performance of three commonly used extraction methods for the gas chromatography-mass spectrometry analysis of wine volatile compounds.

    Science.gov (United States)

    Andujar-Ortiz, I; Moreno-Arribas, M V; Martín-Alvarez, P J; Pozo-Bayón, M A

    2009-10-23

    The analytical performance of three extraction procedures based on cold liquid-liquid extraction using dicloromethane (LLE), solid phase extraction (SPE) using a styrene-divinylbenzene copolymer and headspace solid phase microextraction (SPME) using a carboxen-polydimethylsiloxane coated fibre has been evaluated based on the analysis of 30 representative wine volatile compounds. From the comparison of the three procedures, LLE and SPE showed very good linearity covering a wide range of concentrations of wine volatile compounds, low detection limits, high recovery for most of the volatile compounds under study and higher sensitivity compared to the headspace-SPME procedure. The latter showed in general, poor recovery for polar volatile compounds. Despite some drawbacks associated with the LLE and SPE procedures such as the more tedious sampling treatment and the use of organic solvents, the analytical performance of both procedures showed that they are more adequate for the analysis of wine volatiles.

  1. Simultaneous Determination of Methanol, Ethanol and Formic Acid in Serum and Urine by Headspace GC-FID.

    Science.gov (United States)

    Bursová, Miroslava; Hložek, Tomáš; Čabala, Radomír

    2015-01-01

    A simple, cost-effective headspace gas chromatography (GC) method coupled with GC with flame ionization detection for simultaneous determination of methanol, ethanol and formic acid was developed and validated for clinical and toxicological purposes. Formic acid was derivatized with an excess of isopropanol under acidic conditions to its volatile isopropyl ester while methanol and ethanol remained unchanged. The entire sample preparation procedure is complete within 6 min. The design of the experiment (the face-centered central composite design) was used for finding the optimal conditions for derivatization, headspace sampling and chromatographic separation. The calibration dependences of the method were quadratic in the range from 50 to 5,000 mg/L, with adequate accuracy (89.0-114.4%) and precision (<12%) in the serum. The new method was successfully used for determination of selected analytes in serum samples of intoxicated patients from among those affected by massive methanol poisonings in the Czech Republic in 2012.

  2. Aroma compound analysis of Eruca sativa (Brassicaceae) SPME headspace leaf samples using GC, GC-MS, and olfactometry.

    Science.gov (United States)

    Jirovetz, Leopold; Smith, David; Buchbauer, Gerhard

    2002-07-31

    The aroma compounds of rocket salad (Eruca sativa) SPME headspace samples of fresh leaves were analyzed using GC, GC-MS, and olfactometry. More than 50 constituents of the Eruca headspace could be identified to be essential volatiles, responsible for the characteristic intense green; herbal; nutty and almond-like; Brassicaceae-like (direction of cabbage, broccoli, and mustard); and horseradish-like aroma of these salad leaves. As aroma impact compounds, especially isothiocyanates, and derivatives of butane, hexane, octane, and nonane were identified. 4-Methylthiobutyl isothiocyanate (14.2%), cis-3-hexen-1-ol (11.0%), cis-3-hexenyl butanoate (10.8%), 5-methylthiopentyl isothiocyanate (9.3%), cis-3-hexenyl 2-methylbutanoate (5.4%), and 5-methylthiopentanenitrile (5.0%) were found in concentrations higher than 5.0% (calculated as % peak area of GC analysis using a nonpolar column).

  3. Understanding the role of saliva in aroma release from wine by using static and dynamic headspace conditions.

    Science.gov (United States)

    Muñoz-González, Carolina; Feron, Gilles; Guichard, Elisabeth; Rodríguez-Bencomo, J José; Martín-Álvarez, Pedro J; Moreno-Arribas, M Victoria; Pozo-Bayón, M Ángeles

    2014-08-20

    The aim of this work was to determine the role of saliva in wine aroma release by using static and dynamic headspace conditions. In the latter conditions, two different sampling points (t = 0 and t = 10 min) corresponding with oral (25.5 °C) and postoral phases (36 °C) were monitored. Both methodologies were applied to reconstituted dearomatized white and red wines with different nonvolatile wine matrix compositions and a synthetic wine (without matrix effect). All of the wines had the same ethanol concentration and were spiked with a mixture of 45 aroma compounds covering a wide range of physicochemical characteristics at typical wine concentrations. Two types of saliva (human and artificial) or control samples (water) were added to the wines. The adequacy of the two headspace methodologies for the purposes of the study (repeatability, linear ranges, determination coefficients, etc.) was previously determined. After application of different chemometric analysis (ANOVA, LSD, PCA), results showed a significant effect of saliva on aroma release dependent on saliva type (differences between artificial and human) and on wine matrix using static headspace conditions. Red wines were more affected than white and synthetic wines by saliva, specifically human saliva, which provoked a reduction in aroma release for most of the assayed aroma compounds independent of their chemical structure. The application of dynamic headspace conditions using a saliva bioreactor at the two different sampling points (t = 0 and t = 10 min) showed a lesser but significant effect of saliva than matrix composition and a high influence of temperature (oral and postoral phases) on aroma release.

  4. Rapid Separation of Elemental Species by Fast Multicapillary Gas Chromatography with Multichannel Optical Spectrometry Detection following Headspace Solid Phase Microextraction

    OpenAIRE

    Jacek Giersz; Krzysztof Jankowski; Monika Truskolaska

    2015-01-01

    A method for conducting fast and efficient gas chromatography based on short multicapillaries in straight alignment combined with atomic emission detection was developed for field analysis. The strategy enables for speciation analysis of organometallic compounds. The analytes are simultaneously ethylated and preconcentrated on a solid phase microextraction (SPME) fiber placed in the headspace over the sample for 25 min. The ethylated species are then completely separated and selectively quant...

  5. Direct determination of acrylamide in potato chips by using headspace solid-phase microextraction coupled with gas chromatography-flame ionization detection.

    Science.gov (United States)

    Ghiasvand, Ali Reza; Hajipour, Somayeh

    2016-01-01

    Acrylamide is a potentially toxic and carcinogenic substance present in many high-consumption foods. Recently, this matter has been placed in category of "reasonably anticipated to be a human carcinogen" by National Toxicology Program (NTP). Therefore, simple and cost-effective determination of acrylamide in food samples has attracted intense interest. The most reported techniques for this purpose are GC-MS and LC-MS, which are very expensive and available in few laboratories. In this research, for the first time, a rapid, easy and low-cost method is introduced for sensitive and precise determination of acrylamide in foodstuffs, using gas chromatography-flame ionization detection (GC-FID) system after its direct trapping in the upper atmosphere of samples by headspace solid-phase microextraction (HS-SPME). The effects of main experimental variables were studied and the optimized parameters were obtained as the type of fiber, carboxen/divinylbenzene/polydimethylsiloxane (CAR/DVB/PDMS); extraction time, 30 min; extraction temperature, 60°C; moisture content, 10 µL water per 1g of sample; desorption time, 2 min; and desorption temperature, 230°C. The linear calibration graph was obtained in the range of 0.77-50 µg g(-1), with regression coefficient of 0.998. The detection and quantification limits of the proposed method were 0.22 and 0.77 µg g(-1), respectively. The recoveries, for different food samples, were 79.6-95.7%. The repeatability of measurements, expressed as relative standard deviation (RSD), were found to be 4.1-8.0% (n=9). The proposed HS-SPME-GC-FID method was successfully carried out for quantifying of trace levels of acrylamide in some processed food products (chips and French fries), sold in open local markets.

  6. Orthogonal Design Study on Factors Affecting the Determination of Common Odors in Water Samples by Headspace Solid-Phase Microextraction Coupled to GC/MS

    Directory of Open Access Journals (Sweden)

    Shifu Peng

    2013-01-01

    Full Text Available Geosmin and 2-MIB are responsible for the majority of earthy and musty events related to the drinking water. These two odorants have extremely low odor threshold concentrations at ng L−1 level in the water, so a simple and sensitive method for the analysis of such trace levels was developed by headspace solid-phase microextraction coupled to gas chromatography/mass spectrometry. In this study, the orthogonal experiment design L32 (49 was applied to arrange and optimize experimental conditions. The optimum was the following: temperatures of extraction and desorption, 65°C and 260°C, respectively; times of extraction and desorption, 30 min and 5 min, respectively; ionic strength, 25% (w/v; rotate-speed, 600 rpm; solution pH, 5.0. Under the optimized conditions, limits of detection (S/N=3 were 0.04 and 0.13 ng L−1 for geosmin and 2-MIB, respectively. Calculated calibration curves gave high levels of linearity with a correlation coefficient value of 0.9999 for them. Finally, the proposed method was applied to water samples, which were previously analyzed and confirmed to be free of target analytes. Besides, the proposal method was applied to test environmental water samples. The RSDs were 2.75%~3.80% and 4.35%~7.6% for geosmin and 2-MIB, respectively, and the recoveries were 91%~107% and 91%~104% for geosmin and 2-MIB, respectively.

  7. Orthogonal Design Study on Factors Affecting the Determination of Common Odors in Water Samples by Headspace Solid-Phase Microextraction Coupled to GC/MS.

    Science.gov (United States)

    Peng, Shifu; Ding, Zhen; Xia, Weiwen; Zheng, Hao; Xia, Yuting; Chen, Xiaodong

    2013-01-01

    Geosmin and 2-MIB are responsible for the majority of earthy and musty events related to the drinking water. These two odorants have extremely low odor threshold concentrations at ng L(-1) level in the water, so a simple and sensitive method for the analysis of such trace levels was developed by headspace solid-phase microextraction coupled to gas chromatography/mass spectrometry. In this study, the orthogonal experiment design L32 (4(9)) was applied to arrange and optimize experimental conditions. The optimum was the following: temperatures of extraction and desorption, 65°C and 260°C, respectively; times of extraction and desorption, 30 min and 5 min, respectively; ionic strength, 25% (w/v); rotate-speed, 600 rpm; solution pH, 5.0. Under the optimized conditions, limits of detection (S/N = 3) were 0.04 and 0.13 ng L(-1) for geosmin and 2-MIB, respectively. Calculated calibration curves gave high levels of linearity with a correlation coefficient value of 0.9999 for them. Finally, the proposed method was applied to water samples, which were previously analyzed and confirmed to be free of target analytes. Besides, the proposal method was applied to test environmental water samples. The RSDs were 2.75%~3.80% and 4.35%~7.6% for geosmin and 2-MIB, respectively, and the recoveries were 91%~107% and 91%~104% for geosmin and 2-MIB, respectively.

  8. A salting out system for improving the efficiency of the headspace solid-phase microextraction of short and medium chain free fatty acids.

    Science.gov (United States)

    Fiorini, Dennis; Pacetti, Deborah; Gabbianelli, Rosita; Gabrielli, Serena; Ballini, Roberto

    2015-08-28

    Given the importance of short and medium chain free fatty acids (FFAs) in several fields, this study sought to improve the extraction efficiency of the solid-phase microextraction (SPME) of FFAs by evaluating salting out agents that appear promising for this application. The salts ammonium sulfate ((NH4)2SO4) and sodium dihydrogen phosphate (NaH2PO4) were tried on their own and in combination (3.7/1), in four different total amounts, as salting out agents in the headspace-SPME-gas chromatographic (HS-SPME-GC) analysis of the FFAs from acetic acid (C2) to decanoic acid (C10). Their performance in a model system of an aqueous standard mixture of FFAs at a pH of 3.5 was compared to that of the more commonly used sodium chloride (NaCl) and sodium sulfate (Na2SO4). All of the salts and salt systems evaluated, in proper amount, gave improved results compared to NaCl (saturated), which instead gave interesting results only for the least volatile FFAs C8 and C10. For C2-C6, the salt system that gave the best results compared to NaCl was (NH4)2SO4/NaH2PO4, in the highest of the four amounts evaluated, with factor increases between 1.2 and 4.1-fold, and NaH2PO4, between 1.0 and 4.3-fold. The SPME extraction efficiency given by the mixture (NH4)2SO4/NaH2PO4 was also assessed on biological and food samples, confirming that overall it performed better than NaCl. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Full evaporation headspace gas chromatography for sensitive determination of high boiling point volatile organic compounds in low boiling matrices.

    Science.gov (United States)

    Mana Kialengila, Didi; Wolfs, Kris; Bugalama, John; Van Schepdael, Ann; Adams, Erwin

    2013-11-08

    Determination of volatile organic components (VOC's) is often done by static headspace gas chromatography as this technique is very robust and combines easy sample preparation with good selectivity and low detection limits. This technique is used nowadays in different applications which have in common that they have a dirty matrix which would be problematic in direct injection approaches. Headspace by nature favors the most volatile compounds, avoiding the less volatile to reach the injector and column. As a consequence, determination of a high boiling solvent in a lower boiling matrix becomes challenging. Determination of VOCs like: xylenes, cumene, N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide (DMA), N-methyl-2-pyrrolidone (NMP), 1,3-dimethyl-2-imidazolidinone (DMI), benzyl alcohol (BA) and anisole in water or water soluble products are an interesting example of the arising problems. In this work, a headspace variant called full evaporation technique is worked out and validated for the mentioned solvents. Detection limits below 0.1 μg/vial are reached with RSD values below 10%. Mean recovery values ranged from 92.5 to 110%. The optimized method was applied to determine residual DMSO in a water based cell culture and DMSO and DMA in tetracycline hydrochloride (a water soluble sample). Copyright © 2013 Elsevier B.V. All rights reserved.

  10. [Determination of partition coefficient of dissolved gases in transformer oil using phase ratio variation method and static headspace gas chromatography].

    Science.gov (United States)

    Zhao, Jinghong; Wang, Hailong; Liu, Wenmin; Zhou, Yansheng; Guan, Yafeng

    2004-05-01

    The partition coefficients of dissolved gases in transformer oil were determined using a phase ratio variation method and static headspace gas chromatography (GC). A pressure balancing and gas volume-metering device was connected to the vent of a sample loop on a six-port injection valve of the GC. The gas phase sample from the headspace vial of 25 mL was transferred to an 80 microL sample-loop through a fused silica capillary of 0.53 mm i.d., and then separated and determined quantitatively by GC. A 2 m x 1 mm i.d. GDX502 micro-packed column was used for the separation. Five different gas-liquid volume ratios in the headspace vials were measured at different equilibrium concentrations. The partition coefficients of hydrocarbon gases including methane, acetylene, ethylene, ethane and propane dissolved in transformer oil were determined by using linear regression analysis at 20 degrees C and 50 degrees C separately. The errors between the real values and regression values from experimental data were less than 4.14% except methane. Fundamental data for on-line measurement of dissolved gases in transformer oil are provided by GC.

  11. Volatile compounds in low-acid fermented sausage "espetec" and sliced cooked pork shoulder subjected to high pressure processing. A comparison of dynamic headspace and solid-phase microextraction.

    Science.gov (United States)

    Rivas-Cañedo, Ana; Juez-Ojeda, Cristina; Nuñez, Manuel; Fernández-García, Estrella

    2012-05-01

    Two extraction techniques, dynamic headspace extraction (DHE) and solid-phase microextraction (SPME), were compared to assess the effect of high-pressure treatment (400MPa, 10min, 12°C) on the volatile compounds of low-acid fermented sausage "espetec" and sliced cooked pork shoulder stored at 4°C. DHE was more efficient at extracting low-boiling compounds such as ethanal, 2,3-butanedione and alcohols, while SPME extracted more efficiently a higher number of chemical families, especially fatty acids. The effect of pressurisation on the volatile fraction of "espetec" was better categorized by DHE, whereas SPME was more appropriate for cooked pork shoulder. The volatile fraction of "espetec" changed slightly after pressurisation, mainly showing a decrease in the levels of lipid-derived compounds, like linear alkanes, aldehydes, or 1-alcohols in pressurised samples. The volatile profile of cooked pork shoulder underwent substantial changes during refrigerated storage, mainly due to microbial metabolism, most of these changes being limited by HPP.

  12. Got a Match? Ion Extraction GC-MS Characterization of Accelerants Adsorbed in Charcoal Using Negative Pressure Dynamic Headspace Concentration

    Science.gov (United States)

    Anzivino, Barbara; Tilley, Leon J.; Ingalls, Laura R.; Hall, Adam B.; Drugan, John E.

    2009-01-01

    An undergraduate organic chemistry experiment demonstrating real-life application of GC-MS to arson accelerant identification is described. Students are given the task of comparing a sample recovered from a "crime scene" to that from a "suspect's clothing". Accelerants subjected to different conditions are recovered using a quick and simple…

  13. Aroma Volatile Compound Analysis of SPME Headspace and Extract Samples from Crabapple (Malus sp.) Fruit Using GC-MS

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Volatile compounds from the ripened crabapple fruit of six varieties (Red Splendor, Strawberry Parfait, Pink Spire, Radiant, Sparkler, and Flame) were analyzed by the use of the SPME/GC/MS method. The changes in the volatiles between the ripened and upon full maturity fruit states were studied in Red Splendor and Strawberry Parfait. An effort was made to summarize an effective method for searching and identifying new idioplasms containing a particular fruit aroma within Malus. A total of 37 compounds were identified from the sample. The main aroma volatiles of the six varieties of fruit were comprised of 2-hexenal, 3-hexenal, hexanal, 2,4-hexadienal, benzaldehyde, diethyl phthalate. The main volatile compound of the crabapple fruit was 2-hexenal, but the relative content percentages were different (45.37, 21.98, 33.56, 32.21, 38.60, and 45.88%). The aroma components accumulated differently as the fruits ripened. The relative content of aldehydes and esters decreased as alcohols increased after the Red Splendor and Strawberry Parfait fruit ripened. For Red Splendor, the main volatile was still 2-hexenal, but the relative content decreased to 42.89%, and the relative content of alcohols increased by 13.86% as aldehydes and esters declined by 12.16 and 7.18%, respectively. For Strawberry Parfait, the main volatile was changed to cyclohexanol, and the relative content increased to 46.43%, while the relative content of alcohols increased by 49.03% as aldehydes and esters declined by 23.74 and 9.34%, respectively.

  14. Headspace analysis study of evaporation rate of perfume ingredients applied onto skin.

    Science.gov (United States)

    Vuilleumier, C; Flament, I; Sauvegrain, P

    1995-04-01

    Synopsis Diffusion of perfume ingredients from skin or hair is measured using an original method based on dynamic headspace technology. This has been used for pure odorants, fine fragrances, as well as for perfumed cosmetic applications such as soaps, creams or shampoos, in order to characterize diffusion processes and air/skin or air/hair partitioning. Accordingly, a special collection system, applied on the inner face of the forearm, has been developed, allowing the adsorption of diffusing organic vapours from skin onto Tenax (poly-diphenyl phenylene oxide) with a controlled air flow rate. A simple model composition containing eleven volatile synthetic odorants was prepared in an alcoholic matrix and the solution was applied onto the skin. The diffusion rate of the different components was measured by determining the concentration of each in the gas phase versus time. Conversely, the same experiment was effected by the application of an alcoholic solution of each individual component. In this manner, the relative diffusion from skin of the components alone or mixed was compared using the same experimental technique. The effect of a musky component was also tested. Both compositions (with and without musk) were then applied in a soap base. Thus, following a rigorous protocol, the forearm was washed with the perfumed soap and rinsed with water before collection of the headspace. The results show the different diffusion rates of the individual odorants. In particular, components evaporate slower from the skin when they have been applied from a soap bar compared to when they have been applied from alcoholic solution. We also present results describing the characterization of skin types using a panel comprised of 80 people (40 females and 40 males); amount of sebum, hydration and pH were systematically measured on different parts of the face, the neck as well as the outer and inner faces of the forearm. The panelists were then classified into different sub

  15. Analysis of endogenous aldehydes in human urine by static headspace gas chromatography-mass spectrometry.

    Science.gov (United States)

    Serrano, María; Gallego, Mercedes; Silva, Manuel

    2016-03-11

    Endogenous aldehydes (EAs) generated during oxidative stress and cell processes are associated with many pathogenic and toxicogenic processes. The aim of this research was to develop a solvent-free and automated analytical method for the determination of EAs in human urine using a static headspace generator sampler coupled with gas chromatography-mass spectrometry (HS-GC-MS). Twelve significant EAs used as markers of different biochemical and physiological processes, namely short- and medium-chain alkanals, α,β-unsaturated aldehydes and dicarbonyl aldehydes have been selected as target analytes. Human urine samples (no dilution is required) were derivatized with O-2,3,4,5,6-pentafluorobenzylhydroxylamine in alkaline medium (hydrogen carbonate-carbonate buffer, pH 10.3). The HS-GC-MS method developed renders an efficient tool for the sensitive and precise determination of EAs in human urine with limits of detection from 1 to 15ng/L and relative standard deviations, (RSDs) from 6.0 to 7.9%. Average recoveries by enriching urine samples ranged between 92 and 95%. Aldehydes were readily determined at 0.005-50μg/L levels in human urine from healthy subjects, smokers and diabetic adults.

  16. Determination of ethanol content in medicated syrups by static headspace gas chromatography.

    Science.gov (United States)

    Huzar, Elźbieta; Wodnicka, Alicja

    2013-01-01

    Liquid drug preparations are the most convenient for pediatric patients. Unfortunately, these formulations very often contain ethanol, which may have an impact on children development. Moreover, medicines containing alcohol may cause undesirable interactions in conjunction with other drugs. This work reports complete validated method for the quantitation of ethanol in commercial medicated syrups. For determination of ethanol headspace gas chromatography and different methods of quantitative analysis were used. The analyzed samples of commercial medicated syrups available on the home marked contained from 3.37 to 8.65% (v/v) of ethanol. The estimated theoretical values of blood ethanol concentration for children after single recommended dose ingestion were at least twice lower than 0.125 g/mL. The process of validation showed that the applied GC method is selective, sensitive, linear and precise. The use of internal standard makes it accurate. The developed method could be considered as an analytical tool for the quality control of various liquid drug preparations.

  17. [Simultaneous determination of seven residual solvents in bovis calculus artifactus by headspace gas chromatography].

    Science.gov (United States)

    Chi, Shuyao; Wu, Dike; Sun, Jinhong; Ye, Ruhan; Wang, Xiaoyan

    2014-05-01

    A headspace gas chromatography (HS-GC) method was developed for the simultaneous determination of seven residual solvents (petroleum ether (60-90 degrees C), acetone, ethyl acetate, methanol, methylene chloride, ethanol and butyl acetate) in bovis calculus artifactus. The DB-WAX capillary column and flame ionization detector (FID) were used for the separation and detection of the residual solvents, and the internal standard method was used for the quantification. The chromatographic conditions, such as equilibrium temperature and equilibrium time, were optimized. Under the optimized conditions, all of the seven residual solvents showed good linear relationships with good correlation coefficients (not less than 0.999 3) in the prescribed concentration range. At three spiked levels, the recoveries for the seven residual solvents were 94.7%-105.2% with the relative standard deviations (RSDs) less than 3.5%. The limits of detection (LODs) of the method were 0.43-5.23 mg/L, and the limits of quantification (LOQs) were 1.25-16.67 mg/L. The method is simple, rapid, sensitive and accurate, and is suitable for the simultaneous determination of the seven residual solvents in bovis calculus artifactus.

  18. Headspace Analysis of Philippine Civet Coffee Beans Using Gas Chromatography-Mass Spectrometry and Electronic Nose

    Science.gov (United States)

    Ongo, E.; Sevilla, F.; Antonelli, A.; Sberveglieri, G.; Montevecchi, G.; Sberveglieri, V.; de Paola, E. L.; Concina, I.; Falasconi, M.

    2011-11-01

    Civet coffee, the most expensive and best coffee in the world, is an economically important export product of the Philippines. With a growing threat of food adulteration and counterfeiting, a need for quality authentication is essential to protect the integrity and strong market value of Philippine civet coffee. At present, there is no internationally accepted method of verifying whether a bean is an authentic civet coffee. This study presented a practical and promising approach to identify and establish the headspace qualitative profile of Philippine civet coffee using electronic nose (E-nose) and gas chromatography-mass spectrometry (GC-MS). E-nose analysis revealed that aroma characteristic is one of the most important quality indicators of civet coffee. The findings were supported by GC-MS analysis. Principal component analysis (PCA) exhibited a clearly separated civet coffees from their control beans. The chromatographic fingerprints indicated that civet coffees differed with their control beans in terms of composition and concentration of individual volatile constituents.

  19. Headspace Solid-Phase Microextraction Analysis of Volatile Components in Narcissus tazetta var. chinensis Roem

    Directory of Open Access Journals (Sweden)

    Hai-Shan Chi

    2013-11-01

    Full Text Available The volatile components in single-flowered and double-flowered Chinese narcissus were identified by headspace-solid phase microextraction (HS-SPME coupled with GC and GC/MS. Changes in aroma during the vase-life (days 0, 1, 2, 3, 4, 5 and 6 of two samples were also studied. A total of 35 compounds were identified, of which all were present in single-flowered and 26 in double-flowered samples. The main aroma components were (E-β-ocimene, and benzyl acetate. Single-flowered narcissus have a higher percentage of benzyl acetate, while double-flowered narcissus have a higher percentage of 1,8-cineole. In vase-life, the total volatile component content peaked on day 2 for single-flowered and day 3 for the double-flowered narcissus. For both single-flowered and double-flowered narcissus flowers, the total content of volatile components had decreased significantly by day 4.

  20. Water Determination in Solid Pharmaceutical Products Utilizing Ionic Liquids and Headspace Gas Chromatography.

    Science.gov (United States)

    Frink, Lillian A; Armstrong, Daniel W

    2016-08-01

    A rapid, accurate, and precise headspace gas chromatographic (HSGC) analytical method was developed for the detection and quantification of water in drug products. The analysis is able to be performed in 10 min and automated. The HSGC method used an ionic liquid (IL) based open tubular capillary gas chromatographic column to increase the ruggedness of this method and provide improved peak shapes for water. Due to the ionic liquids low vapor pressure, unique physiochemical properties, and high thermal stability, they also make idea solvents for HSGC. Unlike Karl Fischer titration methods, this HSGC method is not affected by side reactions. The developed method was shown to be broadly applicable. The water content in 12 different samples was found to range from 1%-7% water. The use of HSGC was highly sensitive and only required 10 mg of sample. In addition, it was found to have greater precision and accuracy than Karl Fischer titration and greater precision and speed than loss on drying.

  1. Automated dynamic headspace/GC-MS analyses affect the repeatability of volatiles in irradiated Turkey.

    Science.gov (United States)

    Nam, Ki-Chang; Cordray, Joseph; Ahn, Dong U

    2004-03-24

    Although a dynamic headspace/gas chromatography-mass spectrometry (DH/GC-MS) method is an effective tool for determining volatiles of irradiated turkey meat, the profile of volatiles may be changeable depending upon the availability of oxygen in the sample vial and sample holding time before purge. The objective of this study was to evaluate the effects of helium flushing and sample holding time before purge on the volatiles profiles of irradiated raw and cooked turkey breast meat. Vacuum-packaged turkey breasts were irradiated at 2.5 kGy, and the volatiles of irradiated raw and cooked samples were analyzed using a DH/GC-MS with different holding times up to 280 min. The amounts of dimethyl disulfide and dimethyl trisulfide decreased as sample holding time in an autosampler (4 degrees C) before purge increased, whereas those of aldehdyes increased as holding time increased due to lipid oxidation. Helium flush of sample vials before sample loading on an autosampler retarded lipid oxidation and minimized the changes of sulfur volatiles in raw meat but was not enough to prevent oxidative changes in cooked meat. Although DH/GC-MS is a convenient method for automatic analysis of volatiles in meat samples, the number of samples that can be loaded in an autosampler at a time should be limited within the range that can permit reasonable repeatabilities for target volatile compounds.

  2. Determination of benzene residues in recycled polyethylene terephthalate (PETE) by dynamic headspace-gas chromatography.

    Science.gov (United States)

    Komolprasert, V; Hargraves, W A; Armstrong, D J

    1994-01-01

    A dynamic headspace-gas chromatography (HS/GC) method was developed to quantitate benzene in recycled PETE material derived from 21 PETE beverage bottles. The analytical system consisted of a purge-and-trap apparatus which was interfaced directly with a gas chromatograph/flame ionization detector. Cryofocusing and non-cryofocusing GC systems were used. The technique was applied to spiked PETE test samples which were prepared at various benzene concentrations ranging from 100 ppb to 117 ppm. The initial spiked benzene concentration in the PETE test samples was determined gravimetrically. The HS/GC technique was limited by the slow desorption rate of benzene from the PETE matrix; as a result, multipurges were performed at 60 degrees C. Regression analysis was done on the multipurge data to develop a desorption model which would predict the total amount of benzene in the PETE. The calculated results agreed with the experimental recoveries within +/- 10%. Recovery depended on the initial benzene level in the PETE and ranged from 70 to 90% after the first five purges.

  3. On-matrix derivatization for dynamic headspace sampling of nonvolatile surface residues.

    Science.gov (United States)

    Harvey, Scott D; Wahl, Jon H

    2012-09-21

    The goal of this study is to extend sampling by the field and laboratory emission cell (FLEC) dynamic headspace technique to applications that target nonvolatile residues. On-matrix derivatization of residues to render analytes stable and more volatile is explored to achieve this goal. Results show that on-matrix derivatizations of nerve agent hydrolysis products (monoalkyl methylphosphonic acids and methylphosphonic acid [MPA]) with diazomethane were successful on glass and painted wallboard (at the 10-μg level). It also was successful on the more difficult concrete (at the 500-μg level) and carpet (at the 20-μg level), substrates that cannot be successfully sampled using swipe techniques. Analysis of additional chemical warfare (CW)-associated residues can be approached by on-matrix derivatization with trifluoroacetic anhydride (TFAA). For example, amines (used as stabilizers or present as decomposition products of the nerve agent VX) or thiodiglycol (hydrolysis product of sulfur mustard) could be sampled as their TFAA derivatives from glass, painted wallboard, and concrete (at the 40-μg level), as well as carpet (at the 80-μg level) surfaces. Although the amine and thiodiglycol are semi-volatile and could be sampled directly, derivatization improves the recovery and chromatographic behavior of these analytes.

  4. Rapid analysis of the essential oil components of dried Zanthoxylum bungeanum Maxim by Fe2O3-magnetic-microsphere-assisted microwave distillation and simultaneous headspace single-drop microextraction followed by GC-MS.

    Science.gov (United States)

    Ye, Qing

    2013-06-01

    In this work, microwave distillation assisted by Fe2 O3 magnetic microspheres (FMMS) and headspace single-drop microextraction were combined, and developed for determination of essential oil compounds in dried Zanthoxylum bungeanum Maxim (ZBM). The FMMS were used as microwave absorption solid medium for dry distillation of dried ZBM. Using the proposed method, isolation, extraction, and concentration of essential oil compounds can be carried out in a single step. The experimental parameters including extraction solvent, solvent volume, microwave power, irradiation time, and the amount of added FMMS, were studied. The optimal analytical conditions were: 2.0 μL decane as the extraction solvent, microwave power of 300 W, irradiation time of 2 min, and the addition of 0.1 g FMMS to ZBM. The method precision was from 4 to 10%. A total of 52 compounds were identified by the proposed method. The conventional steam distillation method was also used for the analysis of essential oil in dried ZBM and only 31 compounds were identified by steam distillation method. It was found that the proposed method is a simple, rapid, reliable, and solvent-free technique for the determination of volatile compounds in Chinese herbs. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Rapid and sensitive analysis of polychlorinated biphenyls and acrylamide in food samples using ionic liquid-based in situ dispersive liquid-liquid microextraction coupled to headspace gas chromatography.

    Science.gov (United States)

    Zhang, Cheng; Cagliero, Cecilia; Pierson, Stephen A; Anderson, Jared L

    2017-01-20

    A simple and rapid ionic liquid (IL)-based in situ dispersive liquid-liquid microextraction (DLLME) method was developed and coupled to headspace gas chromatography (HS-GC) employing electron capture (ECD) and mass spectrometry (MS) detection for the analysis of polychlorinated biphenyls (PCBs) and acrylamide at trace levels from milk and coffee samples. The chemical structures of the halide-based ILs were tailored by introducing various functional groups to the cations to evaluate the effect of different structural features on the extraction efficiency of the target analytes. Extraction parameters including the molar ratio of IL to metathesis reagent and IL mass were optimized. The effects of HS oven temperature and the HS sample vial volume on the analyte response were also evaluated. The optimized in situ DLLME method exhibited good analytical precision, good linearity, and provided detection limits down to the low ppt level for PCBs and the low ppb level for acrylamide in aqueous samples. The matrix-compatibility of the developed method was also established by quantifying acrylamide in brewed coffee samples. This method is much simpler and faster compared to previously reported GC-MS methods using solid-phase microextraction (SPME) for the extraction/preconcentration of PCBs and acrylamide from complex food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Effects of gas composition in headspace and bicarbonate concentrations in media on gas and methane production, degradability, and rumen fermentation using in vitro gas production techniques.

    Science.gov (United States)

    Patra, Amlan Kumar; Yu, Zhongtang

    2013-07-01

    Headspace gas composition and bicarbonate concentrations in media can affect methane production and other characteristics of rumen fermentation in in vitro gas production systems, but these 2 important factors have not been evaluated systematically. In this study, these 2 factors were investigated with respect to gas and methane production, in vitro digestibility of feed substrate, and volatile fatty acid (VFA) profile using in vitro gas production techniques. Three headspace gas compositions (N2+ CO2+ H2 in the ratio of 90:5:5, CO2, and N2) with 2 substrate types (alfalfa hay only, and alfalfa hay and a concentrate mixture in a 50:50 ratio) in a 3×2 factorial design (experiment 1) and 3 headspace compositions (N2, N2 + CO2 in a 50:50 ratio, and CO2) with 3 bicarbonate concentrations (80, 100, and 120 mM) in a 3×3 factorial design (experiment 2) were evaluated. In experiment 1, total gas production (TGP) and net gas production (NGP) was the lowest for CO2, followed by N2, and then the gas mixture. Methane concentration in headspace gas after fermentation was greater for CO2 than for N2 and the gas mixture, whereas total methane production (TMP) and net methane production (NMP) were the greatest for CO2, followed by the gas mixture, and then N2. Headspace composition did not affect in vitro digestibility or the VFA profile, except molar percentages of propionate, which were greater for CO2 and N2 than for the gas mixture. Methane concentration in headspace gas, TGP, and NGP were affected by the interaction of headspace gas composition and substrate type. In experiment 2, increasing concentrations of CO2 in the headspace decreased TGP and NGP quadratically, but increased the concentrations of methane, NMP, and in vitro fiber digestibility linearly, and TMP quadratically. Fiber digestibility, TGP, and NGP increased linearly with increasing bicarbonate concentrations in the medium. Concentrations of methane and NMP were unaffected by bicarbonate concentration, but

  7. Tank 241-BX-104 fourth temporal study: Headspace gas and vapor characterization results from samples collected on April 7, 1997. Tank vapor characterization project

    Energy Technology Data Exchange (ETDEWEB)

    Mitroshkov, A.V.; Hayes, J.C.; Evans, J.C. [and others

    1997-09-01

    This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-BX-04 (Tank BX-104) at the Hanford Site in Washington State. Tank headspace samples collected by SGN Eurisys Service Corporation (SESC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by SESC. Ammonia was determined to be above the immediate notification limit specified by the sampling and analysis plan (SAP). Hydrogen was the principal flammable constituent of the Tank BX-104 headspace, determined to be present at approximately 0.208% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <0.536% of the LFL. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in Table S.1. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0.

  8. Tank 241-BY-108 fifth temporal study: Headspace gas and vapor characterization results from samples collected on January 30, 1997. Tank vapor characterization project

    Energy Technology Data Exchange (ETDEWEB)

    Evans, J.C.; Pool, K.H.; Olsen, K.B. [and others

    1997-09-01

    This report presents the results from analyses of samples taken from tile headspace of waste storage tank 241-B-108 (Tank BY - 108) at the Hanford Site in Washington State. Tank headspace samples collected by SGN Eurisys Services Corporation (SESC) and analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by SESC. Ammonia was determined to be above the immediate notification limit of 150 ppm specified by the sampling and analysis plan (SAP). Hydrogen was the principal flammable constituent of the Tank BY-108 headspace, determined to be present at approximately 0.888% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <1.979% of tile LFL. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in Table S.1. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0.

  9. Tank vapor characterization project: Tank 241-S-102 temporal study headspace gas and vapor characterization results from samples collected on September 19, 1996

    Energy Technology Data Exchange (ETDEWEB)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.; Sklarew, D.S. [and others

    1997-08-01

    This report presents the results from analysis of samples taken from the headspace of waste storage tank 241-S-102 (Tank S-102) at the Hanford Site in Washington State. Tank headspace samples collected by Westinghouse Hanford Company (WHC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by WHC. Ammonia was determined to be above the immediate notification limit of 150 ppm as specified by the sampling and analysis plan (SAP). Hydrogen was the principal flammable constituent of the Tank S-102 headspace, determined to be present at approximately 2.948% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <3.659% of the LFL. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in Tables S.1. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0.

  10. Tank vapor characterization project: Tank 241-BX-104 fifth temporal study: Headspace gas and vapor characterization results from samples collected on June 10, 1997

    Energy Technology Data Exchange (ETDEWEB)

    Hayes, J.C.; Pool, K.H.; Evans, J.C.; Olsen, K.B. [and others

    1997-07-01

    This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-BX-104 (Tank BX-104) at the Hanford Site in Washington State. Tank headspace samples collected by SGN Eurisys Service Corporation (SESC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by SESC. Ammonia was determined to be above the immediate notification limit specified by the sampling and analysis plan (SAP). Hydrogen was the principal flammable constituent of the Tank BX-104 headspace, determined to be present at approximately 0.270% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <0.675% of the LFL. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in Table S.1. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0.

  11. Tank 241-BY-108 fourth temporal study: Headspace gas and vapor characterization results from samples collected on November 14, 1997. Tank vapor characterization project

    Energy Technology Data Exchange (ETDEWEB)

    Evans, J.C.; Pool, K.H.; Olsen, K.B. [and others

    1997-07-01

    This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-BY-108 (Tank BY-108) at the Hanford Site in Washington State. Tank headspace samples collected by SGN Eurisys Service Corporation (SESC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected nonradioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by SESC. Ammonia was determined to be above the immediate notification limit of 150 ppm specified by the sampling and analysis plan (SAP). Hydrogen was the principal flammable constituent of the Tank BY-108 headspace, determined to be present at approximately 1.390% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <2.830% of the LFL. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in Table S.1. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0.

  12. Tank Vapor Characterization Project: Tank 241-BX-103 headspace gas and vapor characterization results from samples collected on August 1, 1996

    Energy Technology Data Exchange (ETDEWEB)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.; Sklarew, D.S.; Edwards, J.A. [and others

    1997-08-01

    This report presents the results from analyses of samples taken from headspace of waste storage tank 241-BX-103 (Tank BX-103) at the Hanford Site in Washington State. Tank headspace samples collected by Westinghouse Hanford Company (WHC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by WHC. No analytes were determined to be above the immediate notification limits specified by the sampling and analysis plan (SAP). Hydrogen was the principal flammable constitu