WorldWideScience

Sample records for spme headspace analysis

  1. 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.

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

    OpenAIRE

    Kateb, Huda al; Costello, Ben de Lacy

    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 ide...

  3. Freeze-thaw method improves the detection of volatile compounds in insects using Headspace Solid-Phase Microextraction (HS-SPME)

    Science.gov (United States)

    Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography–mass spectrometry (GC-MS) is commonly used in analyzing insect volatiles. In order to improve the detection of volatiles in insects, a freeze-thaw method was applied to insect samples before the HS-SPME-GC-MS analysis. ...

  4. Use of headspace SPME-GC-MS for the analysis of the volatiles produced by indoor molds grown on different substrates.

    Science.gov (United States)

    Van Lancker, Fien; Adams, An; Delmulle, Barbara; De Saeger, Sarah; Moretti, Antonio; Van Peteghem, Carlos; De Kimpe, Norbert

    2008-10-01

    An automated headspace solid phase microextraction method followed by GC-MS analysis was used to evaluate and compare the in vitro production of microbial volatile organic compounds (MVOCs) on malt extract agar, plasterboard and wallpaper. Five fungal strains were isolated from the walls of water-damaged houses and identified. In addition, four other common molds were studied. In general, MVOC production was the highest on malt extract agar. On this synthetic medium, molds typically produced 2-methylpropanol, 2-methylbutanol and 3-methylbutanol. On wallpaper, mainly 2-ethylhexanol, methyl 2-ethylhexanoate and compounds of the C8-complex such as 1-octene-3-ol, 3-octanone, 3-octanol and 1,3-octadiene were detected. The detection of 2-ethylhexanol and methyl 2-ethylhexanoate indicates an enhanced degradation of the substrate by most fungi. For growth on plasterboard, no typical metabolites were detected. Despite these metabolite differences on malt extract agar, wallpaper and plasterboard, some molds also produced specific compounds independently of the used substrate, such as trichodiene from Fusarium sporotrichioides and aristolochene from Penicillium roqueforti. Therefore, these metabolites can be used as markers for the identification and maybe also mycotoxin production of these molds. All five investigated Penicillium spp. in this study were able to produce two specific diterpenes, which were not produced by the other species studied. These two compounds, which remain unidentified until now, therefore seem specific for Penicillium spp. and are potentially interesting for the monitoring of this fungal genus. Further experiments will be performed with other Penicillium spp. to study the possibility that these two compounds are specific for this group of molds.

  5. 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.)

  6. Determination of organotin compounds by headspace solid-phase microextraction-gas chromatography-pulsed flame-photometric detection (HS-SPME-GC-PFPD).

    Science.gov (United States)

    Bravo, Manuel; Lespes, Gaëtane; De Gregori, Ida; Pinochet, Hugo; Gautier, Martine Potin

    2005-12-01

    A method based on Headspace solid-phase microextraction (HS-SPME, with a 100 mum 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(-1) in water and close to ng (Sn) kg(-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.

  7. 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.

  8. 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 ......-SPME has a great potential use in the analysis of biogenic VOC emissions, including chemotaxonomical studies....

  9. A Headspace Solid Phase Microextraction (HS-SPME method for the chromatographic determination of alkylpyrazines in cocoa samples

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    Pini Gláucia F.

    2004-01-01

    Full Text Available A Headspace Solid Phase Microextraction (HS-SPME procedure for isolation and determination of alkylpyrazines in cocoa liquor, using Gas Chromatography with Flame Ionization Detection (GC-FID for the separation and detection of the analytes, is presented here. The HS-SPME operational conditions were optimized using extractions of samples spiked with known amounts of alkylpyrazines typically found on cocoa products. The maximum extraction efficiency was obtained using SPME fibers coated with 65 µm Carbowax/divinylbenzene. Additionally, the best results were achieved with extraction temperature of 60 ºC, 15 min of sample/headspace equilibration time and 45 min extraction time. It was also observed that suspending the samples in saturated aqueous NaCl solution during extractions resulted in a significant increment on the peak areas. This procedure was found to be effective to determine the so-called pyrazinic ratios (quotient between peak areas of alkylpyrazines, which are useful as quality parameters for cocoa liquor.

  10. Screening of transformation products in soils contaminated with unsymmetrical dimethylhydrazine using headspace SPME and GC-MS

    NARCIS (Netherlands)

    Kenessov, B.N.; Koziel, J.A.; Grotenhuis, J.T.C.; Carlsen, L.

    2010-01-01

    The paper describes a novel SPME-based approach for sampling and analysis of transformation products of highly reactive and toxic unsymmetrical dimethylhydrazine (UDMH) which is used as a fuel in many Russian, European, Indian, and Chinese heavy cargo carrier rockets. The effects of several

  11. Comparative analysis of the aroma chemicals of Melissa officinalis using hydrodistillation and HS-SPME techniques

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    Shakeel-u- Rehman

    2017-05-01

    Full Text Available Headspace solid-phase micro extraction (HS-SPME coupled with gas chromatography–mass spectrometry (GC–MS has been used for the chemical analysis of Melissa officinalis (leaves cultivated in Institute Germplasm. The HS-SPME analysis led to the identification of 22 components constituting 99.1% of the total volatile constituents present in the leaves whereas its hydrodistillate led to the identification of 24 volatile constituents constituting 98.1% of the volatile material. The chemical composition of the SPME and hydrodistilled extract of M. officinalis leaves comprised mainly of oxygenated monoterpenes (78.5% and 57.8% respectively and sesquiterpene hydrocarbons (14.9% and 29.7% respectively. The major components identified in the HS-SPME extract were citronellal (31.1%, citronellol (18.3%, β-caryophyllene (12.0%, (E-citral (11.9%, (Z-citral (9.6%, geraniol (3.6%, (Z-β-ocimene (3.1% and 1-octen-3-ol (2.0% whereas hydrodistilled essential oil was rich in (Z-citral (19.6%, β-caryophyllene (13.2%, (E-citral (11.2%, citronellal (10.2%, germacrene-d (8.3%, δ-3-carene (5.0%, 6-methyl-5-hepten-2-one (3.7% and citronellyl acetate (3.7%. The comparative analysis of volatile constituents of M. officinalis leaf extract using HS-SPME and hydrodistillation techniques shows both qualitative as well as quantitative differences. The current study is the first report involving rapid analysis of volatile components of M. officinalis by HS-SPME.

  12. Headspace solid-phase microextraction procedures for gas chromatographic analysis of biological fluids and materials.

    Science.gov (United States)

    Mills, G A; Walker, V

    2000-12-01

    Solid-phase microextraction (SPME) is a new solventless sample preparation technique that is finding wide usage. This review provides updated information on headspace SPME with gas chromatographic separation for the extraction and measurement of volatile and semivolatile analytes in biological fluids and materials. Firstly the background to the technique is given in terms of apparatus, fibres used, extraction conditions and derivatisation procedures. Then the different matrices, urine, blood, faeces, breast milk, hair, breath and saliva are considered separately. For each, methods appropriate for the analysis of drugs and metabolites, solvents and chemicals, anaesthetics, pesticides, organometallics and endogenous compounds are reviewed and the main experimental conditions outlined with specific examples. Then finally, the future potential of SPME for the analysis of biological samples in terms of the development of new devices and fibre chemistries and its coupling with high-performance liquid chromatography is discussed.

  13. Determination of different recreational drugs in sweat by headspace solid-phase microextraction gas chromatography mass spectrometry (HS-SPME GC/MS): Application to drugged drivers.

    Science.gov (United States)

    Gentili, Stefano; Mortali, Claudia; Mastrobattista, Luisa; Berretta, Paolo; Zaami, Simona

    2016-09-10

    A procedure based on headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography/mass spectrometry (GC/MS) has been developed for the determination of most commonly used drugs of abuse in sweat of drivers stopped during roadside controls. DrugWipe 5A sweat screening device was used to collect sweat by a specific pad rubbed gently over forehead skin surface. The procedure involved an acid hydrolysis, a HS-SPME extraction for drugs of abuse but Δ(9)-tetrahydrocannabinol, which was directly extracted in alkaline medium HS-SPME conditions, a GC separation of analytes by a capillary column and MS detection by electron impact ionisation. The method was linear from the limit of quantification (LOQ) to 50ng drug per pad (r(2)≥0.99), with an intra- and inter-assay precision and accuracy always less than 15% and an analytical recovery between 95.1% and 102.8%, depending on the considered analyte. Using the validated method, sweat from 60 apparently intoxicated drivers were found positive to one or more drugs of abuse, showing sweat patches testing as a viable economic and simple alternative to conventional (blood and/or urine) and non conventional (oral fluid) testing of drugs of abuse in drugged drivers. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Headspace solid-phase microextraction (HS-SPME) combined with GC-MS as a process analytical technology (PAT) tool for monitoring the cultivation of C. tetani.

    Science.gov (United States)

    Ghader, Masoud; Shokoufi, Nader; Es-Haghi, Ali; Kargosha, Kazem

    2018-02-06

    Vaccine production is a biological process in which variation in time and output is inevitable. Thus, the application of Process Analytical Technologies (PAT) will be important in this regard. Headspace solid - phase microextraction (HS-SPME) coupled with GC-MS can be used as a PAT for process monitoring. This method is suitable to chemical profiling of volatile organic compounds (VOCs) emitted from microorganisms. Tetanus is a lethal disease caused by Clostridium tetani (C. tetani) bacterium and vaccination is an ultimate way to prevent this disease. In this paper, SPME fiber was used for the investigation of VOCs emerging from C. tetani during cultivation. Different types of VOCs such as sulfur-containing compounds were identified and some of them were selected as biomarkers for bioreactor monitoring during vaccine production. In the second step, the portable dynamic air sampling (PDAS) device was used as an interface for sampling VOCs by SPME fibers. The sampling procedure was optimized by face-centered central composite design (FC-CCD). The optimized sampling time and inlet gas flow rates were 10 min and 2 m L s -1 , respectively. PDAS was mounted in exhausted gas line of bioreactor and 42 samples of VOCs were prepared by SPME fibers in 7 days during incubation. Simultaneously, pH and optical density (OD) were evaluated to cultivation process which showed good correlations with the identified VOCs (>80%). This method could be used for VOCs sampling from off-gas of a bioreactor to monitoring of the cultivation process. Copyright © 2018. Published by Elsevier B.V.

  15. Analysis of volatile compositions of Magnolia biondii pamp by steam distillation and headspace solid phase micro-extraction.

    Science.gov (United States)

    Zeng, Zhi; Xie, Runqian; Zhang, Tao; Zhang, Han; Chen, Jie Yu

    2011-01-01

    The chemical compositions of volatile components from Magnolia biondii Pamp were determined by steam distillation (SD) and headspace solid phase micro-extraction (HS-SPME) followed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) analysis. Fifty-six compounds were identified and the major volatile components were d-camphor (0.18-43.26%), 1,8-cineol (13.23-38.02%), α-terpineol (6.57-12.29%) and α-cadinene (5.53-15.15%). The comparison of the volatile components from M. biondii Pamp harvested in three regions of China was investigated. Also, the comparison of volatile components by SD and HS-SPME methods in term of isolation time, plant-consuming and chemical compositions was discussed as well. The percentages of the volatile components by HS-SPME method were found to be large difference from the corresponding one by SD method. HS-SPME technique was much faster than SD (60 min (HS-SPME)/420 min (SD)). Although the aromatic profiles between HS-SPME and SD methods showed several quantitative differences, HS-SPME may be applied routinely to analyze aromatic and medicinal plants.

  16. Influence of fibre coating in headspace solid-phase microextraction-gas chromatographic analysis of aromatic and medicinal plants.

    Science.gov (United States)

    Bicchi, C; Drigo, S; Rubiolo, P

    2000-09-15

    Solid-phase microextraction (SPME) is a solvent-free technique, which is well established in headspace analysis since it is sensitive, because of the concentration factor achieved by the fibres, and selective, because of different coating materials which can be used. The performance of eight commercially available SPME fibres was compared to evaluate the recoveries of some characteristic components with different polarities and structures present in the headspace of four aromatic and medicinal plants: rosemary (Rosmarinus officinalis L.), sage (Salvia officinalis L.), thyme (Thymus vulgaris L.) and valerian (Valeriana officinalis L.). The relative concentration capacity of each fibre on the same components of each plant was also determined by comparing their abundance with that obtained by classical static-headspace GC. The partition coefficient, K1, between the headspace gaseous phase and SPME polymeric coating, and the relative concentration factors, of some of the characteristic components of the plant investigated dissolved in dibutyl phtalate, were also determined, under rigorously standardised analysis conditions. The results showed that the most effective fibres were those consisting of two components, i.e., a liquid phase (polydimethylsiloxane) and a porous solid (carboxen or divinylbenzene, or both).

  17. HS-SPME-GC-MS ANALYSIS OF VOLATILE AND SEMI-VOLATILE COMPOUNDS FROM DRIED LEAVES OF Mikania glomerata Sprengel

    Directory of Open Access Journals (Sweden)

    Esmeraldo A. Cappelaro

    2015-03-01

    Full Text Available This paper reports on the identification of volatile and semi-volatile compounds and a comparison of the chromatographic profiles obtained by Headspace Solid-Phase Microextraction/Gas Chromatography with Mass Spectrometry detection (HS-SPME-GC-MS of dried leaves of Mikania glomerata Sprengel (Asteraceae, also known as 'guaco.' Three different types of commercial SPME fibers were tested: polydimethylsiloxane (PDMS, polydimethylsiloxane/divinylbenzene (PDMS/DVB and polyacrylate (PA. Fifty-nine compounds were fully identified by HS-SPME-HRGC-MS, including coumarin, a marker for the quality control of guaco-based phytomedicines; most of the other identified compounds were mono- and sesquiterpenes. PA fibers performed better in the analysis of coumarin, while PDMS-DVB proved to be the best choice for a general and non-selective analysis of volatile and semi-volatile guaco-based compounds. The SPME method is faster and requires a smaller sample than conventional hydrodistillation of essential oils, providing a general overview of the volatile and semi-volatile compounds of M. glomerata.

  18. Analysis of organic micropollutants in drinking water using SPME and GC-MS

    International Nuclear Information System (INIS)

    Guidotti, M.; Ravaioli, G.

    1999-01-01

    In this work the purpose was to develop accurate and reproducible methods for the qualitative and quantitative analysis of pesticides/herbicides, phthalates, chlorinated solvents, trihalomethanes, polycyclic aromatic hydrocarbons (PAHs) and chlorophenols in drinking waters, using solid-phase micro extraction and GC-MS techniques. The SPME developed by J. Pawliszyn and co-workers, consists of an fused silica fibre, coated with an appropriate absorbent phase, hosted inside the needle of a holder that looks like a GC-syringe; the needle pierces the septum of a sealed vial and the fibre is lowered, by depressing the plunger of the holder, into the liquid (or in the headspace, if that is the case) that contains the analytes of interest. After a set period of time, necessary to reach the partitioning equilibrium, the fibre is retracted inside the needle, the needle is inserted into the GC injector port and the fibre pushed in the heated injector. Here the compounds of interest (that have adsorbed onto the fibre) are thermally desorbed and analysed by GC-MS. After three minutes the fibre is extracted and is ready for a new analysis. The SPME technique has already found many applications in food and environmental analysis. Many of the analytes investigated in this research are listed Italian legislation as possible pollutants of drinking waters and their presence and concentrations require monitoring. The list of compounds included in this work is reported in Table 1

  19. MQ NMR and SPME analysis of nonlinearity in the degradation of a filled silicone elastomer

    Energy Technology Data Exchange (ETDEWEB)

    Chinn, S C; Alviso, C T; Berman, E S; Harvey, C A; Maxwell, R S; Wilson, T S; Cohenour, R; Saalwachter, K; Chasse, W

    2008-10-10

    Radiation induced degradation of polymeric materials occurs via numerous, simultaneous, competing chemical reactions. Though degradation is typically found to be linear in adsorbed dose, some silicone materials exhibit non-linear dose dependence due to dose dependent dominant degradation pathways. We have characterized the effects of radiative and thermal degradation on a model filled-PDMS system, Sylgard 184 (commonly used as an electronic encapsulant and in biomedical applications), using traditional mechanical testing, NMR spectroscopy, and sample headspace analysis using Solid Phase Micro-Extraction (SPME) followed by Gas Chromatography/Mass Spectrometry (GC/MS). The mechanical data and {sup 1}H spin-echo NMR indicated that radiation exposure leads to predominantly crosslinking over the cumulative dose range studies (0 to 250 kGray) with a rate roughly linear with dose. {sup 1}H Multiple Quantum NMR detected a bimodal distribution in the network structure, as expected by the proposed structure of Sylgard 184. The MQ-NMR further indicated that the radiation induced structural changes were not linear in adsorbed dose and competing chain scission mechanisms contribute more largely to the overall degradation process in the range of 50 -100 kGray (though crosslinking still dominates). The SPME-GC/MS data were analyzed using Principal Component Analysis (PCA), which identified subtle changes in the distributions of degradation products (the cyclic siloxanes and other components of the material) as a function of age that provide insight into the dominant degradation pathways at low and high adsorbed dose.

  20. 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.

  1. Volatiles and primary metabolites profiling in two Hibiscus sabdariffa (roselle) cultivars via headspace SPME-GC-MS and chemometrics.

    Science.gov (United States)

    Farag, Mohamed A; Rasheed, Dalia M; Kamal, Islam M

    2015-12-01

    Hibiscus sabdariffa (roselle) is a plant of considerable commercial importance worldwide as functional food due to its organic acids, mucilage, anthocyanins, macro and micro-nutrients content. Although Hibiscus flowers are emerging as very competitive targets for phytochemical studies, very little is known about their volatile composition and or aroma, such knowledge can be suspected to be relevant for understanding its olfactory and taste properties. To provide insight into Hibiscus flower aroma composition and for its future use in food and or pharmaceutical industry, volatile constituents from 2 cultivars grown in Egypt, viz. Aswan and Sudan-1 were profiled using solid-phase microextraction (SPME) coupled to GCMS. A total of 104 volatiles were identified with sugar and fatty acid derived volatiles amounting for the major volatile classes. To reveal for cultivar effect on volatile composition in an untargeted manner, multivariate data analysis was applied. Orthogonal projection to latent structures-discriminant analysis (OPLS-DA) revealed for 1-octen-3-ol versus furfural/acetic acid enrichment in Aswan and Sudan-1 cvs., respectively. Primary metabolites contributing to roselle taste and nutritional value viz. sugars and organic acids were profiled using GC-MS after silylation. The impact of probiotic bacteria on roselle infusion aroma profile was further assessed and revealed for the increase in furfural production with Lactobacillus plantarum inoculation and without affecting its anthocyanin content. This study provides the most complete map for volatiles, sugars and organic acids distribution in two Hibiscus flower cultivars and its fermented product. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

    Science.gov (United States)

    Xie, Wei-Qi; Chai, Xin-Sheng

    2017-05-01

    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. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. 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.

  4. Degradation product emission from historic and modern books by headspace SPME/GC-MS: evaluation of lipid oxidation and cellulose hydrolysis.

    Science.gov (United States)

    Clark, Andrew J; Calvillo, Jesse L; Roosa, Mark S; Green, David B; Ganske, Jane A

    2011-04-01

    Volatile organic compounds emitted from a several decade series of bound periodicals (1859-1939) printed on ground wood paper, as well as historical books dating from the 1500s to early 1800s made from cotton/linen rag, were studied using an improved headspace SPME/GC-MS method. The headspace over the naturally aging books, stored upright in glass chambers, was monitored over a 24-h period, enabling the identification of a wide range of organic compounds emanating from the whole of the book. The detection of particular straight chain aldehydes, as well as characteristic alcohols, alkenes and ketones is correlated with oxidative degradation of the C(18) fatty acid constituency of paper. The relative importance of hydrolytic and oxidative chemistry involved in paper aging in books published between 1560 and 1939 was examined by comparing the relative abundances of furfural (FUR) a known cellulose hydrolysis product, and straight chain aldehydes (SCA) produced from the oxidation of fatty acids in paper. The relative abundance of furfural is shown to increase across the 379-year publication time span. A comparison of relative SCA peak areas across the series of books examined reveals that SCA emission is more important in the cotton/linen rag books than in the ground wood books.

  5. Headspace sorptive solid phase microextraction (HS-SPME) combined with a spectrophotometry system: A simple glass devise for extraction and simultaneous determination of cyanide and thiocyanate in environmental and biological samples.

    Science.gov (United States)

    Al-Saidi, H M; Al-Harbi, Sami A; Aljuhani, E H; El-Shahawi, M S

    2016-10-01

    A simple, low cost and efficient headspace sorptive solid phase microextraction (HS-SPME) method for determination of cyanide has been developed. The system comprises of a glass tube with two valves and a moveable glass slide fixed at its centre. It includes an acceptor phase polyurethane foam treated mercury (II) dithizonate [Hg(HDz)2-PUF] complex fixed inside by a septum cap in a cylindrical configuration (5.0cm length and 1.0cm diameter). The extraction is based upon the contact of the acceptor phase to the headspace and subsequently measuring the absorbance of the recovered mercury (II) dithizonate from PUFs sorbent. Unlike other HSSE, extraction and back - extractions was carried out in a closed system, thereby improving the analytical performance by preventing the analyte loss. Under the optimized conditions, a linear calibration plot in the range of 1.0-50.0µmolL(-1) was achieved with limits of detection (LOD) and quantification (LOQ) of 0.34, 1.2µmolL(-1) CN(-), respectively. Simultaneous analysis of cyanide and thiocyanate in saliva was also performed with satisfactory recoveries. Copyright © 2016. Published by Elsevier B.V.

  6. Microwave-assisted headspace solid-phase microextraction for the analysis of bioemissions from Eucalyptus citriodora leaves.

    Science.gov (United States)

    Xiong, Guohua; Goodridge, Carolyn; Wang, Limei; Chen, Yong; Pawliszyn, Janusz

    2003-12-31

    Microwave-assisted headspace solid-phase microextraction (MA-HS-SPME) was developed as a simple and effective method for fast sampling of volatile organic compounds (VOCs) from Eucalyptus citriodora Hook (E. citriodora) leaves. During microwave heating, a simple shielding device made of aluminum foil was used to protect the SPME fiber from microwave irradiation while allowing the sample to be heated. A room temperature water bath was also used to allow microwave heating to be conducted in a more controlled manner. The inner heating caused by microwave irradiation dramatically accelerated the emission of VOCs from the sample, but no marked change in headspace temperature in the sample vial was found. Under optimum conditions, the extraction efficiencies obtained with microwave heating were much higher than those obtained without microwave heating for all fibers used, namely, 7-microm polydimethylsiloxane (PDMS), 100-microm polydimethylsiloxane (PDMS), 65-microm polydimethylsiloxane/divinylbenzene (PDMS/DVB), and 75-microm carboxen/polydimethylsiloxane (CAR/PDMS). The improvement of extraction efficiency using MA-HS-SPME allowed more VOC events to be detected, with more balanced extraction of VOCs of lower and higher molecular masses. Moreover, a good linear relationship was found between sample size and GC-FID response (total peak area of VOCs), indicating the usefulness of MA-HS-SPME for quantitative analysis of individual volatile compounds in E. citriodora leaves.

  7. Headspace Analysis of Ammonium Nitrate

    Science.gov (United States)

    2017-01-25

    explosives. Trac-Trends in Analytical Chemistry 2013, 42, 35-48. 3. Steinkamp, F. L.; Giordano, B.; Collins, G.; Rose-Pehrsson, S., Volatile...Ambient Air. Analytical Chemistry 1982, 54 (3), 358-364. 5. Field, C. R.; Giordano, B. C.; Rogers, D. A.; Lubrano, A. L.; Rose-Pehrsson, S. L... Analytical Chemistry 1973, 45 (6), 936-943. 8. Cody, R. B.; Laramee, J. A.; Durst, H. D., Versatile new ion source for the analysis of materials in open

  8. Comparative Analyses of the Volatile Components of Citrus Aurantium L. Flowers Using Ultrasonic-Assisted Headspace SPME and Hydrodistillation Combined with GC-MS and Evaluation of their Antimicrobial Activities

    Directory of Open Access Journals (Sweden)

    Akram Rahimi

    2014-12-01

    Full Text Available The volatile components of Citrus aurantium L. flowers were characterized by GC-MS with two different extraction techniques, hydrodistillation (HD and ultrasonic-assisted headspace solid phase microextraction (UA-HS-SPME. In the SPME method, the volatile components of the samples, irradiated by ultrasonic radiation, were collected on a polydimethyl siloxane (PDMS commercial fiber as well as some manually prepared nanoporous fibers from the samples headspace. To reach the better results, the extraction conditions were carefully optimized for the PDMS fiber. Under the optimized conditions (i.e. sonication time 15 min, extraction time 30 min and extraction temperature 55 ºC, 54 compounds were identified by the UA-HS-SPME-GC/MS method. The essential oil components of Citrus aurantium L. flower samples from two different regions of Iran and new and old samples from the same region were compared to one another. The major components identified for the samples with both the SPME and HD methods were linalool, linalyl acetate, limonene, β-myrcene, geranyl acetate, and neryl acetate, respectively. However, a substantial variation in the percentages of the components was identified for different samples and different extraction methods. The antimicrobial activities of the oil were also examined against six standard bacteria. There was some activity against Enterococcus fecalis, Escherichia coli, and Bacillus cereus, indicating important biological activities of the oil.

  9. 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.

  10. Analysis of Five Earthy-Musty Odorants in Environmental Water by HS-SPME/GC-MS

    Directory of Open Access Journals (Sweden)

    Zhen Ding

    2014-01-01

    Full Text Available The pressing issue of earthy and musty odor compounds in natural waters, which can affect the organoleptic properties of drinking water, makes it a public health concern. A simple and sensitive method for simultaneous analysis of five odorants in environmental water was developed by headspace solid-phase microextraction (HS-SPME coupled to chromatography-mass spectrometry (GC-MS, including geosmin (GSM and 2-methylisoborneol (2-MIB, as well as dimethyl trisulfide (DMTS, β-cyclocitral, and β-ionone. Based on the simple modification of original magnetic stirrer purchased from CORNING (USA, the five target compounds can be separated within 23 min, and the calibration curves show good linearity with a correlation coefficient above 0.999 (levels = 5. The limits of detection (LOD are all below 1.3 ng L−1, and the relative standard deviation (%RSD is between 4.4% and 9.9% (n = 7 and recoveries of the analytes from water samples are between 86.2% and 112.3%. In addition, the storage time experiment indicated that the concentrations did not change significantly for GSM and 2-MIB if they were stored in canonical environment. In conclusion, the method in this study could be applied for monitoring these five odorants in natural waters.

  11. Influence of harvest maturity and fruit logistics on pineapple (Ananas comosus [L.] Merr.) volatiles assessed by headspace solid phase microextraction and gas chromatography-mass spectrometry (HS-SPME-GC/MS).

    Science.gov (United States)

    Steingass, Christof B; Grauwet, Tara; Carle, Reinhold

    2014-05-01

    Profiling of volatiles from pineapple fruits was performed at four ripening stages using headspace solid-phase microextraction and gas chromatography-mass spectrometry (HS-SPME-GC/MS). In total, 142 volatiles were detected, of which 132 were identified. Multivariate data analysis was carried out to assess the effect of post-harvest storage on volatiles composition of green-ripe sea-freighted pineapple in comparison to air-freighted fruits harvested at full maturity. The latter fruits were characterised by volatiles described as potent odorants in pineapples, such as δ-octalactone, γ-lactones, 1-(E,Z)-3,5-undecatriene and 1,3,5,8-undecatetraene, as well as various methyl esters. In contrast, post-harvest storage of green-ripe sea-freighted fruits resulted in an increased formation of ethyl esters, acetates, acetoxy esters and alcohols, thus allowing the authentication of sea- and air-freighted pineapples, respectively. Particularly, compounds presumably derived from methyl-branched amino acid catabolism were identified in the fruits at later post-harvest stages. In addition, physicochemical traits were determined to characterise the fruit maturity stages. Copyright © 2013 Elsevier Ltd. All rights reserved.

  12. Quantitative and enantioselective analysis of monoterpenes from plant chambers and in ambient air using SPME

    Science.gov (United States)

    Yassaa, N.; Custer, T.; Song, W.; Pech, F.; Kesselmeier, J.; Williams, J.

    2010-11-01

    A headspace solid-phase microextraction (HS-SPME) and gas chromatography/mass spectrometry (GC/MS) system has been developed for quantifying enantiomeric and nonenantiomeric monoterpenes in plant chamber studies and ambient air. Performance of this system was checked using a capillary diffusion system to produce monoterpene standards. The adsorption efficiency, competitive adsorption and chromatographic peak resolution of monoterpene enantiomer pairs were compared for three SPME fibre coatings: 75 μm Carboxen-PDMS (CAR-PDMS), 50/30 μm divinylbenzene-carboxen-polydimethylsiloxane (DVB-CAR-PDMS) and 65 μm divinylbenzene-polydimethylsiloxane (DVB-PDMS). Key parameters such as the linearity and reproducibility of the SPME system have been investigated in this work. The best compromise between the enantiomeric separation of monoterpenes and competitive adsorption of the isoprenoids on the solid SPME fibre coating was found for DVB-PDMS fibres. The optimum conditions using DVB-PDMS fibres were applied to measure the exchange rates of monoterpenes in the emission of Quercus ilex using a laboratory whole plant enclosure under light and dark conditions, as well as in ambient air. With 592 and 223 ng m-2 s-1 respectively, β-myrcene and limonene were the predominant monoterpenes in the emission of Q. ilex. These values were closely comparable to those obtained using a zNose and cartridge GC-FID systems.

  13. Characterisation of the volatile profile of coconut water from five varieties using an optimised HS-SPME-GC analysis.

    Science.gov (United States)

    Prades, Alexia; Assa, Rebecca Rachel Ablan; Dornier, Manuel; Pain, Jean-Pierre; Boulanger, Renaud

    2012-09-01

    Coconut (Cocos nucifera L.) water is a refreshing tropical drink whose international market has recently been growing. However, little is yet known about its physicochemical composition, particularly its aroma. This study set out to characterise the volatile profile of water from five coconut varieties. Aroma compounds were characterised by headspace solid phase microextraction gas chromatography (HS-SPME-GC) analysis. An experimental design was established to optimise SPME conditions, leading to an equilibration time of 10 min followed by an extraction time of 60 min at 50 °C. Accordingly, immature coconut water from WAT (West African Tall), PB121 (MYD × WAT Hybrid), MYD (Malayan Yellow Dwarf), EGD (Equatorial Guinea Green Dwarf) and THD (Thailand Aromatic Green Dwarf) palms was analysed and described. Ketones were mainly present in the Tall and Hybrid varieties, whereas aldehydes were most abundant in the Dwarf palms. Tall coconut water was characterised by a high lactone content. THD exhibited a high ethyl octanoate level. The cluster analysis of the volatile fraction from the five coconut cultivars was found to be related to their genetic classification. The volatile compounds of immature coconut water from five varieties were characterised for the first time. Volatile profile analysis could be a useful tool for the selection of Dwarf coconut varieties, which are mainly consumed as a beverage. Copyright © 2012 Society of Chemical Industry.

  14. Analysis of flavor-related compounds from tabacco using SPME-GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Park, G.B.; Lee, S.G. [Korea Research Institute of Chemical Technology, Taejeon (Korea)

    2001-04-01

    The flavor-related compounds contained in tobacco were analyzed by selected ion monitoring (SIM) method using headspace SPME gas chromatography-mass spectrometry (GC-MS). Flavor-related compounds were estragole, pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methyleugenol and myristicin More than one of the flavor-related compounds were detected in the range of 0.001-1.3 {mu}g/g from all brands of tobacco studied. The recovery was ranged from 89.1 to 102.9% and relative standard deviation was ranged from 2.6 to 25.2%. (author). 19 refs., 4 tabs., 2 figs.

  15. Determination of methyl ethyl ketone in urine samples by headspace solid phase micro extraction (SPME) sampling associated to gas chromatography with flame-ionization detectoR (GC-FID)

    OpenAIRE

    Antunes, Marina Venzon; Linden, Rafael

    2008-01-01

    Methyl ethyl ketone (MEK) is a solvent commonly used in chemical, paint and shoe industry. The aim of this study was to develop and validate a method for urinary quantification of MEK, employing headspace solid phase micro extraction sampling (SPME) coupled to gas chromatography with flame ionization detection (GC-FID). The calibration curve (y=4.6851x-0.0011) presented good linearity with r²=0.9993. Accuracy (94-109%), intra-assay precision (4.07-5.91%) and inter-assay precision (3.03-5.62%)...

  16. HS-SPME-GC-MS Analysis of onion (Allium cepa L. and shallot (Allium ascalonicum L.

    Directory of Open Access Journals (Sweden)

    D’Auria, M.

    2017-06-01

    Full Text Available The volatile organic compounds of onion and shallot were determined via HS-SPME-GC-MS. The main components were dipropyldisulphide and allylpropyldisulphide. Thiopropanal S-oxide were detected only in onion volatiles. In shallot is interesting the presence of 2-methyl-2-pentenal, a compound with an intense fruity aroma, that can characterize the different aroma between onion and shallot. The SPME-GC-MS analysis of shallot after absorption on the SPME fiber at 50°C showed the presence of new compounds, whose structures have been discussed.

  17. Comparison of Spot and Time Weighted Averaging (TWA Sampling with SPME-GC/MS Methods for Trihalomethane (THM Analysis

    Directory of Open Access Journals (Sweden)

    Don-Roger Parkinson

    2016-02-01

    Full Text Available Water samples were collected and analyzed for conductivity, pH, temperature and trihalomethanes (THMs during the fall of 2014 at two monitored municipal drinking water source ponds. Both spot (or grab and time weighted average (TWA sampling methods were assessed over the same two day sampling time period. For spot sampling, replicate samples were taken at each site and analyzed within 12 h of sampling by both Headspace (HS- and direct (DI- solid phase microextraction (SPME sampling/extraction methods followed by Gas Chromatography/Mass Spectrometry (GC/MS. For TWA, a two day passive on-site TWA sampling was carried out at the same sampling points in the ponds. All SPME sampling methods undertaken used a 65-µm PDMS/DVB SPME fiber, which was found optimal for THM sampling. Sampling conditions were optimized in the laboratory using calibration standards of chloroform, bromoform, bromodichloromethane, dibromochloromethane, 1,2-dibromoethane and 1,2-dichloroethane, prepared in aqueous solutions from analytical grade samples. Calibration curves for all methods with R2 values ranging from 0.985–0.998 (N = 5 over the quantitation linear range of 3–800 ppb were achieved. The different sampling methods were compared for quantification of the water samples, and results showed that DI- and TWA- sampling methods gave better data and analytical metrics. Addition of 10% wt./vol. of (NH42SO4 salt to the sampling vial was found to aid extraction of THMs by increasing GC peaks areas by about 10%, which resulted in lower detection limits for all techniques studied. However, for on-site TWA analysis of THMs in natural waters, the calibration standard(s ionic strength conditions, must be carefully matched to natural water conditions to properly quantitate THM concentrations. The data obtained from the TWA method may better reflect actual natural water conditions.

  18. Analysis of lignocellulose derived phenolic monomers by headspace solid-phase microextraction and gas chromatography.

    Science.gov (United States)

    Kolb, Michaela; Schieder, Doris; Faulstich, Martin; Sieber, Volker

    2013-09-13

    A headspace solid-phase microextraction method with subsequent GC-MS (HS-SPME/GC-MS) was established for the quantitative analysis of volatile lignin derived phenolic monomers in complex aqueous solutions. Extraction was done using a polyacrylate fiber. The optimization of HS-SPME - parameters was performed using a multi component model solution of six representative phenolic monomers identified in liquid hot water (LHW) supernatants of hydrothermally treated lignocellulosic biomass: p-coumaric acid, guaiacol, vanillin, acetosyringone, 4-hydroxy-3-methoxyphenylacetone, and acetophenone. Plackett-Burman design was applied for pre-evaluation and 2(3) central composite designs with star points for parameter optimization. LOQ (S/N>10) and LOD (S/N>3) were determined for 12 phenols yielding LOQ of <0.005-618nM and LOD of <0.005-412nM. Within-day and between-day tests (n=6) showed different results for the tested phenols. RSD ranged from 2% to 30% and recovery rates from 99% to 160% in LHW matrix. Tests on storage of LHW supernatants for several weeks indicated a considerable influence of temperature on the stability of the solutions which may even have to be taken into account for auto sampler handling. All in all the method allows a fast and solvent free analysis requiring low sample volumes making it a powerful tool for screening or high-throughput analysis of aqueous solutions of lignin derived aromatics. Copyright © 2013. Published by Elsevier B.V.

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

    International Nuclear Information System (INIS)

    2007-01-01

    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

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

    International Nuclear Information System (INIS)

    2006-01-01

    The Performance Demonstration Program (PDP) for headspace gases distributes sample gases of volatile organic compounds (VOCs) for analysis. 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. Participating measurement

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

    Energy Technology Data Exchange (ETDEWEB)

    Carlsbad Field Office

    2006-04-01

    The Performance Demonstration Program (PDP) for headspace gases distributes sample gases of volatile organic compounds (VOCs) for analysis. 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. Participating measurement

  2. 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

  3. 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

  4. 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.

  5. 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

  6. Headspace-solid-phase microextraction in the analysis of the volatile fraction of aromatic and medicinal plants.

    Science.gov (United States)

    Belliardo, Flavio; Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Rubiolo, Patrizia; Sgorbini, Barbara

    2006-08-01

    Headspace (HS)-solid-phase microextraction (SPME) has assumed an ever increasing importance as a technique for HS sampling to study the composition of the HS of medicinal and aromatic plants. HS-SPME has mainly been applied for (a) studying the composition of the volatile fraction, including in addition to or as an alternative to other sampling techniques; (b) monitoring the biological phenomena involved with the volatile fraction of a plant; (c) discriminating between species, subspecies, varieties, cultivars, or chemotypes; and (d) quality control of plant samples. A review of 108 articles published during 2000-2005 is presented covering the use of HS-SPME in the field of aromatic and medicinal plants, selection of the most effective fiber and sampling conditions, comparison of HS-SPME and other volatile fraction sample preparation techniques, and the advantages and limits of HS-SPME when applied to medicinal and aromatic plants.

  7. Organic analysis of the headspace in Hanford waste tanks

    International Nuclear Information System (INIS)

    Lucke, R.B.; McVeety, B.D.; Clauss, T.W.; Fruchter, J.S.; Goheen, S.C.

    1994-01-01

    Before radioactive mixed waste in Hanford waste tanks can be isolated and permanently stored, several safety issues need to be addressed. The headspace vapors in Hanford Tank 103-C raise two issues: (1) the potential flammability of the vapor and aerosol, and (2) the potential worker health and safety hazards associated with the toxicity of the constituents. As a result, the authors have implemented organic analysis methods to characterize the headspace vapors in Hanford waste tanks. To address the flammability issue, they have used OSHA versatile sampling (OVS) tubes as the sampling method followed by solvent extraction and GC/MS analysis. For analyzing volatile organics and organic air toxins, they have implemented SUMMA trademark canisters as the collection device followed by cryogenic trapping and GC/MS analysis. Strategies for modifying existing NIOSH and EPA methods to make them applicable to vapors in Hanford waste tanks are discussed. Identification and quantification results of volatile and semivolatile organics are presented

  8. Analysis of Volatile Markers for Virgin Olive Oil Aroma Defects by SPME-GC/FID: Possible Sources of Incorrect Data.

    Science.gov (United States)

    Oliver-Pozo, Celia; Aparicio-Ruiz, Ramón; Romero, Inmaculada; García-González, Diego L

    2015-12-09

    The need to explain virgin olive oil (VOO) aroma descriptors by means of volatiles has raised interest in applying analytical techniques for trapping and quantitating volatiles. Static headspace sampling with solid phase microextraction (SPME) as trapping material is one of the most applied solutions for analyzing volatiles. The use of an internal standard and the determination of the response factors of the main volatiles seem to guarantee the correct determination of volatile concentrations in VOOs by SPME-GC/FID. This paper, however, shows that the competition phenomena between volatiles in their adsorption to the SPME fiber, inherent in static headspace sampling, may affect the quantitation. These phenomena are more noticeable in the particular case of highly odorant matrices, such as rancid and vinegary VOOs with high intensity of defect. The competition phenomena can modify the measurement sensitivity, which can be observed in volatile quantitation as well as in the recording of internal standard areas in different matrices. This paper analyzes the bias of the peak areas and concentrations of those volatiles that are markers for each sensory defect of VOOs (rancid, vinegary, musty, and fusty) when the intensity and complexity of aroma are increased. Of the 17 volatile markers studied in this work, 10 presented some anomalies in the quantitation in highly odorant matrices due the competition phenomena. However, quantitation was not affected in the concentration ranges at which each volatile marker is typically found in the defective oils they were characteristic of, validating their use as markers.

  9. Performance demonstration program plan for analysis of simulated headspace gases

    International Nuclear Information System (INIS)

    1995-06-01

    The Performance Demonstration Program (PDP) for analysis of headspace gases will consist of regular distribution and analyses of test standards to evaluate the capability for analyzing VOCs, hydrogen, and methane in the headspace of transuranic (TRU) waste throughout the Department of Energy (DOE) complex. Each distribution is termed a PDP cycle. These evaluation cycles will provide an objective measure of the reliability of measurements performed for TRU waste characterization. Laboratory performance will be demonstrated by the successful analysis of blind audit samples of simulated TRU waste drum headspace gases according to the criteria set within the text of this Program Plan. Blind audit samples (hereinafter referred to as PDP samples) will be used as an independent means to assess laboratory performance regarding compliance with the QAPP QAOs. The concentration of analytes in the PDP samples will encompass the range of concentrations anticipated in actual waste characterization gas samples. Analyses which are required by the WIPP to demonstrate compliance with various regulatory requirements and which are included in the PDP must be performed by laboratories which have demonstrated acceptable performance in the PDP

  10. Comparison of the atmospheric- and reduced-pressure HS-SPME strategies for analysis of residual solvents in commercial antibiotics using a steel fiber coated with a multiwalled carbon nanotube/polyaniline nanocomposite.

    Science.gov (United States)

    Ghiasvand, Ali Reza; Nouriasl, Kolsoum; Yazdankhah, Fatemeh

    2018-01-01

    A low-cost, sensitive and reliable reduced-pressure headspace solid-phase microextraction (HS-SPME) setup was developed and evaluated for direct extraction of residual solvents in commercial antibiotics, followed by determination by gas chromatography with flame ionization detection (GC-FID). A stainless steel narrow wire was made porous and adhesive by platinization by a modified electrophoretic deposition method and coated with a polyaniline/multiwalled carbon nanotube nanocomposite. All experimental variables affecting the extraction efficiency were investigated for both atmospheric-pressure and reduced-pressure conditions. Comparison of the optimal experimental conditions and the results demonstrated that the reduced-pressure strategy leads to a remarkable increase in the extraction efficiency and reduction of the extraction time and temperature (10 min, 25 °Ϲ vs 20 min, 40 °Ϲ). Additionally, the reduced-pressure strategy showed better analytical performances compared with those obtained by the conventional HS-SPME-GC-FID method. Limit of detections, linear dynamic ranges, and relative standard deviations of the reduced-pressure HS-SPME procedure for benzene, toluene, ethylbenzene, and xylene (BTEX) in injectable solid drugs were obtained over the ranges of 20-100 pg g -1 , 0.02-40 μg g -1 , and 2.8-10.2%, respectively. The procedure developed was successful for the analysis of BTEX in commercial containers of penicillin, ampicillin, ceftriaxone, and cefazolin. Graphical abstract Schematic representation of the developed RP-HS-SPME setup.

  11. Optimization of HS-SPME/GC-MS analysis and its use in the profiling of illicit ecstasy tablets (Part 1).

    Science.gov (United States)

    Bonadio, Federica; Margot, Pierre; Delémont, Olivier; Esseiva, Pierre

    2009-05-30

    A headspace solid-phase microextraction procedure (HS-SPME) was developed for the profiling of traces present in 3,4-methylenedioxymethylampethamine (MDMA). Traces were first extracted using HS-SPME and then analyzed by gas chromatography-mass spectroscopy (GC-MS). The HS-SPME conditions were optimized using varying conditions. Optimal results were obtained when 40 mg of crushed MDMA sample was heated at 80 degrees C for 15 min, followed by extraction at 80 degrees C for 15 min with a polydimethylsiloxane/divinylbenzene coated fibre. A total of 31 compounds were identified as traces related to MDMA synthesis, namely precursors, intermediates or by-products. In addition some fatty acids used as tabletting materials and caffeine used as adulterant, were also detected. The use of a restricted set of 10 target compounds was also proposed for developing a screening tool for clustering samples having close profile. 114 seizures were analyzed using an SPME auto-sampler (MultiPurpose Samples MPS2), purchased from Gerstel GMBH & Co. (Germany), and coupled to GC-MS. The data was handled using various pre-treatment methods, followed by the study of similarities between sample pairs based on the Pearson correlation. The results show that HS-SPME, coupled with the suitable statistical method is a powerful tool for distinguishing specimens coming from the same seizure and specimens coming from different seizures. This information can be used by law enforcement personnel to visualize the ecstasy distribution network as well as the clandestine tablet manufacturing.

  12. 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.

  13. Headspace solid-phase microextraction gas chromatography-mass spectrometry analysis of volatiles in orujo spirits from a defined geographical origin.

    Science.gov (United States)

    Peña, Rosa M; Barciela, Julia; Herrero, Carlos; García-Martín, Sagrario

    2008-04-23

    A headspace solid-phase microextraction (HS-SPME) and gas chromatography-selective ion monitoring/mass spectrometry (GC-SIM/MS) method was optimized for analysis of 22 volatile compounds in orujo spirit samples from the Geographic Denomination "Orujo de Galicia/Augardente de Galicia". HS-SPME experimental conditions, such as fiber coating, extraction temperature, extraction and pre-equilibrium time, sample volume, and the presence of salt, were studied to improve the extraction process. The best results were obtained using a 65 microm Carbowax-divinylbenzene fiber during a headspace extraction at 40 degrees C with constant magnetic stirring for 15 min and after a 5 min period of pre-equilibrium time. The sample volume was 6 mL of orujo containing 25% of NaCl, placed in 12 mL glass vials equipped with a screw cap and PTFE/silicone septum. Desorption was performed directly in the gas chromatograph injector port for 5 min at 250 degrees C using the splitless mode. The proposed method is sensible (with detection limits between 0.0045 and 0.2399 mg/L), precise (with coefficients of variation in the range 0.99-8.18%), and linear over more than 1 order of magnitude. The developed method presented recoveries comprised between 76.0 and 112.4%. The applicability of the new method was demonstrated by determining the considered 22 volatile compounds in nine orujo commercial samples with quality and origin brands.

  14. Quantification of selected volatile organic compounds in human urine by gas chromatography selective reagent ionization time of flight mass spectrometry (GC-SRI-TOF-MS) coupled with head-space solid-phase microextraction (HS-SPME).

    Science.gov (United States)

    Mochalski, Paweł; Unterkofler, Karl

    2016-08-07

    Selective reagent ionization time of flight mass spectrometry with NO(+) as the reagent ion (SRI-TOF-MS(NO(+))) in conjunction with gas chromatography (GC) and head-space solid-phase microextraction (HS-SPME) was used to determine selected volatile organic compounds in human urine. A total of 16 volatiles exhibiting high incidence rates were quantified in the urine of 19 healthy volunteers. Amongst them there were ten ketones (acetone, 2-butanone, 3-methyl-2-butanone, 2-pentanone, 3-methyl-2-pentanone, 4-methyl-2-pentanone, 2-hexanone, 3-hexanone, 2-heptanone, and 4-heptanone), three volatile sulphur compounds (dimethyl sulfide, allyl methyl sulfide, and methyl propyl sulfide), and three heterocyclic compounds (furan, 2-methylfuran, 3-methylfuran). The concentrations of the species under study varied between 0.55 nmol L(-1) (0.05 nmol mmol(-1)creatinine) for allyl methyl sulfide and 11.6 μmol L(-1) (1.54 μmol mmol(-1)creatinine) for acetone considering medians. Limits of detection (LODs) ranged from 0.08 nmol L(-1) for allyl methyl sulfide to 1.0 nmol L(-1) for acetone and furan (with RSDs ranging from 5 to 9%). The presented experimental setup assists both real-time and GC analyses of volatile organic compounds, which can be performed consecutively using the same analytical system. Such an approach supports the novel concept of hybrid volatolomics, an approach which combines VOC profiles obtained from two or more body fluids to improve and complement the chemical information on the physiological status of an individual.

  15. Methodological Variability Using Electronic Nose Technology For Headspace Analysis

    Science.gov (United States)

    Knobloch, Henri; Turner, Claire; Spooner, Andrew; Chambers, Mark

    2009-05-01

    Since the idea of electronic noses was published, numerous electronic nose (e-nose) developments and applications have been used in analyzing solid, liquid and gaseous samples in the food and automotive industry or for medical purposes. However, little is known about methodological pitfalls that might be associated with e-nose technology. Some of the methodological variation caused by changes in ambient temperature, using different filters and changes in mass flow rates are described. Reasons for a lack of stability and reproducibility are given, explaining why methodological variation influences sensor responses and why e-nose technology may not always be sufficiently robust for headspace analysis. However, the potential of e-nose technology is also discussed.

  16. Analysis of ammonium nitrate headspace by on-fiber solid phase microextraction derivatization with gas chromatography mass spectrometry.

    Science.gov (United States)

    Lubrano, Adam L; Andrews, Benjamin; Hammond, Mark; Collins, Greg E; Rose-Pehrsson, Susan

    2016-01-15

    A novel analytical method has been developed for the quantitation of trace levels of ammonia in the headspace of ammonium nitrate (AN) using derivatized solid phase microextraction (SPME) fibers with gas chromatography mass spectrometry (GC-MS). Ammonia is difficult to detect via direct injection into a GC-MS because of its low molecular weight and extreme polarity. To circumvent this issue, ammonia was derivatized directly onto a SPME fiber by the reaction of butyl chloroformate coated fibers with the ammonia to form butyl carbamate. A derivatized externally sampled internal standard (dESIS) method based upon the reactivity of diethylamine with unreacted butyl chloroformate on the SPME fiber to form butyl diethylcarbamate was established for the reproducible quantification of ammonia concentration. Both of these compounds are easily detectable and separable via GC-MS. The optimized method was then used to quantitate the vapor concentration of ammonia in the headspace of two commonly used improvised explosive device (IED) materials, ammonium nitrate fuel oil (ANFO) and ammonium nitrate aluminum powder (Ammonal), as well as identify the presence of additional fuel components within the headspace. Published by Elsevier B.V.

  17. Polyelectrolyte coatings prevent interferences from charged nanoparticles in SPME speciation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Zielińska, Katarzyna, E-mail: kzielinska@gmail.com; Leeuwen, Herman P. van

    2014-09-24

    Highlights: • For the first time SPME fiber is coated with polyelectrolyte layer. • Sorption of nanoparticles on the solid phase surface is prevented. • Polyelectrolyte-modified fiber enables extraction of free analyte in presence of sorbing nanoparticles. - Abstract: In this work we present a new approach for protection of the fiber in solid phase microextraction (SPME) from interfering charged particles present in the sample medium. It involves coating of commercial poly(dimethylsiloxane) extraction phase with polyelectrolyte layer composed of poly(diallyldimethylammonium chloride), and poly(sodium 4-styrenesulfonate). The modified fiber provides reproducible, convenient and fast extraction capabilities toward the model analyte, triclosan (TCS). A negatively charged polyelectrolyte coating prevents sorbing oxidic nanoparticles from both partitioning into the PDMS phase and aggregation at its surface. The results for the TCS/nanoparticle sample show that the polyelectrolyte layer-modified solid phase extracts just the free form of the organic compound and enables dynamic speciation analysis of the nanoparticulate target analyte complex.

  18. Polyelectrolyte coatings prevent interferences from charged nanoparticles in SPME speciation analysis

    International Nuclear Information System (INIS)

    Zielińska, Katarzyna; Leeuwen, Herman P. van

    2014-01-01

    Highlights: • For the first time SPME fiber is coated with polyelectrolyte layer. • Sorption of nanoparticles on the solid phase surface is prevented. • Polyelectrolyte-modified fiber enables extraction of free analyte in presence of sorbing nanoparticles. - Abstract: In this work we present a new approach for protection of the fiber in solid phase microextraction (SPME) from interfering charged particles present in the sample medium. It involves coating of commercial poly(dimethylsiloxane) extraction phase with polyelectrolyte layer composed of poly(diallyldimethylammonium chloride), and poly(sodium 4-styrenesulfonate). The modified fiber provides reproducible, convenient and fast extraction capabilities toward the model analyte, triclosan (TCS). A negatively charged polyelectrolyte coating prevents sorbing oxidic nanoparticles from both partitioning into the PDMS phase and aggregation at its surface. The results for the TCS/nanoparticle sample show that the polyelectrolyte layer-modified solid phase extracts just the free form of the organic compound and enables dynamic speciation analysis of the nanoparticulate target analyte complex

  19. An Innovative Rapid Method for Analysis of 10 Organophosphorus Pesticide Residues in Wheat by HS-SPME-GC-FPD/MSD.

    Science.gov (United States)

    Du, Xin; Ren, YongLin; Beckett, Stephen J

    2016-01-01

    The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/PDMS fiber increased with increasing spiking levels, yielding significant (R(2) > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity.

  20. Investigation of a Quantitative Method for the Analysis of Chiral Monoterpenes in White Wine by HS-SPME-MDGC-MS of Different Wine Matrices.

    Science.gov (United States)

    Song, Mei; Xia, Ying; Tomasino, Elizabeth

    2015-04-22

    A valid quantitative method for the analysis of chiral monoterpenes in white wine using head-space solid phase micro-extraction-MDGC-MS (HS-SPME-MDGC-MS) with stable isotope dilution analysis was established. Fifteen compounds: (S)-(-)-limonene, (R)-(+)-limonene, (+)-(2R,4S)-cis-rose oxide, (-)-(2S,4R)-cis-rose oxide, (-)-(2R,4R)-trans-rose oxide, (+)-(2S,4S)-cis-rose oxide, furanoid (+)-trans-linalool oxide, furanoid (-)-cis-linalool oxide, furanoid (-)-trans-linalool oxide, furanoid (+)-cis-linalool oxide, (-)-linalool, (+)-linalool, (-)-α-terpineol, (+)-α-terpineol and (R)-(+)-β-citronellol were quantified. Two calibration curves were plotted for different wine bases, with varying residual sugar content, and three calibration curves for each wine base were investigated during a single fiber's lifetime. This was needed as both sugar content and fiber life impacted the quantification of the chiral terpenes. The chiral monoterpene content of six Pinot Gris wines and six Riesling wines was then analyzed using the verified method. ANOVA with Tukey multiple comparisons showed significant differences for each of the detected chiral compounds in all 12 wines. PCA score plots showed a clear separation between the Riesling and Pinot Gris wines. Riesling wines had greater number of chiral terpenes in comparison to Pinot Gris wines. Beyond total terpene content it is possible that the differences in chiral terpene content may be driving the aromatic differences in white wines.

  1. Application of Microextraction Techniques Including SPME and MESI to the Thermal Degradation of Polymers: A Review.

    Science.gov (United States)

    Kaykhaii, Massoud; Linford, Matthew R

    2017-03-04

    Here, we discuss the newly developed micro and solventless sample preparation techniques SPME (Solid Phase Microextraction) and MESI (Membrane Extraction with a Sorbent Interface) as applied to the qualitative and quantitative analysis of thermal oxidative degradation products of polymers and their stabilizers. The coupling of these systems to analytical instruments is also described. Our comprehensive literature search revealed that there is no previously published review article on this topic. It is shown that these extraction techniques are valuable sample preparation tools for identifying complex series of degradation products in polymers. In general, the number of products identified by traditional headspace (HS-GC-MS) is much lower than with SPME-GC-MS. MESI is particularly well suited for the detection of non-polar compounds, therefore number of products identified by this technique is not also to the same degree of SPME. Its main advantage, however, is its ability of (semi-) continuous monitoring, but it is more expensive and not yet commercialized.

  2. New insight on biological interaction analysis: new nanocrystalline mixed metal oxide SPME fiber for GC-FID analysis of BTEX and its application in human hemoglobin-benzene interaction studies.

    Directory of Open Access Journals (Sweden)

    Reza Hosseinzadeh

    Full Text Available Nanocrystalline mixed metal oxides (MMO of various metal cations were synthesized and were used for coating a piece of copper wire as a new high sensitive solid phase micro extraction (SPME fiber in extraction and determination of BTEX compounds from the headspace of aqueous samples prior to GC-FID analysis. Under optimum extraction conditions, the proposed fiber exhibited low detection limits, and quantification limits, good reproducibility, simple and fast preparation method, high fiber capacity and high thermal and mechanical durability. These are some of the most important advantages of the new fiber. The proposed fiber was used for human hemoglobin upon interaction with benzene. Binding isotherm, Scatchard and Klotz logarithmic plots were constructed using HS-SPME-GC data, accurately. The obtained binding isotherm analyzed using Hill method. The Hill parameters have been obtained by calculating saturation parameter from the ratio of measured chromatographic peak areas in the presence and absence of hemoglobin. In this interaction, Hill coefficient and Hill constant determined as (nH = 6.14 and log KH = 6.47 respectively. These results reveal the cooperativity of hemoglobin upon interaction with benzene.

  3. Fast detection of triacetone triperoxide (TATP) from headspace using planar solid-phase microextraction (PSPME) coupled to an IMS detector.

    Science.gov (United States)

    Fan, Wen; Young, Mimy; Canino, Jon; Smith, James; Oxley, Jimmie; Almirall, Jose R

    2012-04-01

    Triacetone triperoxide (TATP) is a high explosive synthesized from easily available reactants making it accessible for illicit uses. In this study, fast detection of TATP is achieved using a novel planar solid-phase microextraction (PSPME) as a preconcentration and sampling device for headspace analysis offering improved sensitivity and reduced sampling time over the conventional fiber-based solid-phase microextraction (SPME) when followed by ion mobility spectrometer (IMS) detection. Quantitation and comparison of the retention capabilities of PSPME as compared to the commercially available SPME were determined using TATP standards and analyzed using gas chromatography-mass spectrometry for SPME analysis and a commercial IMS with no instrumental modification for PSPME. Static and dynamic headspace extractions were used and compared for PSPME extractions, in which low milligram quantities of TATP were detected within 30 s of static mode sampling and less than 5 s in the dynamic mode sampling for PSPME-IMS.

  4. Analysis of volatile compounds emitted from fresh Syringa oblata flowers in different florescence by headspace solid-phase microextraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Li, Zu-Guang; Lee, Maw-Rong; Shen, De-Long

    2006-08-18

    In this study, a simple and solvent-free method was developed for determination of the volatile compounds from fresh flowers of Syringa oblata using headspace solid-phase microextraction and gas chromatography-mass spectrometry. The SPME parameters were studied, the optimum conditions of a 65mum polydimethylsiloxan/divinylbenezene (PDMS/DVB), extraction temperature of 25 degrees C and extraction time of 30 min were obtained and applied to extraction of the volatile compounds emitted from fresh flowers of S. oblata. The volatile compounds released from fresh flowers of S. oblata were separated and identified by GC-MS. Lilac aldehyde A, lilac aldehyde B, lilac aldehyde C, lilac aldehyde D, lilac alcohol A, lilac alcohol B, lilac alcohol C, lilac alcohol D, alpha-pinene, sabinene, beta-pinene, myrcene, d-limonene, eucalyptol, cis-ocimene, benzaldehyde, terpinolene, linalool, benzene acetaldehyde, alpha-terpineol, p-methoxyanisole, p-anisaldehyde, (Z,E)-alpha-farnesene and (E,E)-alpha-farnesene were the most abundant volatiles released from fresh flowers of S. oblata var. alba. The relative contents of main volatile fragrance were found to be different in emissions from two varieties of S. oblata flowers (white or purple in color). The four isomers of lilac alcohol and four isomer lilac aldehyde were the characteristic components of the scent of fresh flowers of S. oblata. The main volatile fragrance from fresh flowers of S. oblata var. alba in different florescence ((A) flower buds; (B) at the early stage of flower blooming; (C) during the flower blooming; (D) at the end of flower blooming; (E) senescence) were studied in this paper. The results demonstrated that headspace SPME-GC-MS is a simple, rapid and solvent-free method suitable for analysis of volatile compounds emitted from fresh flowers of S. oblata in different florescence.

  5. Determinação de metil-etil-cetona em amostras de urina com amostragem por micro extração em fase sólida (MEFS em headspace associada à cromatografia gasosa com detector de ionização de chama (CG-DIC Determination of methyl ethyl ketone in urine samples by headspace solid phase micro extraction (SPME sampling associated to gas chromatography with flame-ionization detectoR (GC-FID

    Directory of Open Access Journals (Sweden)

    Marina Venzon Antunes

    2008-01-01

    Full Text Available Methyl ethyl ketone (MEK is a solvent commonly used in chemical, paint and shoe industry. The aim of this study was to develop and validate a method for urinary quantification of MEK, employing headspace solid phase micro extraction sampling (SPME coupled to gas chromatography with flame ionization detection (GC-FID. The calibration curve (y=4.6851x-0.0011 presented good linearity with r²=0.9993. Accuracy (94-109%, intra-assay precision (4.07-5.91% and inter-assay precision (3.03-5.62% were acceptable. The quantification limit was 0.19 mg/L. This low cost method can be used routinely in the biological monitoring of occupational exposure to MEK, according to the requirements of the Brazilian legislation.

  6. Headspace Solid-Phase Microextraction Coupled with Gas ...

    African Journals Online (AJOL)

    contact temperature measurement system (ONTMS). Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was used to analyze the volatile composition of raw FCP and its various ...

  7. Polyelectrolyte coatings prevent interferences from charged nanoparticles in SPME speciation analysis

    NARCIS (Netherlands)

    Zielinska, K.; Leeuwen, van H.P.

    2014-01-01

    In this work we present a new approach for protection of the fiber in solid phase microextraction (SPME) from interfering charged particles present in the sample medium. It involves coating of commercial poly(dimethylsiloxane) extraction phase with polyelectrolyte layer composed of

  8. Headspace solid-phase microextraction and gas chromatography ...

    African Journals Online (AJOL)

    Purpose: To extract and analyze the volatile components of Chrysanthemum morifolium Ramat. 'huaiju' by headspace solid-phase microextraction (HS-SPME) and gas chromatography–mass spectrometry. (GC–MS). Methods: Volatile components were extracted by HS-SPME and identified by GC–MS. The relative contents ...

  9. Headspace solid-phase microextraction and gas chromatography ...

    African Journals Online (AJOL)

    Purpose: To extract and analyze the volatile components of Chrysanthemum morifolium Ramat. 'huaiju' by headspace solid-phase microextraction (HS-SPME) and gas chromatography–mass spectrometry (GC–MS). Methods: Volatile components were extracted by HS-SPME and identified by GC–MS. The relative contents ...

  10. 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 (AV...

  11. SPME-GC analysis of THC in saliva samples collected with "EPITOPE" device.

    Science.gov (United States)

    Fucci, N; De Giovanni, N; Chiarotti, M; Scarlata, S

    2001-07-15

    In this study we examined the presence of cannabinoids in saliva samples obtained from 24 drug-abusers. The saliva specimens were collected by "EPITOPE" system and the subsequent elution of samples was achieved by centrifugation. The resulting ultrafiltrates have been directly sampled with solid phase micro-extraction (SPME) and then analyzed by GC/MS. Saliva sampling is less invasive than collection of blood.

  12. Optimization of headspace experimental factors to determine chlorophenols in water by means of headspace solid-phase microextraction and gas chromatography coupled with mass spectrometry and parallel factor analysis.

    Science.gov (United States)

    Morales, Rocío; Cruz Ortiz, M; Sarabia, Luis A

    2012-11-19

    In this work an analytical procedure based on headspace solid-phase microextraction and gas chromatography coupled with mass spectrometry (HS-SPME-GC/MS) is proposed to determine chlorophenols with prior derivatization step to improve analyte volatility and therefore the decision limit (CCα). After optimization, the analytical procedure was applied to analyze river water samples. The following analytes are studied: 2,4-dichlorophenol (2,4-DCP), 2,4,6-trichlorophenol (2,4,6-TrCP), 2,3,4,6-tetrachlorophenol (2,4,6-TeCP) and pentachlorophenol (PCP). A D-optimal design is used to study the parameters affecting the HS-SPME process and the derivatization step. Four experimental factors at two levels and one factor at three levels were considered: (i) equilibrium/extraction temperature, (ii) extraction time, (iii) sample volume, (iv) agitation time and (v) equilibrium time. In addition two interactions between four of them were considered. The D-optimal design enables the reduction of the number of experiments from 48 to 18 while maintaining enough precision in the estimation of the effects. As every analysis took 1h, the design is blocked in 2 days. The second-order property of the PARAFAC (parallel factor analysis) decomposition avoids the need of fitting a new calibration model each time that the experimental conditions change. In consequence, the standardized loadings in the sample mode estimated by a PARAFAC decomposition are the response used in the design because they are proportional to the amount of analyte extracted. It has been found that block effect is significant and that 60°C equilibrium temperature together with 25min extraction time are necessary to achieve the best extraction for the chlorophenols analyzed. The other factors and interactions were not significant. After that, a calibration based in a PARAFAC2 decomposition provided the following values of CCα: 120, 208, 86, 39ngL(-1) for 2,4-DCP, 2,4,6-TrCP, 2,3,4,5-TeCP and PCP respectively for a

  13. Evaluation of volatile metabolites as markers in Lycopersicon esculentum L. cultivars discrimination by multivariate analysis of headspace solid phase microextraction and mass spectrometry data.

    Science.gov (United States)

    Figueira, José; Câmara, Hugo; Pereira, Jorge; Câmara, José S

    2014-02-15

    To gain insights on the effects of cultivar on the volatile metabolomic expression of different tomato (Lycopersicon esculentum L.) cultivars--Plum, Campari, Grape, Cherry and Regional, cultivated under similar edafoclimatic conditions, and to identify the most discriminate volatile marker metabolites related to the cultivar, the chromatographic profiles resulting from headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-qMS) analysis, combined with multivariate analysis were investigated. The data set composed by the 77 volatile metabolites identified in the target tomato cultivars, 5 of which (2,2,6-trimethylcyclohexanone, 2-methyl-6-methyleneoctan-2-ol, 4-octadecyl-morpholine, (Z)-methyl-3-hexenoate and 3-octanone) are reported for the first time in tomato volatile metabolomic composition, was evaluated by chemometrics. Firstly, principal component analysis was carried out in order to visualise data trends and clusters, and then, linear discriminant analysis in order to detect the set of volatile metabolites able to differentiate groups according to tomato cultivars. The results obtained revealed a perfect discrimination between the different Lycopersicon esculentum L. cultivars considered. The assignment success rate was 100% in classification and 80% in prediction ability by using "leave-one-out" cross-validation procedure. The volatile profile was able to differentiate all five cultivars and revealed complex interactions between them including the participation in the same biosynthetic pathway. The volatile metabolomic platform for tomato samples obtained by HS-SPME/GC-qMS here described, and the interrelationship detected among the volatile metabolites can be used as a roadmap for biotechnological applications, namely to improve tomato aroma and their acceptance in the final consumer, and for traceability studies. Copyright © 2013 Elsevier Ltd. All rights reserved.

  14. [Micromethods for determining organic solvents in blood by headspace analysis].

    Science.gov (United States)

    Kostrzewski, P

    1993-01-01

    The evaluation in industrial exposure to volatile organic compounds based on assessing concentrations of unchanged substances in blood of exposed workers seems to gain increasing interest. The main obstacle to a wide application of this method is the difficulty in collecting venous blood samples. Many authors suggest determining volatiles in capillary blood samples because they display the same concentrations as the arterial blood samples. The collection of capillary blood samples is much more convenient in occupational setting than the collection of venous blood samples. The aim of this study was to develop micromethod for determining organic solvents in small blood samples (100 mm3) by gas chromatography with headspace technique. 1.8 cm3 glass vessels (Sapelco) with screw caps, silicone rubber membranes and aluminium foil pads were used. After addition of 0.1 cm3 of blood and 2.0 cm3 of aqueous solution of internal standard, the vessels were closed tightly and shaken for 30 min. at 70 degrees C in water bath. Then about 1 cm3 of the gas phase was sampled with a gastight syringe (Hamilton) injected into the gas chromatograph. The parameters of the recently developed methods for determining organic solvents in blood samples, including linearity, precision, reproducibility, stability and sensitivity, are fully compatible with the principles of biological monitoring.

  15. 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...

  16. Validation of an analytical method for analysis of cannabinoids in hair by headspace solid-phase microextraction and gas chromatography-ion trap tandem mass spectrometry.

    Science.gov (United States)

    Emídio, Elissandro Soares; Prata, Vanessa de Menezes; Dórea, Haroldo Silveira

    2010-06-18

    The development of an analytical method for the determination of Delta(9)-tetrahydrocannabinol (THC), cannabidiol (CBD) and cannabinol (CBN) in samples of human hair is described. Samples were subjected to a procedure based on the combination of headspace solid-phase microextraction (HS-SPME) with gas chromatography linked with mass spectrometry operating in tandem mode (GC-MS/MS). A 10 mg aliquot of sample was firstly decontaminated using petroleum ether, deionized water and dichloromethane (2 mL of each solvent), for 10 min under sonication, and then digested in alkaline solution (1 mol L(-1) NaOH). The method variables evaluated were pH, mass of hair, fiber type, extraction temperature, desorption time, ionic strength, pre-equilibrium time and extraction time. Parameters concerning operation of the tandem mode MS/MS were also assessed and optimized. Validation of the method demonstrated excellent linearity in the range 0.1-8.0 ng mg(-1), with regression coefficients better than 0.994. Precision was determined using two different concentrations (upper and lower limits of the linear range), and RSD values were between 6.6 and 16.4%. Absolute recoveries (measured in triplicate) were in the range 1.1-8.7%, and limits of detection and quantification were 0.007-0.031 ng mg(-1) and 0.012-0.062 ng mg(-1), respectively. The LOQ for THC (0.062 ng mg(-1)) was below the cut-off value (LOQ Toxicologie Analytique (SFTA). The optimized SPME method was applied in analysis of hair samples from Cannabis drug users, showing that CBN and CBD were present in all samples analyzed. 2010 Elsevier B.V. All rights reserved.

  17. 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. Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. Analysis of Organic Volatile Flavor Compounds in Fermented Stinky Tofu Using SPME with Different Fiber Coatings

    Directory of Open Access Journals (Sweden)

    Wei Guan

    2012-03-01

    Full Text Available The organic volatile flavor compounds in fermented stinky tofu (FST were studied using SPME-GC/MS. A total of 39 volatile compounds were identified, including nine esters, seven alcohols, five alkenes, four sulfides, three heterocycles, three carboxylic acids, three ketones, two aldehydes, one phenol, one amine and one ether. These compounds were determined by MS, and conformed by comparison of the retention times of the separated constituents with those of authentic samples and by comparison of retention indexes (RIs of separated constituents with the RIs reported in the literature. The predominant volatile compound in FST was indole, followed by dimethyl trisulfide, phenol, dimethyl disulfide and dimethyl tetrasulfide. In order to find a better extraction time, the extraction times was optimized for each type of SPME fiber; the results show that the best extraction time for Carboxen/PDMS is 60 min, for PDMS/DVB 30 min, for DVB/CAR/PDMS 60 min and for PDMS 75 min. Of the four fibers used in this work, Carboxen/PDMS is found to be the most suitable to extract the organic volatile flavor compounds in fermented stinky tofu.

  19. Passive Sampling and Analysis of Naphthalene in Internal Combustion Engine Exhaust with Retracted SPME Device and GC-MS

    Directory of Open Access Journals (Sweden)

    Nassiba Baimatova

    2017-07-01

    Full Text Available Exhaust gases from internal combustion engines are the main source of urban air pollution. Quantification of Polycyclic aromatic hydrocarbons (PAHs in the exhaust gases is needed for emissions monitoring, enforcement, development, and testing of control technologies. The objective was to develop quantification of gaseous naphthalene in diesel engine exhaust based on diffusion-controlled extraction onto a retracted solid-phase microextraction (SPME fiber coating and analysis on gas chromatography-mass spectrometry (GC-MS. Extraction of naphthalene with retracted fibers followed Fick’s law of diffusion. Extracted mass of naphthalene was proportional to Cg, t, Dg, T and inversely proportional to Z. Method detection limit (p = 0.95 was 11.5 ppb (0.06 mg·m−3 at t = 9 h, Z = 10 mm and T = 40 °C, respectively. It was found that the % mass extracted of naphthalene by SPME needle assembly depended on the type of fiber. Storage time at different temperatures did not affect analyte losses extracted by polydimethylsiloxane (PDMS 100 µm fiber. The developed method was tested on exhaust gases from idling pickup truck and tractor, and compared side-by-side with a direct injection of sampled exhaust gas method. Time-weighted average (TWA concentrations of naphthalene in exhaust gases from idling pickup truck and a tractor ranged from 0.08 to 0.3 mg·m−3 (15.3–53.7 ppb.

  20. Dynamic Headspace Sampling as an Initial Step for Sample Preparation in Chromatographic Analysis.

    Science.gov (United States)

    Wojnowski, Wojciech; Majchrzak, Tomasz; Dymerski, Tomasz; Gębicki, Jacek; Namieśnik, Jacek

    2017-11-01

    This work represents a brief summary of the use of dynamic headspace (DHS) as a technique for sample preparation in chromatographic analysis. Despite numerous developments in the area of analyte isolation and enrichment, DHS remains one of the fundamental methods used with GC. In our opinion, interest in this technique will not diminish significantly because it conforms to stipulations of green analytical chemistry. Moreover, DHS fulfills the need for methods that facilitate detection and determination of analytes present at ultratrace levels in complex matrixes. The main focus of this work was placed on the theoretical fundamentals of this method. Also described herein were DHS development, the advantages and disadvantages of this technique compared with other headspace sampling techniques, and selected examples of its applications in food and environmental analyses.

  1. Organic analysis of the headspace of Hanford waste Tank 241-C-103

    International Nuclear Information System (INIS)

    Goheen, S.C.; McVeety, B.D.; Clauss, T.W.; Lucke, R.B.; Ligotke, M.W.; Edwards, J.A.; Fruchter, J.S.

    1996-01-01

    Organic species from the headspace of one Hanford radioactive waste tank are described. Samples were collected either using a sorbent trap or a SUMMA TM canister and were analyzed by gas chromatography and mass spectrometry. The headspace contained several organic components, including alkanes, alkanes, ketones, aldehydes, organic nitriles, and chlorinated hydrocarbons. Sorbent trap samples were designed to collect only normal paraffin hydrocarbons (NPHs). A comparison of NPH data from sorbent traps and SUMMA TM cans revealed results of 693 and 1320 mg/m 3 , NPH respectively. Significant differences were observed in NPH values when samples were collected at different times, or at different locations in the tank. These data suggest either the time of collection, or the position of the sampling device are important variables in the analysis of organic species from Hanford tanks. (author). 16 refs., 3 figs., 2 tabs

  2. Analysis of hydrogen and methane in seawater by "Headspace" method: Determination at trace level with an automatic headspace sampler.

    Science.gov (United States)

    Donval, J P; Guyader, V

    2017-01-01

    "Headspace" technique is one of the methods for the onboard measurement of hydrogen (H 2 ) and methane (CH 4 ) in deep seawater. Based on the principle of an automatic headspace commercial sampler, a specific device has been developed to automatically inject gas samples from 300ml syringes (gas phase in equilibrium with seawater). As valves, micro pump, oven and detector are independent, a gas chromatograph is not necessary allowing a reduction of the weight and dimensions of the analytical system. The different steps from seawater sampling to gas injection are described. Accuracy of the method is checked by a comparison with the "purge and trap" technique. The detection limit is estimated to 0.3nM for hydrogen and 0.1nM for methane which is close to the background value in deep seawater. It is also shown that this system can be used to analyze other gases such as Nitrogen (N 2 ), carbon monoxide (CO), carbon dioxide (CO 2 ) and light hydrocarbons. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Development and validation of automatic HS-SPME with a gas chromatography-ion trap/mass spectrometry method for analysis of volatiles in wines.

    Science.gov (United States)

    Paula Barros, Elisabete; Moreira, Nathalie; Elias Pereira, Giuliano; Leite, Selma Gomes Ferreira; Moraes Rezende, Claudia; Guedes de Pinho, Paula

    2012-11-15

    An automated headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-ion trap/mass spectrometry (GC-IT/MS) was developed in order to quantify a large number of volatile compounds in wines such as alcohols, ester, norisoprenoids and terpenes. The procedures were optimized for SPME fiber selection, pre-incubation temperature and time, extraction temperature and time, and salt addition. A central composite experimental design was used in the optimization of the extraction conditions. The volatile compounds showed optimal extraction using a DVB/CAR/PDMS fiber, incubation of 5 ml of wine with 2g NaCl at 45 °C during 5 min, and subsequent extraction of 30 min at the same temperature. The method allowed the identification of 64 volatile compounds. Afterwards, the method was validated successfully for the most significant compounds and was applied to study the volatile composition of different white wines. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. Fabrication of novel nanoporous array anodic alumina solid-phase microextraction fiber coating and its potential application for headspace sampling of biological volatile organic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Zhuomin [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China); Wang Qingtang [Key Laboratory of Analysis and Detection for Food Safety of Ministry of Education, College of Chemistry and Chemical Engineering, Fuzhou University, Fuzhou, Fujian 350002 (China); Li Gongke, E-mail: cesgkl@mail.sysu.edu.cn [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China)

    2012-05-21

    Highlights: Black-Right-Pointing-Pointer Nanoporous array anodic alumina (NAAA) SPME coating was originally prepared. Black-Right-Pointing-Pointer NAAA SPME coating achieved excellent enrichment capability and selectivity for VOCs. Black-Right-Pointing-Pointer NAAA SPME coating can be applied for the headspace sampling of biological VOCs. - Abstract: In the study, nanoporous array anodic alumina (NAAA) prepared by a simple, rapid and stable two-step anodic oxidization method was introduced as a novel solid-phase microextraction (SPME) fiber coating. The regular nanoporous array structure and chemical composition of NAAA SPME fiber coating was characterized and validated by scanning electron microscopy and energy dispersive spectroscopy, respectively. Compared with the commercial polydimethylsiloxane (PDMS) SPME fiber coating, NAAA SPME fiber coating achieved the higher enrichment capability (1.7-4.7 folds) for the mixed standards of volatile organic compounds (VOCs). The selectivity for volatile alcohols by NAAA SPME fiber coating demonstrated an increasing trend with the increasing polarity of alcohols caused by the gradually shortening carbon chains from 1-undecanol to 1-heptanol or the isomerization of carbon chains of some typical volatile alcohols including 2-ethyl hexanol, 1-octanol, 2-phenylethanol, 1-phenylethanol, 5-undecanol, 2-undecanol and 1-undecanol. Finally, NAAA SPME fiber coating was originally applied for the analysis of biological VOCs of Bailan flower, stinkbug and orange peel samples coupled with gas chromatography-mass spectrometry (GC-MS) detection. Thirty, twenty-seven and forty-four VOCs of Bailan flower, stinkbug and orange peel samples were sampled and identified, respectively. Moreover, the contents of trace 1-octanol and nonanal of real orange peel samples were quantified for the further method validation with satisfactory recoveries of 106.5 and 120.5%, respectively. This work proposed a sensitive, rapid, reliable and convenient

  5. Fabrication of novel nanoporous array anodic alumina solid-phase microextraction fiber coating and its potential application for headspace sampling of biological volatile organic compounds

    International Nuclear Information System (INIS)

    Zhang Zhuomin; Wang Qingtang; Li Gongke

    2012-01-01

    Highlights: ► Nanoporous array anodic alumina (NAAA) SPME coating was originally prepared. ► NAAA SPME coating achieved excellent enrichment capability and selectivity for VOCs. ► NAAA SPME coating can be applied for the headspace sampling of biological VOCs. - Abstract: In the study, nanoporous array anodic alumina (NAAA) prepared by a simple, rapid and stable two-step anodic oxidization method was introduced as a novel solid-phase microextraction (SPME) fiber coating. The regular nanoporous array structure and chemical composition of NAAA SPME fiber coating was characterized and validated by scanning electron microscopy and energy dispersive spectroscopy, respectively. Compared with the commercial polydimethylsiloxane (PDMS) SPME fiber coating, NAAA SPME fiber coating achieved the higher enrichment capability (1.7–4.7 folds) for the mixed standards of volatile organic compounds (VOCs). The selectivity for volatile alcohols by NAAA SPME fiber coating demonstrated an increasing trend with the increasing polarity of alcohols caused by the gradually shortening carbon chains from 1-undecanol to 1-heptanol or the isomerization of carbon chains of some typical volatile alcohols including 2-ethyl hexanol, 1-octanol, 2-phenylethanol, 1-phenylethanol, 5-undecanol, 2-undecanol and 1-undecanol. Finally, NAAA SPME fiber coating was originally applied for the analysis of biological VOCs of Bailan flower, stinkbug and orange peel samples coupled with gas chromatography–mass spectrometry (GC–MS) detection. Thirty, twenty-seven and forty-four VOCs of Bailan flower, stinkbug and orange peel samples were sampled and identified, respectively. Moreover, the contents of trace 1-octanol and nonanal of real orange peel samples were quantified for the further method validation with satisfactory recoveries of 106.5 and 120.5%, respectively. This work proposed a sensitive, rapid, reliable and convenient analytical method for the potential study of trace and small molecular

  6. A comparison of sample preparation methods for extracting volatile organic compounds (VOCs) from equine faeces using HS-SPME.

    Science.gov (United States)

    Hough, Rachael; Archer, Debra; Probert, Christopher

    2018-01-01

    Disturbance to the hindgut microbiota can be detrimental to equine health. Metabolomics provides a robust approach to studying the functional aspect of hindgut microorganisms. Sample preparation is an important step towards achieving optimal results in the later stages of analysis. The preparation of samples is unique depending on the technique employed and the sample matrix to be analysed. Gas chromatography mass spectrometry (GCMS) is one of the most widely used platforms for the study of metabolomics and until now an optimised method has not been developed for equine faeces. To compare a sample preparation method for extracting volatile organic compounds (VOCs) from equine faeces. Volatile organic compounds were determined by headspace solid phase microextraction gas chromatography mass spectrometry (HS-SPME-GCMS). Factors investigated were the mass of equine faeces, type of SPME fibre coating, vial volume and storage conditions. The resultant method was unique to those developed for other species. Aliquots of 1000 or 2000 mg in 10 ml or 20 ml SPME headspace were optimal. From those tested, the extraction of VOCs should ideally be performed using a divinylbenzene-carboxen-polydimethysiloxane (DVB-CAR-PDMS) SPME fibre. Storage of faeces for up to 12 months at - 80 °C shared a greater percentage of VOCs with a fresh sample than the equivalent stored at - 20 °C. An optimised method for extracting VOCs from equine faeces using HS-SPME-GCMS has been developed and will act as a standard to enable comparisons between studies. This work has also highlighted storage conditions as an important factor to consider in experimental design for faecal metabolomics studies.

  7. Headspace Analysis of Volatile Compounds Coupled to Chemometrics in Leaves from the Magnoliaceae Family

    Directory of Open Access Journals (Sweden)

    Mohamed A. Farag

    2015-01-01

    Full Text Available Headspace volatile analysis has been used for volatiles profiling in leaves of 4 Magnolia species with a total of 75 compounds were identified. Monterpene hydrocarbons dominated the volatile blend of M. calophylla (86%, M. acuminata (78%, M. virginiana (70% and M. grandiflora (47% with b -pinene and b -ocimene occurring in the largest amounts, whereas sesquiterpenes were the most abundant compounds in M. grandiflora (39%. High levels of oxygenated compounds were only found in M. virginiana volatile blend (11.4% with 2-phenylethyl alcohol as major component. Hierarchical cluster analysis performed on volatiles content revealed the close relationship between M. acuminata and M. calophylla.

  8. 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.

  9. 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.

  10. Separation and identification of volatile constituents in Artemisia argyi flowers by GC-MS with SPME and steam distillation.

    Science.gov (United States)

    Li, Ning; Mao, Yu; Deng, Chunhui; Zhang, Xiangmin

    2008-01-01

    Artemisia argyi leaf is a widely used traditional Chinese medicine (TCM). In this work, for the first time, the separation and identification of volatile constituents in Artemisia argyi flowers is performed. Gas chromatography-mass spectrometry (GC-MS) with solid-phase microextraction (SPME) is developed for the fast analysis of volatile constituents in the flowers. Several headspace SPME parameters, including fiber coating, extraction temperature, and extraction time, are optimized. Forty-nine compounds in the flowers are re-identified by SPME-GC-MS. At the same time, in order to compare with the SPME, steam distillation is used for analysis of the volatile constituents in the flowers, and forty-seven are detected. The total fifty-three compounds in the flowers, which mainly include cylcofenchene, alpha-pinene, alpha-myrcene, D-limonene, caryophyllene, and germacrene D, are identified by the two methods. Compared to the volatile components in Artemisia argyi leaves, the main components (including the two active compounds of borneol and borneol acetate) are also found in Artemisia argyi flowers. These results show that Artemisia argyi flowers as well as leaves might be used as TCM.

  11. HS-SPME-GC-MS analysis of body odor to test the efficacy of foot deodorant formulations.

    Science.gov (United States)

    Caroprese, Alessandro; Gabbanini, Simone; Beltramini, Claudia; Lucchi, Elena; Valgimigli, Luca

    2009-11-01

    Foot malodor is mostly due to short-chain fatty acids produced by bacterial metabolism of eccrine sweating. We aimed to develop a protocol for an objective (instrumental) efficacy evaluation of foot deodorant formulations. Head-space solid-phase microextractions of target fatty acids from the feet of six healthy volunteers were analyzed by GC-MS. A comparative analysis of the treated vs. the untreated foot was performed in each subject after washing the feet with a physiologic solution and incubating at 36 degrees C for 24-72 h in tryptic soy agar growth medium. Acetic, butyric, isobutyric and isovaleric acids were identified as the main contributors to foot malodor in the majority of volunteers. Propionic, valeric and isocaproic acids were also detected in some subjects. Comparative analysis according to the protocol developed showed a statistically significant (Pdeodorant formulations in human volunteers.

  12. Establishment of Exposure to Organophosphorus Warfare Agents by Means of SPME-GSMS Analysis of Bodily Fluids

    International Nuclear Information System (INIS)

    Saveleva, E. I.; Koryagina, N. L.; Radilov, A. S.; Khlebnikova, N. S.; Khrustaleva, V. S.; Feld, V. E.

    2007-01-01

    Reliable chemical analytical procedures for revealing an exposure to toxic chemicals, identifying the active substance, and assessing the degree of exposure are necessary as a component of medical and forensic activities in cases of the possible use of highly toxic chemicals in war conflicts and terrorism acts, as well as emergency situations in chemical industry, specifically at chemical weapons storage and destruction facilities. According to Chemical Weapons Convention, Part XI, Appendix 4, e-17, 'samples of importance in the investigation of alleged use include biomedical samples from human or animal sources (blood, urine, excreta, tissue etc.)'. Urinary metabolites, O-alkyl esters of methylphosphic acid, offer one of the simplest means of confirming an exposure to organophosphorus warfare agents (OPWA). Urine, unlike blood or tissues, does not require invasive collection demanding in terms of sterility. Excretion with urine is the major route of elimination of OPWA from an organism. According to published data, 90% of OPWA metabolites are excreted within 48-72 h after intoxication. We developed an SPME-GCMS procedure for the determination of O-alkyl esters methylphosphonic acid in urine, with the following detection limits,: isopropyl and isobutyl esters 5 ng/ml and pinacolyl ester 1 ng/ml. The procedure involves derivatization of the target compounds directly on the microfiber. The total analysis time is 1-1.5 h. In animal experiments in vivo we could establish the exposure to OPWA at a half-LD50 level within no less than 48 h after intoxication. In principle, OPWA metabolites could be detected in urine within two weeks after intoxication but at higher doses. Retrospective analysis of urinary metabolites in cases of the exposure to low doses of OPWA requires lower detection limits (0.1-1 ng/ml). Optimal objects for the retrospective analysis of OPWA in an organism are long-lived blood protein adducts. We developed a procedure for revealing an exposure to

  13. Analysis of Listeria using exogenous volatile organic compound metabolites and their detection by static headspace-multi-capillary column-gas chromatography-ion mobility spectrometry (SHS-MCC-GC-IMS).

    Science.gov (United States)

    Taylor, Carl; Lough, Fraser; Stanforth, Stephen P; Schwalbe, Edward C; Fowlis, Ian A; Dean, John R

    2017-07-01

    Listeria monocytogenes is a Gram-positive bacterium and an opportunistic food-borne pathogen which poses significant risk to the immune-compromised and pregnant due to the increased likelihood of acquiring infection and potential transmission of infection to the unborn child. Conventional methods of analysis suffer from either long turn-around times or lack the ability to discriminate between Listeria spp. reliably. This paper investigates an alternative method of detecting Listeria spp. using two novel enzyme substrates that liberate exogenous volatile organic compounds in the presence of α-mannosidase and D-alanyl aminopeptidase. The discriminating capabilities of this approach for identifying L. monocytogenes from other species of Listeria are investigated. The liberated volatile organic compounds (VOCs) are detected using an automated analytical technique based on static headspace-multi-capillary column-gas chromatography-ion mobility spectrometry (SHS-MCC-GC-IMS). The results obtained by SHS-MCC-GC-IMS are compared with those obtained by the more conventional analytical technique of headspace-solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS). The results found that it was possible to differentiate between L. monocytogenes and L. ivanovii, based on their VOC response from α-mannosidase activity.

  14. Headspace Solid-Phase Microextraction Analysis of Volatile Components in Phalaenopsis Nobby’s Pacific Sunset

    Directory of Open Access Journals (Sweden)

    Chih-Hsin Yeh

    2014-09-01

    Full Text Available Phalaenopsis is the most important economic crop in the Orchidaceae family. There are currently numerous beautiful and colorful Phalaenopsis flowers, but only a few species of Phalaenopsis have an aroma. This study reports the analysis volatile components present in P. Nobby’s Pacific Sunset by solid-phase microextraction (SPME coupled with gas chromatography (GC and gas chromatography/mass spectrometry (GC-MS. The results show that the optimal extraction conditions were obtained by using a DVB/CAR/PDMS fiber. A total of 31 compounds were identified, with the major compounds being geraniol, linalool and α-farnesene. P. Nobby’s Pacific Sunset had the highest odor concentration from 09:00 to 13:00 on the eighth day of storage. It was also found that in P. Nobby’s Pacific Sunset orchids the dorsal sepals and petals had the highest odor concentrations, whereas the column had the lowest.

  15. SPME GC/MS determination of organochlorine pesticides in water samples

    Directory of Open Access Journals (Sweden)

    Yerbolat Sailaukhanuly

    2013-05-01

    Full Text Available Headspace solid phase microextraction (HS-SPME in combination with gas chromatography and mass-spectrometry (GC/MS was studied for analysis of water samples. The organochlorine pesticides (OCPs, p,p'-DDT, p,p'-DDD, and p,p'-DDE were collected and analyzed by GC/MS. To select of effective fiber coatings four types of SPME fibers were examined and compared. The parameters effecting the efficiency of HS-SPME such as extraction and pre-incubation time and extraction temperature, effect of solvent nature, ionic strength were studied to obtain optimal parameters. The method was developed using spiked water samples in a concentration range  10 - 500 ng/L. The calibration curve was linear over the studied concentration range with r≥0.9925. The detection limits varied from 1.57 to 2.08 ng/L. An authentic water samples from contaminated lake with OCPs were analyzed by developed method.

  16. 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

  17. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. 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.

  19. Analysis of residual toluene in food packaging via headspace extraction method using gas chromatography

    International Nuclear Information System (INIS)

    Lim, Ying Chin; Mohd Marsin Sanagi

    2008-01-01

    Polymeric materials are used in many food contact applications as packaging material. The presence of residual toluene in this food packaging material can migrate into food and thus affect the quality of food. In this study, a manual headspace analysis was successfully designed and developed. The determination of residual toluene was carried out with standard addition method and multiple headspace extraction, MHE) method using gas chromatography-flame ionization detector, GC-FID). Identification of toluene was performed by comparison of its retention time with standard toluene and GC-MS. It was found that the suitable heating temperature was 180 degree Celsius with an optimum heating time of 10 minutes. The study also found that the concentration of residual toluene in multicolored sample was higher compared to mono colored sample whereas residual toluene in sample analyzed using standard addition method was higher compared to MHE method. However, comparison with the results obtained from De Paris laboratory, France found that MHE method gave higher accuracy for sample with low analyte concentration. On the other hand, lower accuracy was obtained for sample with high concentration of residual toluene due to systematic errors. Comparison between determination methods showed that MHE method is more precise compared to standard addition method. (author)

  20. 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

  1. Analysis of tetramethylene disulfotetramine in foods using solid-phase microextraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    De Jager, Lowri S; Perfetti, Gracia A; Diachenko, Gregory W

    2008-05-23

    An automated solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) method for the determination of tetramethylene disulfotetramine in foods was developed. A comparison of direct immersion (DI) and headspace (HS) extraction techniques using a 70microm carbowax/divinylbenzene (CW/DVB) fiber is presented. The optimized DI-SPME method provided an aqueous extraction limit of detection (LOD) of 9.0ng/g while the HS-SPME LOD was 2.7ng/g. In both SPME modes, recovery was highly matrix dependent and quantification requires standard addition calibrations. Analysis of foods using DI-SPME encountered many obstacles including fiber fouling, low recovery and poor reproducibility. HS-SPME was successfully applied to food analysis with minimal interferences. Standard addition calibration curves for foods gave high linearity (R2>0.98), reproducibility (RSD<12%) and sensitivity with LODs ranging from 0.9 to 4.3ng/g.

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

    International Nuclear Information System (INIS)

    Costa, Rosaria; Tedone, Laura; De Grazia, Selenia; Dugo, Paola; Mondello, Luigi

    2013-01-01

    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

  3. 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.

  4. Optimisation and validation of a HS-SPME-GC-IT/MS method for analysis of carbonyl volatile compounds as biomarkers in human urine: Application in a pilot study to discriminate individuals with smoking habits.

    Science.gov (United States)

    Calejo, Isabel; Moreira, Nathalie; Araújo, Ana Margarida; Carvalho, Márcia; Bastos, Maria de Lourdes; de Pinho, Paula Guedes

    2016-02-01

    A new and simple analytical approach consisting of an automated headspace solid-phase microextraction (HS-SPME) sampler coupled to gas chromatography-ion trap/mass spectrometry detection (GC-IT/MS) with a prior derivatization step with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) was developed to detect volatile carbonyl metabolites with low molecular weights in human urine. A central composite design (CCD) was used to optimise the PFBHA concentration and extraction conditions that affect the efficiency of the SPME procedure. With a sample volume of 1 mL, optimal conditions were achieved by adding 300 mg/L of PFBHA and allowing the sample to equilibrate for 6 min at 62°C and then extracting the samples for 51 min at the same temperature, using a divinylbenzene/polydimethylsiloxane (DVB/PDMS) fibre. The method allowed the simultaneous identification and quantification of 44 carbonyl compounds consisting of aldehydes, dialdehydes, heterocyclic aldehydes and ketones. The method was validated with regards to the linearity, inter- and intra-day precision and accuracy. The detection limits ranged from 0.009 to 0.942 ng/mL, except for 4-hydroxy-2-nonenal (15 ng/mL), and the quantification limits varied from 0.029 to 1.66 ng/mL, except for butanal (2.78 ng/mL), 2-butanone (2.67 ng/mL), 4-heptanone (3.14 ng/mL) and 4-hydroxy-2-nonenal (50.0 ng/mL). The method accuracy was satisfactory, with recoveries ranging from 90 to 107%. The proof of applicability of the methodology was performed in a pilot target analysis of urine samples obtained from 18 healthy smokers and 18 healthy non-smokers (control group). Chemometric supervised analysis was performed using the volatile patterns acquired for these samples and clearly showed the potential of the volatile carbonyl profiles to discriminate urine from smoker and non-smoker subjects. 5-Methyl-2-furfural (p<0.0001), 2-methylpropanal, nonanal and 2-methylbutanal (p<0.05) were identified as potentially useful

  5. Comparison of membrane assisted solvent extraction, stir bar sorptive extraction, and solid phase microextraction in analysis of tetramine in food.

    Science.gov (United States)

    De Jager, Lowri S; Perfetti, Gracia A; Diachenko, Gregory W

    2009-04-01

    Three environmentally friendly extraction techniques, membrane assisted solvent extraction (MASE), stir bar sorptive extraction (SBSE), and headspace solid phase microextraction (HS-SPME), were compared for the direct analysis of the highly toxic rodenticide tetramine in food. The optimized MASE method was applied to seven foods fortified with tetramine and compared to previously reported SBSE and HS-SPME results. Parameters such as the standard addition linearity (MASE (0.964-0.999), SBSE (0.966-0.999), HS-SPME (0.955-0.999)), recovery (MASE (12-86%), SBSE (36-130%), HS-SPME (50-200%)), reproducibility (MASE (3.0-30%), SBSE (4.4-9.6%), HS-SPME (1-12%)), and LOD (MASE (1.6-6.4 ng/g), SBSE (0.2-2.1 ng/g), HS-SPME (0.9-4.3 ng/g)) were compared.

  6. Ultra trace analysis of PAHs by designing simple injection of large amounts of analytes through the sample reconcentration on SPME fiber after magnetic solid phase extraction.

    Science.gov (United States)

    Khodaee, Nader; Mehdinia, Ali; Esfandiarnejad, Reyhaneh; Jabbari, Ali

    2016-01-15

    A simple solventless injection method was introduced based on the using of a solid-phase microextraction (SPME) fiber for injection of large amounts of the analytes extracted by the magnetic solid phase extraction (MSPE) procedure. The resulted extract from MSPE procedure was loaded on a G-coated SPME fiber, and then the fiber was injected into the gas chromatography (GC) injection port. This method combines the advantages of exhaustive extraction property of MSPE and the solvent-less injection of SPME to improve the sensitivity of the analysis. In addition, the analytes were re-concentrated prior to inject into the gas chromatography (GC) inlet because of the organic solvent removing from the remaining extract of MSPE technique. Injection of the large amounts of analytes was made possible by using the introduced procedure. Fourteen polycyclic aromatic hydrocarbons (PAHs) with different volatility were used as model compounds to investigate the method performance for volatile and semi-volatile compounds. The introduced method resulted in the higher enhancement factors (5097-59376), lower detection limits (0.29-3.3pgmL(-1)), and higher sensitivity for the semi-volatile compounds compared with the conventional direct injection method. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Comparative analysis of the vapor headspace of military-grade TNT versus NESTT TNT under dynamic and static conditions

    Science.gov (United States)

    Edge, Cindy C.; Gibb, Julie; Wasserzug, Louis S.

    1998-09-01

    The Institute for Biological Detection Systems (IBDS) has developed a quantitative vapor delivery system that can aid in characterizing dog's sensitivity and ability to recognize odor signatures for explosives and contraband substances. Determining of the dog's odor signature for detection of explosives is important because it may aid in eliminating the risk of handling explosives and reducing cross-contamination. Progress is being made in the development of training aids that represent the headspace of the explosives. NESTTTM TNT materials have been proposed as an approach to developing training aid simulates. In order for such aids to be effective they must mimic the headspace of the target material. This study evaluates the NESTTTM TNT product with regard to this criterion. NESTTTM TNT vapor was generated by the IBDS vapor delivery system, which incorporates a vapor generation cell that enables the user to control the conditions under which a substance is tested. The NESTTTM TNT vapor was compared to the headspace of military-grade TNT. The findings identify and quantify major vapor constituents of military-grade TNT and NESTTTM TNT. A comparative analysis evaluated the degree to which the NESTTTM TNT mimics the headspace of an actual TNT sample.

  8. UPTAKE OF RADIONUCLIDE METALS BY SPME FIBERS

    Energy Technology Data Exchange (ETDEWEB)

    Duff, M; S Crump, S; Robert02 Ray, R; Keisha Martin, K; Donna Beals, D

    2006-08-28

    The Federal Bureau of Investigation (FBI) Laboratory currently does not have on site facilities for handling radioactive evidentiary materials and there are no established FBI methods or procedures for decontaminating high explosive (HE) and fire debris (FD) evidence while maintaining evidentiary value. One experimental method for the isolation of HE and FD residue involves using solid phase microextraction or SPME fibers to remove residue of interest. Due to their high affinity for organics, SPME fibers should have little affinity for most metals. However, no studies have measured the affinity of radionuclides for SPME fibers. The focus of this research was to examine the affinity of dissolved radionuclide ({sup 239/240}Pu, {sup 238}U, {sup 237}Np, {sup 85}Sr, {sup 133}Ba, {sup 137}Cs, {sup 60}Co and {sup 226}Ra) and stable radionuclide surrogate metals (Sr, Co, Ir, Re, Ni, Ba, Cs, Nb, Zr, Ru, and Nd) for SPME fibers at the exposure conditions that favor the uptake of HE and FD residues. Our results from radiochemical and mass spectrometric analyses indicate these metals have little measurable affinity for these SPME fibers during conditions that are conducive to HE and FD residue uptake with subsequent analysis by liquid or gas phase chromatography with mass spectrometric detection.

  9. 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.

  10. Analysis of volatile headspace gases sampled by cryogenic traps from Westinghouse Hanford Company Tank 242-C-112 March 1992

    International Nuclear Information System (INIS)

    Lucke, R.B.; Clauss, S.A.

    1993-10-01

    Results are given from gas chromatography/mass spectrometry (GC/MS) analyses of the headspace samples obtained by using cryogenic traps from Westinghouse Hanford Company (WHC) Tank 112-C during the month of March, 1992. Samples were analyzed as received with no sample preparation. Analyses included direct GC/MS for volatile/semivolatile components, and direct GC/MS for ammonia. Purge and trap GC/MS analysis was not done. In addition, aliquots were sent to Karl Pool, Pacific Northwest Laboratory, for hydrogen cyanide analysis by ion chromatography, the results are reported here. All concentrations are reported for the methanol extract solutions. To calculate concentrations in the headspace, the cryo-sampling air volume and the methanol rinse volume must be obtained from cryo-sampling personnel at WHC. Triplicate analyses were done on all samples, and average concentrations and standard deviations are reported. One significant result was that no ammonia was detected

  11. Field portable low temperature porous layer open tubular cryoadsorption headspace sampling and analysis part I: Instrumentation.

    Science.gov (United States)

    Bruno, Thomas J

    2016-01-15

    Building on the successful application in the laboratory of PLOT-cryoadsorption as a means of collecting vapor (or headspace) samples for chromatographic analysis, in this paper a field portable apparatus is introduced. This device fits inside of a briefcase (aluminum tool carrier), and can be easily transported by vehicle or by air. The portable apparatus functions entirely on compressed air, making it suitable for use in locations lacking electrical power, and for use in flammable and explosive environments. The apparatus consists of four aspects: a field capable PLOT-capillary platform, the supporting equipment platform, the service interface between the PLOT-capillary and the supporting equipment, and the necessary peripherals. Vapor sampling can be done with either a hand piece (containing the PLOT capillary) or with a custom fabricated standoff module. Both the hand piece and the standoff module can be heated and cooled to facilitate vapor collection and subsequent vapor sample removal. The service interface between the support platform and the sampling units makes use of a unique counter current approach that minimizes loss of cooling and heating due to heat transfer with the surroundings (recuperative thermostatting). Several types of PLOT-capillary elements and sampling probes are described in this report. Applications to a variety of samples relevant to forensic and environmental analysis are discussed in a companion paper. Published by Elsevier B.V.

  12. SOLID PHASE MICRO EXTRACTION (SPME) FLAVOR ANALYSIS OF APPLE JUICE AND COFFEE MIXTURES USING GAS CHROMATOGRAPHY-MASS SPECTROMETRY (GC-MS)

    OpenAIRE

    Mi Ja Kim; Jeehyun Lee; Jaeyoung Byun; Sunmi Choi; Wonsik Choi

    2016-01-01

    This research was conducted to evaluate the flavor of apple juice and coffee mixtures and the sensory quality of SPME extracts using gas chromatography-mass spectrometry (GC-MS). Three samples with different compositions were examined. Sample A1 contained85% apple juiceand 15% coffee, sample A2 had87.5% apple and 12.5% coffee, and sample A3 had90% apple juiceand 10% coffee. The sensory analysis involved 100 panelists and a sequential monadic test. Sample presentation orders were balanced in ...

  13. Analysis of Odor-Causing VOCs and Semi-VOCs Associated with Particulate Matter in Swine Barns Using SPME-GC-MS-Olfactometry

    Science.gov (United States)

    Cai, Lingshuang; Koziel, Jacek A.; Lo, Yin-Cheung; Hoff, Steven J.

    2009-05-01

    Swine operations can affect air quality by emissions of odor, volatile organic compounds (VOCs) and other gases, and particulate matter (PM). Particulate matter has been proposed to be an important pathway for carrying odor. However, little is known about the odor-VOCs-PM interactions. In this research, continuous PM sampling was conducted simultaneously with three collocated TEOM analyzers inside a 1000-head swine finish barn located in central Iowa. Each TEOM (tapered element oscillating microbalance) was fitted with total suspended particulate (TSP), PM-10, PM-2.5 and PM-1 preseparators. Used filters were stored in 40 mL vials and transported to the laboratory. VOCs adsorbed/absorbed to dust were allowed to equilibrate with vial headspace. Solid-phase microextraction (SPME) Carboxen/polydimethylsiloxane(PDMS) 85 μm fibers were used to extract VOCs. Simultaneous chemical and olfactometry analyses of VOCs and odor associated with swine PM were completed using a gas chromatography-mass-olfactometry (GC-MS-O) system. Fifty VOCs categorized into nine chemical function groups were identified and confirmed with standards. Five of them are classified as hazardous air pollutants. VOCs were characterized with a wide range of molecular weight, boiling points, vapor pressures, water solubilities, odor detection thresholds, and atmospheric reactivities. All characteristic swine VOCs and odorants were present in PM and their abundance was proportional to PM size. However, the majority of VOCs and characteristic swine odorants were preferentially bound to smaller-size PM. The findings indicate that a significant fraction of swine odor can be carried by PM. Research of the effects of PM control on swine odor mitigation is warranted.

  14. Essential oil from Rhaponticum acaule L. roots: Comparative study using HS-SPME/GC/GC–MS and hydrodistillation techniques

    Directory of Open Access Journals (Sweden)

    Batoul Benyelles

    2014-12-01

    Full Text Available The composition of essential oil extracted from Rhaponticum acaule L. roots growing wild in Algeria was studied by hydrodistillation (HD and by Head-Space Solid Phase Micro-Extraction (HS-SPME. Quantitative but not qualitative differences have been found in the chemical composition of both analysed samples depending on the extraction method. However, the oil obtained from R. acaule roots shows that aliphatic alcohols were found to be the major class (69.2%, followed by the terpenes (5.5%, alkenes (5.2% and alkynes (4.0%. In both cases the analysis were carried out using Gas Chromatography (GC and Gas Chromatography–Mass Spectrometry (GC–MS. Our study shows that HS-SPME extraction could be considered as an alternative technique for the isolation of volatiles from plant. 25 components were identified in oil vs. 39 in the HS-SPME. However the oil composition of roots was mainly represented by a variety of aliphatic hydrocarbons (alcohols, aldehydes and ketones and terpenes which are known for their antimicrobial activities.

  15. Reliability of fibres in solid-phase microextraction for routine analysis of the headspace of aromatic and medicinal plants.

    Science.gov (United States)

    Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Sgorbini, Barbara; Rubiolo, Patrizia

    2007-06-08

    This article evaluates the HS-SPME recovery repeatability, intermediate precision and their performance over time when applied to HS-SPME sampling for quality control of medicinal and aromatic plants. Experiments were carried out on two sets of fibres coated with two different coatings and belonging to different lots (i.e 100 microm polydimethylsyloxane (PDMS) and Carboxen/divinylbenzene/PDMS 50/30 microm, l: 1 cm (CAR/DVB/PDMS)) and on chamomile (Matricaria chamomilla L.), sage (Salvia lavandulifolia Vahl.) and a standard solution containing 3-hexanol, isoamyl acetate, 1,8-cineole and menthol in diisobutyl phthalate. The performance of each set of fibres was evaluated by determining a group of complementary statistical parameters including: (i) repeatability of the absolute areas of each marker from each matrix with each fibre; (ii) intra-fibre repeatability of the total absolute areas of the markers of each matrix obtained with each fibre of each set; (iii) inter-fibre intermediate precision of the total absolute areas of the markers of each matrix obtained with all fibres of each set; and (iv) analysis of variance by one-way ANOVA with Fisher and Tukey tests. The influence of the number of analyses on fibre effectiveness (fibre life-time) was studied by linear regression analysis (LRA). The results proved that HS-SPME can successfully be used for routine control analysis of aromatic ad medicinal plants since both types of fibres showed good repeatability and intermediate precision of analytes recovery and consistency over time. Unlike data previously reported by other authors, CAR/DVB/PDMS coated fibres gave better results than those coated with PDMS. The fibre-life seemed mainly to be influenced by the number and conditions of samplings and nature of the matrix investigated.

  16. Determination of 2,5-hexanedione in urine by headspace solid-phase microextraction and gas chromatography.

    Science.gov (United States)

    Oliveira, Antônio Felipe F; Maia, Patrícia P; Paiva, Maria José N; Siqueira, Maria Elisa P B

    2009-05-01

    2,5-Hexanedione (2,5-HD) is the most important metabolite of n-hexane and methyl ethyl ketone in human urine. Urinary 2,5-HD is used as a biomarker for biological monitoring of workers exposed to n-hexane. A simple method using headspace solid-phase microextraction (HS-SPME) and gas chromatography (GC) equipped with a flame-ionization detector (FID) was developed. The parameters that affect the HS-SPME-GC-FID process were optimized (i.e., fiber coating, sample volume, adsorption and heating time, salt addition, and extraction temperature). The assay presented linearity in the range of 0.075 to 20.0 mg/L, precision (coefficient of variation L for 2,5-HD in urine. The method was successfully applied to the analysis of 2,5-HD in urine samples from eight workers occupationally exposed to n-hexane in shoemaker's glue.

  17. An improved method for the analysis of 2-aminoacetophenone in wine based on headspace solid-phase microextraction and heart-cut multidimensional gas chromatography with selective detection by tandem mass spectrometry.

    Science.gov (United States)

    Schmarr, Hans-Georg; Keiser, Jutta; Krautwald, Susann

    2016-12-16

    Heart-cut multidimensional gas chromatography coupled to selective mass spectrometric detection (H/C MDGC-MS-MS) was shown to be a suitable combination for analysis of the key component for the wine off-flavor named "atypical aging off-flavor" (german: "Untypische Alterungsnote", UTA), 2-aminoacetophenone (2-AAP). Headspace solid phase microextraction (HS-SPME) was applied as an easy to automate sample preparation step suiting routine control situations. During method development two critical aspects were found, of which one is the chemical degradation of the neat substance, leading to signal reduction and a false response behavior. A second aspect is the pH stability of the deuterated isotopologue 1-(2-aminophenyl)-2,2,2-trideuterio-ethanone (2-AAP-d3) used for quantification via a stable isotope dilution assay. Despite an earlier suggestion to increase the extractable amount of 2-AAP and its isotopic standard in the headspace, alkalization of 2-AAP-d3 containing aqueous samples were found to be critical. In such a milieu a deuterium exchange can then cause erroneous quantitative results. The method proposed in our study thus uses native wine pH conditions and proved to be suitable for routine control with respect to the detection of the "atypical aging off-flavor" in wine at concentration levels below its sensory threshold of about 1μgL -1 . Good linearity was obtained in the calibrated range from 0.1-8μgL -1 (y=1,2338x+0,1029, R=0,9985) with limits of detection or quantification being 0.01 and 0.14μg/L, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Second order kinetic modeling of headspace solid phase microextraction of flavors released from selected food model systems.

    Science.gov (United States)

    Zhang, Jiyuan; Cheong, Mun-Wai; Yu, Bin; Curran, Philip; Zhou, Weibiao

    2014-09-04

    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.

  19. 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.

  20. A preconcentrator chip employing μ-SPME array coated with in-situ-synthesized carbon adsorbent film for VOCs analysis.

    Science.gov (United States)

    Wong, Ming-Yee; Cheng, Wei-Rui; Liu, Mao-Huang; Tian, Wei-Cheng; Lu, Chia-Jung

    2012-11-15

    We report the design, fabrication, and evaluation of a μ-preconcentrator chip that utilizes an array of solid-phase microextraction (SPME) needles coated with in-situ-grown carbon adsorbent film. The structure of the SPME needle (diameter=100 μm, height=250 μm) array inside the sampling chamber was fabricated using a deep reactive-ion etching (DRIE) process to enhance the attachable surface area for adsorbent film. Heaters and temperature sensors were fabricated onto the back of a μ-preconcentrator chip using lithography patterning and a metal lift-off process. The devices were sealed by anodic bonding and diced prior to the application of the adsorbent film. An adsorbent precursor, cellulose was dissolved in water and dynamically coated onto the SPME needle array. The coated cellulose film was converted into a porous carbon film via pyrolysis at 600 °C in a N(2) atmosphere. The surface area of the carbon adsorbent film was 308 m(2)/g, which is higher than that of a commercial adsorbent Carbopack X. A preconcentration factor as high as 13,637-fold was demonstrated using toluene. Eleven volatile organic compounds (VOCs) of different volatilities and functional groups were sampled and analyzed by GC-FID, and the desorption peak widths at half height were all less than 2.6 s after elution from a 15m capillary GC column. There was no sign of performance degradation after continuous operation for 50 cycles in air. Copyright © 2012 Elsevier B.V. All rights reserved.

  1. Volatile Hydrocarbon Analysis in Blood by Headspace Solid-Phase Microextraction: The Interpretation of VHC Patterns in Fire-Related Incidents.

    Science.gov (United States)

    Waters, Brian; Hara, Kenji; Ikematsu, Natsuki; Takayama, Mio; Kashiwagi, Masayuki; Matsusue, Aya; Kubo, Shin-Ichi

    2017-05-01

    A headspace solid-phase microextraction (HS-SPME) technique was used to quantitate the concentration of volatile hydrocarbons from the blood of cadavers by cryogenic gas chromatography-mass spectroscopy. A total of 24 compounds including aromatic and aliphatic volatile hydrocarbons were analyzed by this method. The analytes in the headspace of 0.1 g of blood mixed with 1.0 mL of distilled water plus 1 µL of an internal standard solution were adsorbed onto a 100-µm polydimethylsiloxane fiber at 0°C for 15 min, and measured using a GC-MS full scan method. The limit of quantitation for the analytes ranged from 6.8 to 10 ng per 1 g of blood. This method was applied to actual autopsy cases to quantitate the level of volatile hydrocarbons (VHCs) in the blood of cadavers who died in fire-related incidents. The patterns of the VHCs revealed the presence or absence of accelerants. Petroleum-based fuels such as gasoline and kerosene were differentiated. The detection of C8-C13 aliphatic hydrocarbons indicated the presence of kerosene; the detection of C3 alkylbenzenes in the absence of C8-C13 aliphatic hydrocarbons was indicative of gasoline; and elevated levels of styrene or benzene in the absence of C3/C4 alkylbenzenes and aliphatic hydrocarbons indicated a normal construction fire. This sensitive HS-SPME method could help aid the investigation of fire-related deaths by providing a simple pattern to use for the interpretation of VHCs in human blood. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  2. A rapid analysis of plasma/serum ethylene and propylene glycol by headspace gas chromatography.

    Science.gov (United States)

    Ehlers, Alexandra; Morris, Cory; Krasowski, Matthew D

    2013-12-01

    A rapid headspace-gas chromatography (HS-GC) method was developed for the analysis of ethylene glycol and propylene glycol in plasma and serum specimens using 1,3-propanediol as the internal standard. The method employed a single-step derivitization using phenylboronic acid, was linear to 200 mg/dL and had a lower limit of quantitation of 1 mg/dL suitable for clinical analyses. The analytical method described allows for laboratories with HS-GC instrumentation to analyze ethanol, methanol, isopropanol, ethylene glycol, and propylene glycol on a single instrument with rapid switch-over from alcohols to glycols analysis. In addition to the novel HS-GC method, a retrospective analysis of patient specimens containing ethylene glycol and propylene glycol was also described. A total of 36 patients ingested ethylene glycol, including 3 patients who presented with two separate admissions for ethylene glycol toxicity. Laboratory studies on presentation to hospital for these patients showed both osmolal and anion gap in 13 patients, osmolal but not anion gap in 13 patients, anion but not osmolal gap in 8 patients, and 1 patient with neither an osmolal nor anion gap. Acidosis on arterial blood gas was present in 13 cases. Only one fatality was seen; this was a patient with initial serum ethylene glycol concentration of 1282 mg/dL who died on third day of hospitalization. Propylene glycol was common in patients being managed for toxic ingestions, and was often attributed to iatrogenic administration of propylene glycol-containing medications such as activated charcoal and intravenous lorazepam. In six patients, propylene glycol contributed to an abnormally high osmolal gap. The common presence of propylene glycol in hospitalized patients emphasizes the importance of being able to identify both ethylene glycol and propylene glycol by chromatographic methods.

  3. Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation.

    Science.gov (United States)

    Musumeci, Lauren E; Ryona, Imelda; Pan, Bruce S; Loscos, Natalia; Feng, Hui; Cleary, Michael T; Sacks, Gavin L

    2015-07-06

    Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH), 3-mercaptohexylacetate (3-MHA), and 4-mercapto-4-methyl-2-pentanone (4-MMP)) are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography electron impact mass spectrometry (GC-EI-MS). We describe a method in which thiols are converted to pentafluorobenzyl (PFB) derivatives by extractive alkylation and the organic layer is evaporated prior to headspace solid phase microextraction (HS-SPME) and GC-EI-MS analysis. Optimal parameters were determined by response surface area modeling. The addition of NaCl solution to the dried SPME vials prior to extraction resulted in up to less than fivefold improvement in detection limits. Using 40 mL wine samples, limits of detection for 4-MMP, 3-MH, and 3-MHA were 0.9 ng/L, 1 ng/L, and 17 ng/L, respectively. Good recovery (90%-109%) and precision (5%-11% RSD) were achieved in wine matrices. The new method was used to survey polyfunctional thiol concentrations in 61 commercial California and New York State wines produced from V. vinifera (Riesling, Gewürztraminer, Cabernet Sauvignon, Sauvignon blanc and non-varietal rosé wines), V. labruscana (Niagara), and Vitis spp. (Cayuga White). Mean 4-MMP concentrations in New York Niagara (17 ng/L) were not significantly different from concentrations in Sauvignon blanc, but were significantly higher than 4-MMP in other varietal wines.

  4. The dynamics of the HS/SPME-GC/MS as a tool to assess the spoilage of minced beef stored under different packaging and temperature conditions.

    Science.gov (United States)

    Argyri, Anthoula A; Mallouchos, Athanasios; Panagou, Efstathios Z; Nychas, George-John E

    2015-01-16

    The aim of the current study was to assess meat spoilage through the evolution of volatile compounds using chemometrics. Microbiological and sensory assessment, pH measurement and headspace solid phase microextraction gas chromatography/mass spectroscopy (headspace SPME-GC/MS) analysis were carried out in minced beef stored aerobically and under modified atmosphere packaging (MAP) at 0, 5, 10, and 15 °C. It was shown that the HS/SPME-GC/MS analysis provided useful information about a great number of volatile metabolic compounds detected during meat storage. Many of the identified and semi-quantified compounds were correlated with the sensory scores through the use of chemometrics, depicting possible spoilage indicators such as 2-pentanone, 2-nonanone, 2-methyl-1-butanol, 3-methyl-1-butanol, ethyl hexanoate, ethyl propanoate, ethyl lactate, ethyl acetate, ethanol, 2-heptanone, 3-octanone, diacetyl, and acetoin. Finally, the applied GC/MS global models were able to estimate the microbial counts of the different microorganisms and the sensory scores of a meat sample regardless of storage conditions (i.e. packaging and temperature). Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Comparison of Ultrasound-Assisted Headspace Solid-Phase Microextraction and Hydrodistillation for the Identification of Major Constituents in Two Species of Hypericum.

    Science.gov (United States)

    Ghiasvand, Alireza; Shadabi, Shahriar; Hajipour, Somayeh; Nasirian, Afagh; Borzouei, Mohammad; Hassani-Moghadam, Esfandyar; Hashemi, Payman

    2016-02-01

    Ultrasound-assisted headspace solid-phase microextraction (UA-HS-SPME) and hydrodistillation (HD) methods, coupled to gas chromatography-mass spectrometry (GC-MS), were used for the extraction and analysis of volatile compounds from Hypericum perforatum and Hypericum scabrum collected from two different sites in Iran. In the UA-HS-SPME method, various experimental parameters such as the type of fiber coating, sonication time, extraction time, extraction temperature and desorption time were investigated. The highest extraction efficiency was achieved by a 100-µm polydimethylsiloxane (PDMS) fiber. Consequently, 36 compounds were identified in H. perforatum and H. scabrum samples, using the UA-HS-SPME-GC-MS method, of which 14 were the same in both species. On the other hand, 57 compounds of these species were identified by the HD-GC-MS method, of which 21 were the same. The predominant constituents identified using the UA-HS-SPME method in H. perforatum included β-caryophyllene, α-pinene, γ-cadinene, α-selinene, germacrene-D, limonene and myrcene, and in H. scabrum were α-pinene, nonane, β-pinene and limonene. The common constituents identified by the HD-GC-MS method for H. perforatum involved germacrene-D, limonene, β-caryophyllene, α-pinene, β-pinene and germacrene-B, and for H. scabrum were α-pinene, β-pinene, germacrene-D, nonane, limonene and γ-cadinene. The results about the main constituents of the examined species correspond to the findings of other researchers. Additionally, comparing UA-HS-SPME-GC-MS and HD-GC-MS methods showed that the UA-HS-SPME-GC-MS method is much faster and simpler, and it requires much less sample size and lower temperature. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  6. Analysis of volatile compounds in gluten-free bread crusts with an optimised and validated SPME-GC/QTOF methodology.

    Science.gov (United States)

    Pico, Joana; Antolín, Beatriz; Román, Laura; Gómez, Manuel; Bernal, José

    2018-04-01

    The aroma of bread crust, as one of the first characteristics perceived, is essential for bread acceptance. However, gluten-free bread crusts exhibit weak aroma. A SPME-GC/QTOF methodology was optimised with PCA and RSM and validated for the quantification of 44 volatile compounds in bread crust, extracting 0.75 g of crust at 60 °C for 51 min. LODs ranged between 3.60 and 1760 μg Kg -1 , all the R 2 were higher than 0.99 and %RSD for precision and %Er for accuracy were lower than 9% and 12%, respectively. A commercial wheat bread crust was quantified, and furfural was the most abundant compound. Bread crusts of wheat starch and of japonica rice, basmati rice and teff flours were also quantified. Teff flour and wheat starch crusts were very suitable for improving gluten-free bread crust aroma, due to their similar content in 2-acetyl-1-pyrroline and 4-hydroxy-2,5-dimethyl-3(2H)-furanone compared to wheat flour crust and also for their high content in pyrazines. Copyright © 2018 Elsevier Ltd. All rights reserved.

  7. Experimental design-based isotope-dilution SPME-GC/MS method development for the analysis of smoke flavouring products.

    Science.gov (United States)

    Giri, Anupam; Zelinkova, Zuzana; Wenzl, Thomas

    2017-12-01

    For the implementation of Regulation (EC) No 2065/2003 related to smoke flavourings used or intended for use in or on foods a method based on solid-phase micro extraction (SPME) GC/MS was developed for the characterisation of liquid smoke products. A statistically based experimental design (DoE) was used for method optimisation. The best general conditions to quantitatively analyse the liquid smoke compounds were obtained with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre, 60°C extraction temperature, 30 min extraction time, 250°C desorption temperature, 180 s desorption time, 15 s agitation time, and 250 rpm agitation speed. Under the optimised conditions, 119 wood pyrolysis products including furan/pyran derivatives, phenols, guaiacol, syringol, benzenediol, and their derivatives, cyclic ketones, and several other heterocyclic compounds were identified. The proposed method was repeatable (RSD% method proved to be fit for purpose, allowing the rapid identification and quantification of volatile compounds in liquid smoke flavourings.

  8. 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.)

  9. 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

    2017-09-01

    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 CO 2 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 CO 2 formed from the oxidation reaction between wheat flour and potassium dichromate in an acidic condition.

  10. 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.

  11. 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. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Validation of SPME-GCMS method for the analysis of virgin olive oil volatiles responsible for sensory defects.

    Science.gov (United States)

    Romero, I; García-González, D L; Aparicio-Ruiz, R; Morales, M T

    2015-03-01

    Volatile compounds are responsible for the aroma of virgin olive oil and also for its quality. The high number and different nature of volatile compounds drive to the need of a reliable analytical method that allows their proper quantification to explain the standard method of panel test. Although there are some analytical solutions available, they have not been validated and the regulatory bodies are reluctant to adopt them since they can be subjected to unknown errors. In this regards, the European Union has encouraged the validation of these analytical tools through the research program Horizon2020, which involves gaining knowledge from the analytical properties of the chemical methods for sensory assessment. This work is focused on the analytical validation of the methodology used to determine the actual concentration of volatiles in virgin olive oils when applying SPME-GCMS. The validation process includes the calibration curves for 29 volatile compounds responsible for the most common sensory perceptions in virgin olive oils, the determination of their working ranges with linear response, the detection and quantification limits, the sensitivity, the accuracy estimated as trueness and precision and the selectivity. Sixty-seven percent of the compounds presented a relative standard deviation in repeatability lower than 10%, and this percentage rises to 95% in lampante virgin olive oils. The accuracy was established in 97% of the studied volatile compounds. Finally, an empirical example of the ability of the method to discriminate virgin olive oils of different categories (extra virgin, virgin, ordinary and lampante) by the quantification of their volatiles is provided. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. HS-SPME-GC×GC-qMS volatile metabolite profiling of Chrysolina herbacea frass and Mentha spp. leaves.

    Science.gov (United States)

    Cordero, Chiara; Zebelo, Simon Atsbaha; Gnavi, Giorgio; Griglione, Alessandra; Bicchi, Carlo; Maffei, Massimo E; Rubiolo, Patrizia

    2012-02-01

    Headspace solid-phase microextraction (HS-SPME) comprehensive two-dimensional (2D) gas chromatography combined with quadrupole-mass spectrometry (GC×GC-qMS) with dedicated comparative data elaboration was applied to separate chemical patterns arising from the interaction between some Mentha species and the herbivore Chrysolina herbacea, also known as the mint bug. Upon feeding on different Mentha species (Mentha spicata L., Mentha × piperita L. and Mentha longifolia L.), C. herbacea produced frass (faeces) which were characterized by a typical volatile fraction. HS-SPME GC×GC-qMS analysis of the complex volatile fraction of both mint leaf and C. herbacea frass was submitted to advanced fingerprinting analysis of 2D chromatographic data. 1,8-Cineole, found in the leaves of all the Mentha species examined, was oxidized, and C. herbacea frass yielded high rates of several hydroxy-1,8-cineoles, including 2α-hydroxy-, 3α-hydroxy-, 3β-hydroxy- and 9-hydroxy-1,8-cineole. Upon insect feeding, several unknown oxidized monoterpenes, a p-menthane diol and three unknown phenylpropanoids were also detected in the frass volatiles. In M. longifolia, the occurrence of the monoterpene piperitenone oxide was found to be toxic and associated with insect death. The results of this work show that high throughput techniques such as HS-SPME and GC×GC-qMS fingerprint analysis are ideal tools to analyze complex volatile matrices, and provide a sensitive method for the direct comparison and chemical visualization of plant and insect emitted volatile components.

  14. Optimization of biological and instrumental detection of explosives and ignitable liquid residues including canines, SPME/ITMS and GC/MSn

    Science.gov (United States)

    Furton, Kenneth G.; Harper, Ross J.; Perr, Jeannette M.; Almirall, Jose R.

    2003-09-01

    A comprehensive study and comparison is underway using biological detectors and instrumental methods for the rapid detection of ignitable liquid residues (ILR) and high explosives. Headspace solid phase microextraction (SPME) has been demonstrated to be an effective sampling method helping to identify active odor signature chemicals used by detector dogs to locate forensic specimens as well as a rapid pre-concentration technique prior to instrumental detection. Common ignitable liquids and common military and industrial explosives have been studied including trinitrotoluene, tetryl, RDX, HMX, EGDN, PETN and nitroglycerine. This study focuses on identifying volatile odor signature chemicals present, which can be used to enhance the level and reliability of detection of ILR and explosives by canines and instrumental methods. While most instrumental methods currently in use focus on particles and on parent organic compounds, which are often involatile, characteristic volatile organics are generally also present and can be exploited to enhance detection particularly for well-concealed devices. Specific examples include the volatile odor chemicals 2-ethyl-1-hexanol and cyclohexanone, which are readily available in the headspace of the high explosive composition C-4; whereas, the active chemical cyclo-1,3,5-trimethylene-2,4,6-trinitramine (RDX) is not. The analysis and identification of these headspace 'fingerprint' organics is followed by double-blind dog trials of the individual components using certified teams in an attempt to isolate and understand the target compounds to which dogs are sensitive. Studies to compare commonly used training aids with the actual target explosive have also been undertaken to determine their suitability and effectiveness. The optimization of solid phase microextraction (SPME) combined with ion trap mobility spectrometry (ITMS) and gas chromatography/mass spectrometry/mass spectrometry (GC/MSn) is detailed including interface development

  15. Analysis of low-molar-mass materials in commercial rubber samples by Soxhlet and headspace extractions followed by GC-MS analysis.

    Science.gov (United States)

    Delaunay-Bertoncini, N; van der Wielen, F W M; de Voogt, P; Erlandsson, B; Schoenmakers, P J

    2004-09-03

    Very tight regulations apply to materials used for pharmaceutical packaging and for administering drugs. In this paper, we describe a simple and reliable procedure involving both gas- and liquid-phase extraction steps followed by an analysis step to identify the low-molar-mass materials in commercial-rubber samples. Representative commercial rubbers, that could be used for pharmaceutical packaging, have been selected and cryogenically powdered. Headspace and Soxhlet extractions have been carried out and the key parameters are discussed. The obtained extracts have been analyzed by gas chromatography (GC)-mass spectrometry (MS). More than 100 compounds have been detected and identified. Headspace allowed to extract the more-volatile compounds, whereas Soxhlet extraction recovered less-volatile compounds, but induced a loss of the volatile ones. Thus, both extraction techniques are required to fully characterize the low-molar-mass compounds present in rubber.

  16. [Determination of five synthetic musks in perfume by headspace solid-phase microextraction and gas chromatography-mass spectrometry].

    Science.gov (United States)

    Wang, Guannan; Tang, Hua; Chen, Dazhou; Feng, Jie; Li, Lei

    2012-02-01

    A method for headspace solid-phase microextraction (HS-SPME), followed by gas chromatography-mass spectrometry (GC-MS) analysis was established for the determination of five commonly used synthetic musks in perfume. Two polycyclic musks (celestolide and tonalide) and three nitro musks (musk ambrette, musk xylene and musk ketone) were used as analytes in the optimization of the analytical method. Six parameters, such as the extraction temperature, equilibrium time, extraction time, desorption time, injector temperature and solution of salting out, were optimized by exposing the 65 microm polydimethylsiloxane-divinyl-benzene (PDMS-DVB) fiber to the headspace of magnetically stirred (600 r/min) sample. According to the results of the optimization experiments, the following conclusion can be drawn: The water-diluted sample in a 10 mL headspace-vial was efficiently extracted for 20 min after the system was equilibrated for 3 min at 60 degrees C. After extraction, the fiber was immediately inserted into the GC injector and desorbed at 250 degrees C for 3 min. The spiked recoveries were in the range of 82.0% - 103.3% and the relative standard deviations (RSDs) were between 1.8% and 9.4%. Meanwhile, the limits of detection (LODs) ranged from 0.6 ng/g to 2.1 ng/g. This method is characterized by rapidity, high sensitivity, good linearity and repeatability for all the target compounds. It is applicable to the analysis of synthetic musks in perfumes.

  17. Multiple headspace-solid-phase microextraction: an application to quantification of mushroom volatiles.

    Science.gov (United States)

    Costa, Rosaria; Tedone, Laura; De Grazia, Selenia; Dugo, Paola; Mondello, Luigi

    2013-04-03

    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. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation

    Directory of Open Access Journals (Sweden)

    Lauren E. Musumeci

    2015-07-01

    Full Text Available Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH, 3-mercaptohexylacetate (3-MHA, and 4-mercapto-4-methyl-2-pentanone (4-MMP are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography electron impact mass spectrometry (GC-EI-MS. We describe a method in which thiols are converted to pentafluorobenzyl (PFB derivatives by extractive alkylation and the organic layer is evaporated prior to headspace solid phase microextraction (HS-SPME and GC-EI-MS analysis. Optimal parameters were determined by response surface area modeling. The addition of NaCl solution to the dried SPME vials prior to extraction resulted in up to less than fivefold improvement in detection limits. Using 40 mL wine samples, limits of detection for 4-MMP, 3-MH, and 3-MHA were 0.9 ng/L, 1 ng/L, and 17 ng/L, respectively. Good recovery (90%–109% and precision (5%–11% RSD were achieved in wine matrices. The new method was used to survey polyfunctional thiol concentrations in 61 commercial California and New York State wines produced from V. vinifera (Riesling, Gewürztraminer, Cabernet Sauvignon, Sauvignon blanc and non-varietal rosé wines, V. labruscana (Niagara, and Vitis spp. (Cayuga White. Mean 4-MMP concentrations in New York Niagara (17 ng/L were not significantly different from concentrations in Sauvignon blanc, but were significantly higher than 4-MMP in other varietal wines.

  19. Optimization of headspace solid-phase microextraction for analysis of {beta}-caryophyllene in a nanoemulsion dosage form prepared with copaiba (Copaifera multijuga Hayne) oil

    Energy Technology Data Exchange (ETDEWEB)

    Dias, Daiane de O; Colombo, Mariana; Kelmann, Regina G. [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS, Av. Ipiranga, 2752, CEP 90610-000 (Brazil); De Souza, Tatiane P. [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Universidade Federal do Amazonas, Manaus, Amazonas (Brazil); Bassani, Valquiria L.; Teixeira, Helder F. [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS, Av. Ipiranga, 2752, CEP 90610-000 (Brazil); Veiga, Valdir F. [Departamento de Quimica, Instituto de Ciencias Exatas, UFAM, Av. Gal. Rodrigo Octavio, 6.200 - Japiim, 69.079-000, Manaus - AM (Brazil); Limberger, Renata P. [Programa de Pos-Graduacao em Ciencias Farmaceuticas, Faculdade de Farmacia, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS, Av. Ipiranga, 2752, CEP 90610-000 (Brazil); and others

    2012-04-06

    Highlights: Black-Right-Pointing-Pointer A SPME-CG method is proposed for {beta}-caryophyllene assay in nanoemulsions containing copaiba oil. Black-Right-Pointing-Pointer SPME parameters were optimized for efficient {beta}-caryophyllene extraction. Black-Right-Pointing-Pointer The stability-indicating capability and specificity of the method were satisfied. Black-Right-Pointing-Pointer Nanoemulsions partially protected {beta}-caryophyllene under stressing conditions. Black-Right-Pointing-Pointer The proposed method presents linearity, lows LOD and LOQ, good precision, accuracy and robustness. - Abstract: Recent studies have shown the anti-inflammatory activity of Copaiba oils may be addressed to the high content of {beta}-caryophyllene, the most common sesquiterpene detected, especially in the Copaifera multijuga Hayne species. In the present study, nanoemulsions were proposed as a delivery system for copaiba oil in view to treat locally inflamed skin. This article describes the optimization and validation of a stability-indicating SPME-GC method, for {beta}-caryophyllene analysis in the nanoemulsions produced by high pressure homogenization. SPME methods are performed with PDMS (polydimethylsiloxane) fiber (100 {mu}m). Three SPME parameters were evaluated by a three-level-three-factor Box-Behnken factorial design as potentially affecting the technique efficiency. According to the results obtained, the best conditions to extract {beta}-caryophyllene were: (i) sampling temperature of 45 Degree-Sign C, (ii) sampling time of 20 min and (iii) no NaCl addition. Results coming from the forced degradation tests showed a reduction of {beta}-caryophyllene peak area when both caryophyllene methanolic solution and nanoemulsions were exposed to acid hydrolysis, UV-A irradiation, oxidative (H{sub 2}O{sub 2}) and thermolitic (60 Degree-Sign C) conditions. Such reduction occurred in lower extent in the nanoemulsions, suggesting a protective effect of the formulation to {beta

  20. Quantitative Analysis of Bisphenol A Leached from Household Plastics by Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry (SPME-GC-MS)

    Science.gov (United States)

    Johnson, Bettie Obi; Burke, Fernanda M.; Harrison, Rebecca; Burdette, Samantha

    2012-01-01

    The measurement of trace levels of bisphenol A (BPA) leached out of household plastics using solid-phase microextraction (SPME) with gas chromatography-mass spectrometry (GC-MS) is reported here. BPA is an endocrine-disrupting compound used in the industrial manufacture of polycarbonate plastic bottles and epoxy resin can liners. This experiment…

  1. Multivariate statistical analysis of hemlock (Tsuga) volatiles by SPME/GC/MS: insights into the phytochemistry of the hemlock woolly adelgid (Adelges tsugae Annand)

    Science.gov (United States)

    Anthony Lagalante; Frank Calvosa; Michael Mirzabeigi; Vikram Iyengar; Michael Montgomery; Kathleen Shields

    2007-01-01

    A previously developed single-needle, SPME/GC/MS technique was used to measure the terpenoid content of T. canadensis growing in a hemlock forest at Lake Scranton, PA (Lagalante and Montgomery 2003). The volatile terpenoid composition was measured over a 1-year period from June 2003 to May 2004 to follow the annual cycle of foliage development from...

  2. Multi-volatile method for aroma analysis using sequential dynamic headspace sampling with an application to brewed coffee.

    Science.gov (United States)

    Ochiai, Nobuo; Tsunokawa, Jun; Sasamoto, Kikuo; Hoffmann, Andreas

    2014-12-05

    A novel multi-volatile method (MVM) using sequential dynamic headspace (DHS) sampling for analysis of aroma compounds in aqueous sample was developed. The MVM consists of three different DHS method parameters sets including choice of the replaceable adsorbent trap. The first DHS sampling at 25 °C using a carbon-based adsorbent trap targets very volatile solutes with high vapor pressure (>20 kPa). The second DHS sampling at 25 °C using the same type of carbon-based adsorbent trap targets volatile solutes with moderate vapor pressure (1-20 kPa). The third DHS sampling using a Tenax TA trap at 80 °C targets solutes with low vapor pressure (0.9910) and high sensitivity (limit of detection: 1.0-7.5 ng mL(-1)) even with MS scan mode. The feasibility and benefit of the method was demonstrated with analysis of a wide variety of aroma compounds in brewed coffee. Ten potent aroma compounds from top-note to base-note (acetaldehyde, 2,3-butanedione, 4-ethyl guaiacol, furaneol, guaiacol, 3-methyl butanal, 2,3-pentanedione, 2,3,5-trimethyl pyrazine, vanillin, and 4-vinyl guaiacol) could be identified together with an additional 72 aroma compounds. Thirty compounds including 9 potent aroma compounds were quantified in the range of 74-4300 ng mL(-1) (RSD<10%, n=5). Copyright © 2014 The Authors. Published by Elsevier B.V. All rights reserved.

  3. Direct quantitation of volatile organic compounds in packaging materials by headspace solid-phase microextraction-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Ezquerro, Scar; Pons, Begoña; Tena, María Teresa

    2003-01-24

    The quantification of volatile organic compounds (VOCs) in flexible multilayer packaging materials using headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) was studied. The analytes imclude 22 compounds such as aldehydes. ketones, carboxylic acids and hydrocarbons formed by thermooxidative degradation of polyethylene during the extrusion coating process in the manufacture of the packaging, and many of them are involved in the unpleasant and undesirable odour of these materials. External standard calibration using a solution of the analytes in an appropriate solvent was the first approach studied. Aqueous solutions of the analytes provided low reproducibility and the reduction of aldehydes to alcohols under the HS-SPME conditions. Hexadecane was chosen as the solvent since its polarity is similar to that of polyethylene and its volatility is lower than that of the analytes. However, hexadecane should be added to the sample before the analysis as it modifies the absorption capacity of the fibre. A 75-microm Carboxen-poly(dimethylsiloxane) fibre was used to extract the VOCs from the headspace above the packaging in a 15-ml sealed vial at 100 degrees C after 5 min of preincubation. The influence of the extraction time on the amount extracted was studied for a standard solution of the analytes in hexadecane, together with the influence of the volume of the standard solution and the amount of the sample placed in the vial. Standard addition and multiple HS-SPME were also studied as calibration methods and the results obtained in the quantitative analysis of a packaging material were compared.

  4. 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.

  5. Rapid analysis of dissolved methane, ethylene, acetylene and ethane using partition coefficients and headspace-gas chromatography.

    Science.gov (United States)

    Lomond, Jasmine S; Tong, Anthony Z

    2011-01-01

    Analysis of dissolved methane, ethylene, acetylene, and ethane in water is crucial in evaluating anaerobic activity and investigating the sources of hydrocarbon contamination in aquatic environments. A rapid chromatographic method based on phase equilibrium between water and its headspace is developed for these analytes. The new method requires minimal sample preparation and no special apparatus except those associated with gas chromatography. Instead of Henry's Law used in similar previous studies, partition coefficients are used for the first time to calculate concentrations of dissolved hydrocarbon gases, which considerably simplifies the calculation involved. Partition coefficients are determined to be 128, 27.9, 1.28, and 96.3 at 30°C for methane, ethylene, acetylene, and ethane, respectively. It was discovered that the volume ratio of gas-to-liquid phase is critical to the accuracy of the measurements. The method performance can be readily improved by reducing the volume ratio of the two phases. Method validation shows less than 6% variation in accuracy and precision except at low levels of methane where interferences occur in ambient air. Method detection limits are determined to be in the low ng/L range for all analytes. The performance of the method is further tested using environmental samples collected from various sites in Nova Scotia.

  6. Graphene deposited onto aligned zinc oxide nanorods as an efficient coating for headspace solid-phase microextraction of gasoline fractions from oil samples.

    Science.gov (United States)

    Wen, Congying; Li, Mengmeng; Li, Wangbo; Li, Zizhou; Duan, Wei; Li, Yulong; Zhou, Jie; Li, Xiyou; Zeng, Jingbin

    2017-12-29

    The content of gasoline fraction in oil samples is not only an important indicator of oil quality, but also an indispensable fundamental data for oil refining and processing. Before its determination, efficient preconcentration and separation of gasoline fractions from complicated matrices is essential. In this work, a thin layer of graphene (G) was deposited onto oriented ZnO nanorods (ZNRs) as a SPME coating. By this approach, the surface area of G was greatly enhanced by the aligned ZNRs, and the surface polarity of ZNRs was changed from polar to less polar, which were both beneficial for the extraction of gasoline fractions. In addition, the ZNRs were well protected by the mechanically and chemically stable G, making the coating highly durable for use. With headspace SPME (HS-SPME) mode, the G/ZNRs coating can effectively extract gasoline fractions from various oil samples, whose extraction efficiency achieved 1.5-5.4 and 2.1-8.2 times higher than those of a G and commercial 7-μm PDMS coating respectively. Coupled with GC-FID, the developed method is sensitive, simple, cost effective and easily accessible for the analysis of gasoline fractions. Moreover, the method is also feasible for the detection of gasoline markers in simulated oil-polluted water, which provides an option for the monitoring of oil spill accident. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. ANALYTICAL APPROACH OF THE VOLATILE FRACTION OF Solanum quitoense BY HS-SPME/GC-MS

    Directory of Open Access Journals (Sweden)

    EDUARDO CORPAS IGUARÁN

    2017-07-01

    Full Text Available The species of lulo fruit (Solanum quitoense, predominant in Colombia, is a promising fruit for both national and international market due to its flavor and nutritional characteristics, which generated the interest to know the volatile composition of its pulp. After adjusting, the chromatographic conditions necessary to analyze volatile fraction of this fruit, the effect of the temperature and time of adsorption was measured through the headspace - solid phase microextraction (HS-SPME and gas chromatography - mass spectrometry (GC-MS, on the area of volatile compounds of S. quitoense, by applying the experimental design of a factor. The descriptive analysis suggested that the adsorption at 60°C and 30 minutes promoted optimal recovery of volatiles as well as internal standard (1-Octanol, with recovery of 99,66% at 60ºC, while the non-parametric test Kruskal-Wallis showed statistical differences in the effect of time (P= 0,018, but not of the temperature adsorption (P= 0,058 upon the volatiles compounds area. A predominance of esters (48,98%, aldehydes (18,37%, and alcohols (14,29% was observed and also were found compounds of greatest area such as 3-hexen-1-ol acetate, acetic acid methyl ester, and acetic acid hexyl ester. These metabolites determine the characteristic aroma from lulo pulp and influence the consumer preference.

  8. 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.

  9. Automated determination of aliphatic primary amines in wastewater by simultaneous derivatization and headspace solid-phase microextraction followed by gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Llop, Anna; Pocurull, Eva; Borrull, Francesc

    2010-01-22

    This paper presents a fully automated method for determining ten primary amines in wastewater at ng/L levels. The method is based on simultaneous derivatization with pentafluorobenzaldehyde (PFBAY) and headspace solid-phase microextraction (HS-SPME) followed by gas chromatography coupled to ion trap tandem mass spectrometry (GC-IT-MS-MS). The influence of main factors on the efficiency of derivatization and of HS-SPME is described in detail and optimized by a central composite design. For all species, the highest enrichment factors were achieved using a 85 microm polyacrylate (PA) fiber exposed in the headspace of stirred water samples (750 rpm) at pH 12, containing 360 g/L of NaCl, at 40 degrees C for 15 min. Under optimized conditions, the proposed method achieved detection limits ranging from 10 to 100 ng/L (except for cyclohexylamine). The optimized method was then used to determine the presence of primary amines in various types of wastewater samples, such as influent and effluent wastewater from municipal and industrial wastewater treatment plants (WWTPs) and a potable water treatment plant. Although the analysis of these samples revealed the presence of up to 1500 microg/L of certain primary amines in influent industrial wastewater, the concentration of these compounds in the effluent and in municipal and potable water was substantially lower, at low microg/L levels. The new derivatization-HS-SPME-GC-IT-MS-MS method is suitable for the fast, reliable and inexpensive determination of primary amines in wastewater in an automated procedure. Copyright 2009 Elsevier B.V. All rights reserved.

  10. A simple and automated method to determine macrocyclic musk fragrances in sewage sludge samples by headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Vallecillos, Laura; Pocurull, Eva; Borrull, Francesc

    2013-11-01

    For the first time, headspace solid-phase microextraction (HS-SPME) has shown to be a powerful technique to extract macrocyclic musk fragrances directly from sewage sludge. It avoids the need to use additional extraction/preconcentration techniques or clean-up procedure and facilitates the automation of the method. Thus, a simple and fully automated method based on HS-SPME and GC-MS has been developed which allows the determination of eight macrocyclic musk fragrances at ngg(-1) (d.w.) levels. The optimal HS-SPME conditions were achieved when a PDMS/DVB 65μm fibre was exposed for 45min in the headspace of 0.25g sewage sludge samples mixed with 0.5mL of water stirred at 750rpm at 80°C. Optimal desorption conditions were found to be 250°C for 3min. Method detection limits were found in the low pgg(-1) range between 10pgg(-1) (d.w.) and 25pgg(-1) (d.w.) depending on the target analytes. In addition, under optimized conditions, the method gave good levels of intra-day and inter-day repeatabilities in sewage sludge with relative standard deviations varying between 1% to 9% and 6% to 15% respectively (n=5, 1000pgg(-1) d.w.). The applicability of the method was tested with sewage sludge from three urban sewage treatment plants (STPs). The analysis revealed the presence of the macrocyclic musks studied in several samples, with concentrations ranging between below MQL (method quantification limit) and 0.89ngg(-1) (d.w.). Copyright © 2013 Elsevier B.V. All rights reserved.

  11. Method for sampling and analysis of volatile biomarkers in process gas from aerobic digestion of poultry carcasses using time-weighted average SPME and GC-MS.

    Science.gov (United States)

    Koziel, Jacek A; Nguyen, Lam T; Glanville, Thomas D; Ahn, Heekwon; Frana, Timothy S; Hans van Leeuwen, J

    2017-10-01

    A passive sampling method, using retracted solid-phase microextraction (SPME) - gas chromatography-mass spectrometry and time-weighted averaging, was developed and validated for tracking marker volatile organic compounds (VOCs) emitted during aerobic digestion of biohazardous animal tissue. The retracted SPME configuration protects the fragile fiber from buffeting by the process gas stream, and it requires less equipment and is potentially more biosecure than conventional active sampling methods. VOC concentrations predicted via a model based on Fick's first law of diffusion were within 6.6-12.3% of experimentally controlled values after accounting for VOC adsorption to the SPME fiber housing. Method detection limits for five marker VOCs ranged from 0.70 to 8.44ppbv and were statistically equivalent (p>0.05) to those for active sorbent-tube-based sampling. The sampling time of 30min and fiber retraction of 5mm were found to be optimal for the tissue digestion process. Copyright © 2017 Elsevier Ltd. All rights reserved.

  12. Rapid Separation of Elemental Species by Fast Multicapillary Gas Chromatography with Multichannel Optical Spectrometry Detection following Headspace Solid Phase Microextraction

    Directory of Open Access Journals (Sweden)

    Jacek Giersz

    2015-05-01

    Full Text Available 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 quantified within 25 s under isothermal conditions. A new miniaturized speciation analyzer has been constructed and evaluated. The system consists of a GC injection port and a lab-made miniaturized GC unit directly coupled with miniaturized plasma excitation source. The emitted light is transferred via optical fiber and registered with a miniaturized charged coupled device (CCD based spectrometer. Working parameters for multicapillary column gas chromatography with atomic emission detector, including carrier gas flow rate, desorption temperature, and GC column temperature, were optimized to achieve good separation of analytes. Basic investigations of the fundamental properties of 5 cm-long multicapillary column, to evaluate its potential and limitations as a rapid separation unit, are presented. The adaptation of the technique for use with a SPME system and with a multichannel element-selective plasma-emission detector is highlighted.

  13. Analysis of polysulfides in drinking water distribution systems using headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Kristiana, Ina; Heitz, Anna; Joll, Cynthia; Sathasivan, Arumugam

    2010-09-17

    Sulfide and polysulfides are strong nucleophiles and reducing agents that participate in many environmentally significant processes such as the formation of sulfide minerals and volatile organic sulfur compounds. Their presence in drinking water distribution systems are of particular concern and need to be assessed, since these species consume disinfectants and dissolved oxygen, react with metal ions to produce insoluble metal sulfides, and cause taste and odour problems. The analysis of sulfide and polysulfides in drinking water distribution systems is challenging due to their low concentrations, thermal instability and their susceptibility to undergo oxidation and disproportionation reactions. This paper reports on the development and optimisation of a rapid, simple, and sensitive method for the determination of sulfide and polysulfides in drinking water distribution systems. The method uses methyl iodide to derivatize sulfide and polysulfides into their corresponding dimethyl(poly)sulfides, which are then extracted using solid-phase microextraction in the headspace mode and analysed by gas chromatography-mass spectrometry. Good sensitivity was achieved for the analysis of dimethyl(poly)sulfides, with detection limits ranging from 50 to 240 ng L(-1). The method also demonstrated good precision (repeatability: 3-7%) and good linearity over two orders of magnitude. Matrix effects from raw drinking water containing organic carbon (3.8 mg L(-1)) and from sediment material from a drinking water distribution system were shown to have no interferences in the analysis of dimethyl(poly)sulfides. The method provides a rapid, robust, and reliable mean to analyse trace levels of sulfides and polysulfides in aqueous systems. The new method described here is more accessible and user-friendly than methods based on closed-loop stripping analysis, which have been traditionally used for the analysis of these compounds. The optimised method was used to analyse samples collected

  14. Analysis of Volatile Components of Cape Gooseberry (Physalis peruviana L.) Grown in Turkey by HS-SPME and GC-MS

    OpenAIRE

    Murat Yilmaztekin

    2014-01-01

    Volatile components in cape gooseberry fruit at ripe stage were collected using headspace-solid phase microextraction, and analyzed by gas chromatography-mass spectrometry. Three solid phase microextraction fiber coatings (DVB/CAR/PDMS, CAR/PDMS, and PDMS/DVB) were tested for evaluation of volatile compounds. DVB/CAR/PDMS fiber showed a strong extraction capacity for volatile compounds and produced the best result in case of total peak areas. A total of 133 volatile compounds were identified ...

  15. Further research on the photo-SPME of triclosan

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez-Prado, Lucia; Llompart, Maria; Lores, Marta; Fernandez-Alvarez, Maria; Garcia-Jares, Carmen; Cela, Rafael [Universidad de Santiago de Compostela, Departamento de Quimica Analitica, Nutricion y Bromatologia. Facultad de Quimica, Instituto de Investigacion y Analisis Alimentario, Santiago de Compostela (Spain)

    2006-04-15

    In this study the photoinduced degradation of triclosan has been investigated by photo-solid-phase microextraction (photo-SPME). In photo-SPME, photodegradation is carried out on the SPME fibre containing the target compound. Triclosan was extracted from aqueous solutions by use of polydimethylsiloxane SPME fibres and these were subsequently exposed to UV irradiation (power 8 W, wavelength 254 nm) for different times (from 2 to 60 min). The photodegradation kinetics of triclosan were investigated, the photoproducts generated were tentatively identified, and the photochemical behaviour of these products was studied by use of this on-fibre approach followed by gas chromatographic-mass spectrometric analysis. Eight photoproducts were tentatively identified, including chlorinated phenols, chlorohydroxydiphenyl ethers, 2,8-dichlorodibenzo-p-dioxin, and a possible dichlorodibenzodioxin isomer or dichlorohydroxydibenzofuran. The main photodegradation mechanisms were postulated and photodegradation pathways proposed. The effect of pH on triclosan degradation and on triclosan-to-dioxin conversion was also investigated. Triclosan degradation occurred, and generation of 2,8-dichlorodibenzo-p-dioxin was confirmed, throughout the pH range studied (from 3 to 9). (orig.)

  16. 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.

  17. Detection of Pseudomonas aeruginosa in sputum headspace through volatile organic compound analysis

    Directory of Open Access Journals (Sweden)

    Goeminne Pieter C

    2012-10-01

    Full Text Available Abstract Introduction Chronic pulmonary infection is the hallmark of Cystic Fibrosis lung disease. Searching for faster and easier screening may lead to faster diagnosis and treatment of Pseudomonas aeruginosa (P. aeruginosa. Our aim was to analyze and build a model to predict the presence of P. aeruginosa in sputa. Methods Sputa from 28 bronchiectatic patients were used for bacterial culturing and analysis of volatile compounds by gas chromatography–mass spectrometry. Data analysis and model building were done by Partial Least Squares Regression Discriminant analysis (PLS-DA. Two analysis were performed: one comparing P. aeruginosa positive with negative cultures at study visit (PA model and one comparing chronic colonization according to the Leeds criteria with P. aeruginosa negative patients (PACC model. Results The PA model prediction of P. aeruginosa presence was rather poor, with a high number of false positives and false negatives. On the other hand, the PACC model was stable and explained chronic P. aeruginosa presence for 95% with 4 PLS-DA factors, with a sensitivity of 100%, a positive predictive value of 86% and a negative predictive value of 100%. Conclusion Our study shows the potential for building a prediction model for the presence of chronic P. aeruginosa based on volatiles from sputum.

  18. Analysis of aroma compounds of Roselle by Dynamic Headspace Sampling using different preparation methods

    DEFF Research Database (Denmark)

    Juhari, Nurul Hanisah Binti; Varming, Camilla; Petersen, Mikael Agerlin

    2015-01-01

    The influence of different methods of sample preparation on the aroma profiles of dried Roselle (Hibiscus sabdariffa) was studied. Least amounts of aroma compounds were recovered by analysis of whole dry calyxes (WD) followed by ground dry (GD), blended together with water (BTW), and ground...... and then mixed with water (GMW). The highest number of aroma compounds was found in Roselle treated in water bath (2hr/40°C) (GMWKB). GMW was chosen as the preparation method because it was shown to be an efficient extraction method without the possibility of excessive chemical changes of the sample....

  19. Evaluation and application of static headspace-multicapillary column-gas chromatography-ion mobility spectrometry for complex sample analysis.

    Science.gov (United States)

    Denawaka, Chamila J; Fowlis, Ian A; Dean, John R

    2014-04-18

    An evaluation of static headspace-multicapillary column-gas chromatography-ion mobility spectrometry (SHS-MCC-GC-IMS) has been undertaken to assess its applicability for the determination of 32 volatile compounds (VCs). The key experimental variables of sample incubation time and temperature have been evaluated alongside the MCC-GC variables of column polarity, syringe temperature, injection temperature, injection volume, column temperature and carrier gas flow rate coupled with the IMS variables of temperature and drift gas flow rate. This evaluation resulted in six sets of experimental variables being required to separate the 32 VCs. The optimum experimental variables for SHS-MCC-GC-IMS, the retention time and drift time operating parameters were determined; to normalise the operating parameters, the relative drift time and normalised reduced ion mobility for each VC were determined. In addition, a full theoretical explanation is provided on the formation of the monomer, dimer and trimer of a VC. The optimum operating condition for each VC calibration data was obtained alongside limit of detection (LOD) and limit of quantitation (LOQ) values. Typical detection limits ranged from 0.1ng bis(methylthio)methane, ethylbutanoate and (E)-2-nonenal to 472ng isovaleric acid with correlation coefficient (R(2)) data ranging from 0.9793 (for the dimer of octanal) through to 0.9990 (for isobutyric acid). Finally, the developed protocols were applied to the analysis of malodour in sock samples. Initial work involved spiking an inert matrix and sock samples with appropriate concentrations of eight VCs. The average recovery from the inert matrix was 101±18% (n=8), while recoveries from the sock samples were lower, that is, 54±30% (n=8) for sock type 1 and 78±24% (n=6) for sock type 2. Finally, SHS-MCC-GC-IMS was applied to sock malodour in a field trial based on 11 volunteers (mixed gender) over a 3-week period. By applying the SHS-MCC-GC-IMS database, four VCs were

  20. 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. Copyright © 2012 Elsevier Ltd. All rights reserved.

  1. Rapid method for quantitative analysis of the aroma impact compound, 2-acetyl-1-pyrroline, in fragrant rice using automated headspace gas chromatography.

    Science.gov (United States)

    Sriseadka, Tinakorn; Wongpornchai, Sugunya; Kitsawatpaiboon, Pisan

    2006-10-18

    A rapid method employing static headspace gas chromatography (HS-GC) has been developed and validated for quantitative analysis of the impact aroma compound, 2-acetyl-1-pyrroline (2AP), in grains of fragrant rice. This developed method excludes wet extraction, and the rice headspace volatiles are brought directly and automatically to GC analysis. The conditions of the static HS autosampler were optimized to achieve high recovery and sensitivity. The most effective amount of rice sample used was 1 g, which provided 51% recovery and a linear multiple headspace extraction (MHE) plot of the peak area of 2AP. The sensitivity of the method was enhanced by utilizing a megabore fused silica capillary column in conjunction with a nitrogen-phosphorus detector (NPD). Method validations performed for both static HS-GC-FID and HS-GC-NPD demonstrated linear calibration ranges of 20-10 000 (r(2) = 0.9997) and 5-8000 (r(2) = 0.9998) ng of 2AP/g of rice sample, respectively. The limits of detection for both systems were 20 and 5 ng of 2AP, and the limits of quantitation were 0.30 and 0.01 g of brown rice sample, respectively. Reproducibility calculated as intraday and interday coefficients of variation were 3.25% RSD (n = 15) and 3.92% RSD (n = 35), respectively, for SHS-GC-FID and 1.87% RSD (n = 15) and 2.85% RSD (n = 35), respectively, for SHS-GC-NPD. The method was found to be effective when applied to the evaluation of aroma quality, based on 2AP concentrations, of some fragrant rice samples.

  2. Headspace in-tube extraction gas chromatography-mass spectrometry for the analysis of hydroxylic methyl-derivatized and volatile organic compounds in blood and urine.

    Science.gov (United States)

    Rasanen, Ilpo; Viinamäki, Jenni; Vuori, Erkki; Ojanperä, Ilkka

    2010-04-01

    A novel headspace in-tube extraction gas chromatography-mass spectrometry (ITEX-GC-MS) approach was developed for broad-scale analysis of low molecular weight organic compounds in blood and/or urine. One sample was analyzed following in-vial derivatization with dimethyl sulfate for ethylene glycol (EG), glycolic acid (GA), formic acid (FA), other hydroxylic compounds, and another sample for underivatized volatile organic compounds. Tenax adsorbent resin was used in the microtrap, and a porous layer, open tubular GC capillary column was used for separation. MS was operated in the full-scan mode, identification was based on the Automated Mass Spectral Deconvolution and Identification System, and quantification was based on extracted ions. The limits of quantification for EG, GA, and FA in blood were 10, 50, and 30 mg/L, respectively, and the expanded uncertainties of measurement were 20%, 16%, and 14%, respectively. The procedure allowed for the first time the inclusion of EG and GA as their methyl derivatives within a quantitative HS analysis. The ITEX method described here was more sensitive for analysis of volatile organic compounds than the corresponding static headspace analysis as demonstrated for 11 representative compounds.

  3. 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.

  4. Analysis of Odorants in Marking Fluid of Siberian Tiger (Panthera tigris altaica Using Simultaneous Sensory and Chemical Analysis with Headspace Solid-Phase Microextraction and Multidimensional Gas Chromatography-Mass Spectrometry-Olfactometry

    Directory of Open Access Journals (Sweden)

    Simone B. Soso

    2016-06-01

    Full Text Available Scent-marking is the most effective method of communication in the presence or absence of a signaler. These complex mixtures result in a multifaceted interaction triggered by the sense of smell. The objective was to identify volatile organic compound (VOC composition and odors emitted by total marking fluid (MF associated with Siberian tigers (Panthera tigris altaica. Siberian tiger, an endangered species, was chosen because its MF had never been analyzed. Solid phase microextraction (SPME for headspace volatile collection combined with multidimensional gas chromatography-mass spectrometry-olfactometry for simultaneous chemical and sensory analyses were used. Thirty-two VOCs emitted from MF were identified. 2-acetyl-1-pyrroline, the sole previously identified compound responsible for the “characteristic” odor of P. tigris MF, was identified along with two additional compounds confirmed with standards (urea, furfural and four tentatively identified compounds (3-methylbutanamine, (R-3-methylcyclopentanone, propanedioic acid, and 3-hydroxybutanal as being responsible for the characteristic aroma of Siberian tiger MF. Simultaneous chemical and sensory analyses improved characterization of scent-markings and identified compounds not previously reported in MF of other tiger species. This research will assist animal ecologists, behaviorists, and zookeepers in understanding how scents from specific MF compounds impact tiger and wildlife communication and improve management practices related to animal behavior. Simultaneous chemical and sensory analyses is applicable to unlocking scent-marking information for other species.

  5. Analysis of Odorants in Marking Fluid of Siberian Tiger (Panthera tigris altaica) Using Simultaneous Sensory and Chemical Analysis with Headspace Solid-Phase Microextraction and Multidimensional Gas Chromatography-Mass Spectrometry-Olfactometry.

    Science.gov (United States)

    Soso, Simone B; Koziel, Jacek A

    2016-06-25

    Scent-marking is the most effective method of communication in the presence or absence of a signaler. These complex mixtures result in a multifaceted interaction triggered by the sense of smell. The objective was to identify volatile organic compound (VOC) composition and odors emitted by total marking fluid (MF) associated with Siberian tigers (Panthera tigris altaica). Siberian tiger, an endangered species, was chosen because its MF had never been analyzed. Solid phase microextraction (SPME) for headspace volatile collection combined with multidimensional gas chromatography-mass spectrometry-olfactometry for simultaneous chemical and sensory analyses were used. Thirty-two VOCs emitted from MF were identified. 2-acetyl-1-pyrroline, the sole previously identified compound responsible for the "characteristic" odor of P. tigris MF, was identified along with two additional compounds confirmed with standards (urea, furfural) and four tentatively identified compounds (3-methylbutanamine, (R)-3-methylcyclopentanone, propanedioic acid, and 3-hydroxybutanal) as being responsible for the characteristic aroma of Siberian tiger MF. Simultaneous chemical and sensory analyses improved characterization of scent-markings and identified compounds not previously reported in MF of other tiger species. This research will assist animal ecologists, behaviorists, and zookeepers in understanding how scents from specific MF compounds impact tiger and wildlife communication and improve management practices related to animal behavior. Simultaneous chemical and sensory analyses is applicable to unlocking scent-marking information for other species.

  6. Comparison of extraction techniques and mass spectrometric ionization modes in the analysis of wine volatile carbonyls

    Energy Technology Data Exchange (ETDEWEB)

    Zapata, Julian; Mateo-Vivaracho, Laura; Cacho, Juan [Laboratory for Flavor Analysis and Enology, Institute of Engineering of Aragon, I3A, Department of Analytical Chemistry, Faculty of Sciences, University of Zaragoza, 50009 Zaragoza (Spain); Ferreira, Vicente, E-mail: vferre@unizar.es [Laboratory for Flavor Analysis and Enology, Institute of Engineering of Aragon, I3A, Department of Analytical Chemistry, Faculty of Sciences, University of Zaragoza, 50009 Zaragoza (Spain)

    2010-02-15

    This work presents a comparative study of the analytical characteristics of two methods for the analysis of carbonyl compounds in wine, both based on the derivatization with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA). In the first method derivatives are formed in the solid phase extraction (SPE) cartridge in which the analytes have been previously isolated, while in the second method derivatives are formed in a solid phase microextraction (SPME) fibre saturated with vapors of the reagent and exposed to the sample headspace. In both cases detection has been carried out by electron impact (EI) or negative chemical ionization (NCI) mass spectrometry. The possibility of determining haloanisols simultaneously has been also considered. The method based on SPE presents, in general, better analytical properties than the SPME one. Although linearity was satisfactory for both methods (R{sup 2} > 0.99), repeatability of the SPE method (RSD < 10%) was better than that obtained with SPME (9% < RSD < 20%). Detection limits obtained with EI are better for the SPE method except for trihaloanisols, while with NCI detection limits for both strategies are comparable, although the SPME strategy presents worse results for ketones and methional. Detection limits are always lower with NCI, being the improvement most notable for SPME. Recovery experiments show that in the case of SPE, uncertainties are lower than 12% in all cases, while with the SPME method the imprecision plus the existence of matrix effects make the global uncertainty to be higher than 15%.

  7. Comparison of extraction techniques and mass spectrometric ionization modes in the analysis of wine volatile carbonyls

    International Nuclear Information System (INIS)

    Zapata, Julian; Mateo-Vivaracho, Laura; Cacho, Juan; Ferreira, Vicente

    2010-01-01

    This work presents a comparative study of the analytical characteristics of two methods for the analysis of carbonyl compounds in wine, both based on the derivatization with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA). In the first method derivatives are formed in the solid phase extraction (SPE) cartridge in which the analytes have been previously isolated, while in the second method derivatives are formed in a solid phase microextraction (SPME) fibre saturated with vapors of the reagent and exposed to the sample headspace. In both cases detection has been carried out by electron impact (EI) or negative chemical ionization (NCI) mass spectrometry. The possibility of determining haloanisols simultaneously has been also considered. The method based on SPE presents, in general, better analytical properties than the SPME one. Although linearity was satisfactory for both methods (R 2 > 0.99), repeatability of the SPE method (RSD < 10%) was better than that obtained with SPME (9% < RSD < 20%). Detection limits obtained with EI are better for the SPE method except for trihaloanisols, while with NCI detection limits for both strategies are comparable, although the SPME strategy presents worse results for ketones and methional. Detection limits are always lower with NCI, being the improvement most notable for SPME. Recovery experiments show that in the case of SPE, uncertainties are lower than 12% in all cases, while with the SPME method the imprecision plus the existence of matrix effects make the global uncertainty to be higher than 15%.

  8. Analysis of the volatiles emitted by whole flowers and isolated flower organs of the carob tree using HS-SPME-GC/MS.

    Science.gov (United States)

    Custódio, Luísa; Serra, Hugo; Nogueira, José Manuel F; Gonçalves, Sandra; Romano, Anabela

    2006-05-01

    The volatiles emitted by fresh whole flowers and isolated flower organs of male, female, and hermaphrodite carob trees (Ceratonia siliqua L.; Leguminosae) were analyzed by headspace solid-phase microextraction followed by capillary gas chromatography and mass spectrometry. The headspace of carob flowers is mainly constituted of high amounts of monoterpenes and sesquiterpenes, and more than 25 compounds were identified. The gender and cultivar affected both the qualitative profile and the relative abundances of the volatiles of whole flowers and isolated floral organs. Linalool and its derivatives (cis-linalool furan oxide, 2,2,6-trimethyl-3-keto-6-vinyltetrahydropyran, cis-linalool pyran oxide, and trans-linalool furan oxide), alpha-pinene, and alpha-farnesene were the dominant volatiles. Female flowers had a higher diversity of volatile compounds than males and hermaphrodites, but a lower abundance of the major ones. Similarly, the floral scent of female flowers of cv. Mulata had a higher content of volatiles but a lower abundance of the major ones, when compared to cv. Galhosa. In each of the three gender types of flowers, the nectary disks seemed to be the major source of volatiles.

  9. Traceability of Satsuma Mandarin (Citrus unshiu Marc.) Honey through Nectar/Honey-Sac/Honey Pathways of the Headspace, Volatiles, and Semi-Volatiles: Chemical Markers

    OpenAIRE

    Igor Jerković; Saša Prđun; Zvonimir Marijanović; Marina Zekić; Dragan Bubalo; Lidija Svečnjak; Carlo I. G. Tuberoso

    2016-01-01

    Headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE), followed by GC-MS/FID, were applied for monitoring the nectar (NE)/honey-sac (HoS)/honey (HO) pathways of the headspace, volatiles, and semi-volatiles. The major NE (4 varieties of Citrus unshiu) headspace compounds were linalool, α-terpineol, 1H-indole, methyl anthranilate, and phenylacetonitrile. Corresponding extracts contained, among others, 1H-indole, methyl anthranilate, 1,3-dihydro-2H-indol-2-one a...

  10. Highly porous nanostructured copper foam fiber impregnated with an organic solvent for headspace liquid-phase microextraction.

    Science.gov (United States)

    Saraji, Mohammad; Ghani, Milad; Rezaei, Behzad; Mokhtarianpour, Maryam

    2016-10-21

    A new headspace liquid-phase microextraction technique based on using a copper foam nanostructure substrate followed by gas chromatography-flame ionization detection was developed for the determination of volatile organic compounds in water and wastewater samples. The copper foam with highly porous nanostructured walls was fabricated on the surface of a copper wire by a rapid and facile electrochemical process and used as the extractant solvent holder. Propyl benzoate was immobilized in the pores of the copper foam coating and used for the microextraction of benzene, toluene, ethylbenzene and xylenes. The experimental parameters such as the type of organic solvent, desorption temperature, desorption time, salt concentration, sample temperature, equilibrium time and extraction time, were investigated and optimized. Under the optimum conditions, the method detection limit was between 0.06 and 0.25μgL -1 . The relative standard deviation of the method for the analytes at 4-8μgL -1 concentration level ranged from 7.9 to 11%. The fiber-to-fiber reproducibility for three fibers prepared under the same condition was 9.3-12%. The enrichment factor was in the range of 615-744. Different water samples were analyzed for the evaluation of the method in real sample analysis. Relative recoveries for spiked tap, river and wastewater samples were in the range of 85-94%. Finally, the extraction efficiency of the method was compared with those of headspace single drop microextraction and headspace SPME with the commercial fibers. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. 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

    efficiency obtained with the SPME method can be affected by different factors such as fiber type, stirring of sample versus not stirring, extraction temperature and time. These factors can easily be controlled and optimized to obtain the highest possible extraction efficiency. However, extraction efficiency...... can also be affected by uncontrollable factors such as batch to batch variation between fibers of the same type and presence of compounds in the sample matrix, which competes with the compounds of interest for adsorption to the SPME fiber. The latter factor is particularly a problem when SPME is used...... for analysis of lipid oxidation during storage of complex food matrices. Examples on how uncontrollable factors have affected results obtained with the SPME method in the authors’ lab will be given and the appropriateness of the SPME method for the analysis of volatile oxidation products in selected food...

  12. 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

    efficiency obtained with the SPME method can be affected by different factors such as fiber type, stirring of sample versus not stirring, extraction temperature and time. These factors can easily be controlled and optimized to obtain the highest possible extraction efficiency. However, extraction efficiency...... can also be affected by uncontrollable factors such as batch to batch variation between fibers of the same type and presence of compounds in the sample matrix, which competes with the compounds of interest for adsorption to the SPME fiber. The latter factor is particularly a problem when SPME is used...... for analysis of lipid oxidation during storage of complex food matrices. Examples on how uncontrollable factors have affected results obtained with the SPME method in the authors’ lab will be given and the appropriateness of the SPME method for the analysis of volatile oxidation products in selected food...

  13. Analysis of volatile components of cape gooseberry (Physalis peruviana L.) grown in Turkey by HS-SPME and GC-MS.

    Science.gov (United States)

    Yilmaztekin, Murat

    2014-01-01

    Volatile components in cape gooseberry fruit at ripe stage were collected using headspace-solid phase microextraction, and analyzed by gas chromatography-mass spectrometry. Three solid phase microextraction fiber coatings (DVB/CAR/PDMS, CAR/PDMS, and PDMS/DVB) were tested for evaluation of volatile compounds. DVB/CAR/PDMS fiber showed a strong extraction capacity for volatile compounds and produced the best result in case of total peak areas. A total of 133 volatile compounds were identified in fruit pulp; among them 1-hexanol (6.86%), eucalyptol (6.66%), ethyl butanoate (6.47%), ethyl octanoate (4.01%), ethyl decanoate (3.39%), 4-terpineol (3.27%), and 2-methyl-1-butanol (3.10%) were the major components in the sample extracts.

  14. Analysis of Volatile Components of Cape Gooseberry (Physalis peruviana L. Grown in Turkey by HS-SPME and GC-MS

    Directory of Open Access Journals (Sweden)

    Murat Yilmaztekin

    2014-01-01

    Full Text Available Volatile components in cape gooseberry fruit at ripe stage were collected using headspace-solid phase microextraction, and analyzed by gas chromatography-mass spectrometry. Three solid phase microextraction fiber coatings (DVB/CAR/PDMS, CAR/PDMS, and PDMS/DVB were tested for evaluation of volatile compounds. DVB/CAR/PDMS fiber showed a strong extraction capacity for volatile compounds and produced the best result in case of total peak areas. A total of 133 volatile compounds were identified in fruit pulp; among them 1-hexanol (6.86%, eucalyptol (6.66%, ethyl butanoate (6.47%, ethyl octanoate (4.01%, ethyl decanoate (3.39%, 4-terpineol (3.27%, and 2-methyl-1-butanol (3.10% were the major components in the sample extracts.

  15. 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. Copyright © 2015 Elsevier B.V. All

  16. 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

  17. 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. Copyright © 2012 Elsevier Ltd. All rights reserved.

  18. Headspace solid-phase microextraction with 1-pyrenyldiazomethane on-fibre derivatisation for analysis of fluoroacetic acid in biological samples.

    Science.gov (United States)

    Sporkert, Frank; Pragst, Fritz; Hübner, Sandra; Mills, Graham

    2002-05-25

    A new and in part automated headspace solid-phase microextraction method for quantitative determination of the highly toxic rodenticide fluoroacetic acid (FAA) in serum and other biological samples has been developed. FAA and deuterated acetic acid (internal standard) were extracted from acidified samples by a StableFlex divinylbenzene-Carboxen on polydimethylsiloxane fibre. The acids were derivatised on the fibre in-situ with 1-pyrenyldiazomethane and detected using gas chromatography-mass spectrometry with electron impact ionisation and selected ion monitoring. The calibration curve for FAA in serum was linear over the range from 0.02 to 5 microg/ml, with limits of detection and quantification of 0.02 and 0.07 microg/ml, respectively. The method was also tested with spiked whole blood, urine, stomach contents and kidney samples. It was sufficiently reliable, reproducible and sensitive for use in routine forensic toxicology applications.

  19. Ultrasensitive Speciation Analysis of Mercury in Rice by Headspace Solid Phase Microextraction Using Porous Carbons and Gas Chromatography-Dielectric Barrier Discharge Optical Emission Spectrometry.

    Science.gov (United States)

    Lin, Yao; Yang, Yuan; Li, Yuxuan; Yang, Lu; Hou, Xiandeng; Feng, Xinbin; Zheng, Chengbin

    2016-03-01

    Rice consumption is a primary pathway for human methylmercury (MeHg) exposure in inland mercury mining areas of Asia. In addition, the use of iodomethane, a common fumigant that significantly accelerates the methylation of mercury in soil under sunlight, could increase the MeHg exposure from rice. Conventional hyphenated techniques used for mercury speciation analysis are usually too costly for most developing countries. Consequently, there is an increased interest in the development of sensitive and inexpensive methods for the speciation of mercury in rice. In this work, gas chromatography (GC) coupled to dielectric barrier discharge optical emission spectrometry (DBD-OES) was developed for the speciation analysis of mercury in rice. Prior to GC-DBD-OES analysis, mercury species were derivatized to their volatile species with NaBPh4 and preconcentrated by headspace solid phase microextraction using porous carbons. Limits of detection of 0.5 μg kg(-1) (0.16 ng), 0.75 μg kg(-1) (0.24 ng), and 1.0 μg kg(-1) (0.34 ng) were obtained for Hg(2+), CH3Hg(+), and CH3CH2Hg(+), respectively, with relative standard deviations (RSDs) better than 5.2% and 6.8% for one fiber or fiber-to-fiber mode, respectively. Recoveries of 90-105% were obtained for the rice samples, demonstrating the applicability of the proposed technique. Owing to the small size, low power, and low gas consumption of DBD-OES as well as efficient extraction of mercury species by porous carbons headspace solid phase micro-extraction, the proposed technique provides several advantages including compactness, cost-effectiveness, and potential to couple with miniature GC to accomplish the field speciation of mercury in rice compared to conventional hyphenated techniques.

  20. Natural compounds of Palestine flora. Comparison analysis by static headspace and steam distillation GC-MS of semivolatile secondary metabolites from leaves of cultivated Palestinian Majorana syriaca.

    Science.gov (United States)

    Abu-Lafi, Saleh; Odeh, Imad; Dewik, Hasan; Qabajah, Mohammed; Imam, Amin; Dembitsky, Valery M; Hanus, Lumir O

    2007-06-01

    A comparative analysis by using static headspace (HS) and steam distillation (SD) GC-MS of the volatile and the semi-volatile secondary metabolites from leaves of cultivated Majorana syriaca. The essential oils endogenous to cultivated thyme were isolated and identified by HS-GC-MS technology and compared to those from SD-GC-MS. The HS-GC-MS results showed that the Palestinian cultivated thyme is rich in monoterpene hydrocarbons and phenolic monoterpenes such as alpha-phellandrene, alpha-pinene, beta-myrcene, m-cymene, p-cymene, gamma-terpinene, thymol and carvacrol. In all the samples gamma-terpinene, p-cymene, thymol and carvacrol were the most abundant compounds. HS and SD-GC-MS have proved that most of the cultivated thyme samples examined has thymol isomer as the major phenolic constituent.

  1. Development of a rapid and sensitive method for the simultaneous determination of 1,2-dibromoethane, 1,4-dichlorobenzene and naphthalene residues in honey using HS-SPME coupled with GC-MS.

    Science.gov (United States)

    Tsimeli, K; Triantis, T M; Dimotikali, D; Hiskia, A

    2008-06-09

    A new method for the simultaneous determination of 1,4-dichlorobenzene (p-DCB), naphthalene and 1,2-dibromoethane (1,2-DBE) residues in honey has been developed. Analysis is carried out using gas chromatography-mass spectrometry (GC/MS) in selected ion monitoring mode (SIM), after extraction and preconcentration of target analytes by headspace solid-phase microextraction (HS-SPME), with a 100 microm film thickness polydimethylsiloxane (PDMS) fiber. Several parameters affecting the extension of the adsorption process (i.e., addition of salt, extraction time, extraction temperature) were studied. The optimal conditions for the determination of these analytes were established. The proposed HS-SPME method showed good sensitivity, without carryover between the samples. Linearity was studied from 5 to 2500 microg kg(-1) for p-DCB, 0.5 to 500 microg kg(-1) for naphthalene and 5 to 500 microg kg(-1) honey for 1,2-DBE with correlation coefficients (r(2)) ranging from 0.9901 to 0.9999. Precision was assessed and both intra and inter-day R.S.D.s (%) were below 6.3%. The detection limits were found to be 1, 0.1 and 2 microg kg(-1) honey for p-DCB, naphthalene and 1,2-DBE, respectively. The percentage recoveries that were evaluated with the proposed HS-SPME method and the standard addition calibration technique gave values among 72.8 and 104.3% for measurements in samples spiked with one target analyte or mixtures of the three. This method has been applied for the analysis of unknown honey samples. The results showed an excellent applicability of the proposed method for the determination of the target compounds in honey samples.

  2. Volatile compound changes during shelf life of dried Boletus edulis: comparison between SPME-GC-MS and PTR-ToF-MS analysis.

    Science.gov (United States)

    Aprea, Eugenio; Romano, Andrea; Betta, Emanuela; Biasioli, Franco; Cappellin, Luca; Fanti, Marco; Gasperi, Flavia

    2015-01-01

    Drying process is commonly used to allow long time storage of valuable porcini mushrooms (Boletus edulis). Although considered a stable product dried porcini flavour changes during storage. Monitoring of volatile compounds during shelf life may help to understand the nature of the observed changes. In the present work two mass spectrometric techniques were used to monitor the evolution of volatile compounds during commercial shelf life of dried porcini. Solid phase microextraction (SPME) coupled to gas chromatography - mass spectrometry (GC-MS) allowed the identification of 66 volatile compounds, 36 of which reported for the first time, monitored during the commercial shelf life of dried porcini. Proton transfer reaction - time of flight - mass spectrometry (PTR-ToF-MS) , a direct injection mass spectrometric technique, was shown to be a fast and sensitive instrument for the general monitoring of volatile compound evolution during storage of dried porcini. Furthermore, PTR-ToF-MS grants access to compounds whose determination would otherwise require lengthy pre-concentration and/or derivatization steps such as ammonia and small volatile amines. The two techniques, both used for the first time to study dried porcini, provided detailed description of time evolution of volatile compounds during shelf life. Alcohols, aldehydes, ketones and monoterpenes diminish during the storage while carboxylic acids, pyrazines, lactones and amines increase. The storage temperature modifies the rate of the observed changes influencing the final quality of the dried porcini. We showed the advantages of both techniques, suggesting a strategy to be adopted to follow time evolution of volatile compounds in food products during shelf life, based on the identification of compounds by GC-MS and the rapid time monitoring by PTR-ToF-MS measurements in order to maximize the advantages of both techniques. Copyright © 2015 John Wiley & Sons, Ltd.

  3. Determination of Odor Release in Hydrocolloid Model Systems Containing Original or Carboxylated Cellulose at Different pH Values Using Static Headspace Gas Chromatographic (SHS-GC Analysis

    Directory of Open Access Journals (Sweden)

    Pahn-Shick Chang

    2013-02-01

    Full Text Available Static headspace gas chromatographic (SHS-GC analysis was performed to determine the release of 13 odorants in hydrocolloid model systems containing original or regio-selectively carboxylated cellulose at different pH values. The release of most odor compounds was decreased in the hydrocolloid solutions compared to control, with the amounts of 2-propanol, 3-methyl-1-butanol, and 2,3-butanedione released into the headspace being less than those of any other odor compound in the hydrocolloid model systems. However, there was no considerable difference between original cellulose-containing and carboxylated-cellulose containing systems in the release of most compounds, except for relatively long-chain esters such as ethyl caprylate and ethyl nonanoate. The release from the original and carboxylated cellulose solutions controlled to pH 10 was significantly higher than that from solutions adjusted to pH 4 and 7 in the case of some esters (ethyl acetate, methyl propionate, ethyl propionate, ethyl butyrate, butyl propionate, ethyl caproate and alcohols (2-propanol, 3-methyl-1-butanol, in particular, ethyl butyrate and 3-methyl-1-butanol. In contrast, the release of 2,3-butanedione from both the original and carboxylated cellulose solutions was increased at pH 4 and 7 compared to that at pH 10 by about 70% and 130%, respectively. Our study demonstrated that the release of some odorants could be changed significantly by addition of both original and carboxylated cellulose in hydrocolloid model systems, but only minor effect was observed in pH of the solution.

  4. Identification of Flavor Components in Perfumes by Headspace Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry

    Science.gov (United States)

    Knupp, Gerd; Kusch, Peter; Neugebauer, Michael

    2002-01-01

    An experiment for identification of flavor components in Original Eau de Cologne by headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS) with electron impact ionization was developed. A new SPME fiber with a dual coating of divinylbenzene and Carboxen, each suspended in polydimethylsiloxane, was used. The compounds were identified by search of the NIST 98 MS Library or by comparison with pure standards. The experiment was developed for second-year chemistry students to learn the principles of analytical instrumentation (GC-MS) and sample preparation techniques (HS-SPME). The students are able to complete this experiment in a single four-hour laboratory session.

  5. Sampling methods for the study of volatile profile of PDO wine vinegars. A comparison using multivariate data analysis.

    Science.gov (United States)

    Ríos-Reina, Rocío; Morales, M Lourdes; García-González, Diego L; Amigo, José M; Callejón, Raquel M

    2018-03-01

    High-quality wine vinegars have been registered in Spain under protected designation of origin (PDO): "Vinagre de Jerez", "Vinagre de Condado de Huelva" and "Vinagre de Montilla-Moriles". The raw material, production and aging processes determine their quality and their aromatic composition. Vinegar volatile profile is usually analyzed by gas chromatography-mass spectrometry (GC-MS), being necessary a previous extraction step. Thus, three different sampling methods (Headspace solid phase microextraction "HS-SPME", Headspace stir bar sorptive extraction "HSSE" and Dynamic headspace extraction "DHS") were studied for the analysis of the volatile composition of Spanish PDO wine vinegars. Multivariate curve resolution (MCR) was used to solve chromatographic problems, improving the results obtained. Principal component analysis (PCA) showed that not all the sampling methods were equally suitable for the characterization and differentiation between PDOs and categories, being HSSE the technique that made able the best vinegar characterization. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

    Directory of Open Access Journals (Sweden)

    Z. Marijanović

    2009-01-01

    Full Text Available 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 extraction (USE. These methods display a varying degree of selectivity and effectiveness depending upon the compounds involved and the extraction conditions. Recent developments of these methods are discussed, with application examples drawn from the literature as well from our own research. Flavour qualities of the honey are very much dependent on the volatile and semivolatile organic compounds present in both the sample matrix and the headspace aroma. Therefore the use of one single technique is not adequate for reliable honey volatiles profiling, but combined use of headspace extraction and ultrasonic solvent extraction could be a useful tool for the characterization of the honey and identification of its botanical source through typical volatile marker compounds.

  7. NMR investigation of acrolein stability in hydroalcoholic solution as a foundation for the valid HS-SPME/GC–MS quantification of the unsaturated aldehyde in beverages

    Energy Technology Data Exchange (ETDEWEB)

    Kächele, Martin [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Hochschule Mannheim, Paul-Wittsack-Strasse 10, D-68163 Mannheim (Germany); Monakhova, Yulia B. [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Bruker Biospin GmbH, Silbersteifen, 76287 Rheinstetten (Germany); Department of Chemistry, Saratov State University, Astrakhanskaya Street 83, 410012 Saratov (Russian Federation); Kuballa, Thomas [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Lachenmeier, Dirk W., E-mail: lachenmeier@web.de [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Ministry of Rural Affairs and Consumer Protection, Kernerplatz 10, 70182 Stuttgart (Germany)

    2014-04-01

    Highlights: • Acrolein in hydroalcoholic solution degrades to 1,3,3-propanetriol and 3-hydroxypropionaldehyde. • Hydroquinone (0.2%) at pH 3.0 stabilizes acrolein solutions. • Quantitative HS-SPME/GC–MS determination of acrolein in alcoholic beverages was developed (LOD 14 μg L⁻¹. • 6 of 117 samples had acrolein levels above the WHO threshold (1500 μg L⁻¹). Abstract: Acrolein (propenal) is found in many foods and beverages and may pose a health hazard due to its cytotoxicity. Considerable knowledge gaps regarding human exposure to acrolein exist, and there is a lack of reliable analytical methods. Hydroalcoholic dilutions prepared for calibration purposes from pure acrolein show considerable degradation of the compound and nuclear magnetic resonance (NMR) spectroscopy showed that 1,3,3-propanetriol and 3-hydroxypropionaldehyde are formed. The degradation can be prevented by addition of hydroquinone as stabilizer to the calibration solutions, which then show linear concentration-response behaviour required for quantitative analysis. The stabilized calibration solutions were used for quantitative headspace solid-phase microextraction/gas chromatography–mass spectrometry (HS-SPME/GC–MS) determination of acrolein in alcoholic beverages with a detection limit of 14 μg L⁻¹. Of 117 tested alcoholic beverages, 64 were tested positive with the highest incidence in grape marc spirits and whiskey (100%, mean 252 μg L⁻¹), followed by fruit spirits (86%, mean 591 μg/L⁻¹), tequila (86%, mean 404 μg L⁻¹), Asian spirits (43%, mean 54 μg L⁻¹) and wine (9%, mean 0.7 μg L⁻¹). Acrolein could not be detected in beer, vodka, absinthe and bottled water. Six of the fruit and grape marc spirits had acrolein levels above the World Health Organization (WHO) provisional tolerable concentration of 1.5 mg L⁻¹.

  8. NMR investigation of acrolein stability in hydroalcoholic solution as a foundation for the valid HS-SPME/GC–MS quantification of the unsaturated aldehyde in beverages

    International Nuclear Information System (INIS)

    Kächele, Martin; Monakhova, Yulia B.; Kuballa, Thomas; Lachenmeier, Dirk W.

    2014-01-01

    Highlights: • Acrolein in hydroalcoholic solution degrades to 1,3,3-propanetriol and 3-hydroxypropionaldehyde. • Hydroquinone (0.2%) at pH 3.0 stabilizes acrolein solutions. • Quantitative HS-SPME/GC–MS determination of acrolein in alcoholic beverages was developed (LOD 14 μg L −1 ). • 6 of 117 samples had acrolein levels above the WHO threshold (1500 μg L −1 ). - Abstract: Acrolein (propenal) is found in many foods and beverages and may pose a health hazard due to its cytotoxicity. Considerable knowledge gaps regarding human exposure to acrolein exist, and there is a lack of reliable analytical methods. Hydroalcoholic dilutions prepared for calibration purposes from pure acrolein show considerable degradation of the compound and nuclear magnetic resonance (NMR) spectroscopy showed that 1,3,3-propanetriol and 3-hydroxypropionaldehyde are formed. The degradation can be prevented by addition of hydroquinone as stabilizer to the calibration solutions, which then show linear concentration-response behaviour required for quantitative analysis. The stabilized calibration solutions were used for quantitative headspace solid-phase microextraction/gas chromatography–mass spectrometry (HS-SPME/GC–MS) determination of acrolein in alcoholic beverages with a detection limit of 14 μg L −1 . Of 117 tested alcoholic beverages, 64 were tested positive with the highest incidence in grape marc spirits and whiskey (100%, mean 252 μg L −1 ), followed by fruit spirits (86%, mean 591 μg/L −1 ), tequila (86%, mean 404 μg L −1 ), Asian spirits (43%, mean 54 μg L −1 ) and wine (9%, mean 0.7 μg L −1 ). Acrolein could not be detected in beer, vodka, absinthe and bottled water. Six of the fruit and grape marc spirits had acrolein levels above the World Health Organization (WHO) provisional tolerable concentration of 1.5 mg L −1

  9. Characterization of volatile profile from ten different varieties of Chinese jujubes by HS-SPME/GC-MS coupled with E-nose.

    Science.gov (United States)

    Chen, Qinqin; Song, Jianxin; Bi, Jinfeng; Meng, Xianjun; Wu, Xinye

    2018-03-01

    Volatile profile of ten different varieties of fresh jujubes was characterized by HS-SPME/GC-MS (headspace solid phase micro-extraction combined with gas chromatography-mass spectrometry) and E-nose (electronic nose). GC-MS results showed that a total of 51 aroma compounds were identified in jujubes, hexanoic acid, hexanal, (E)-2-hexenal, (Z)-2-heptenal, benzaldehyde and (E)-2-nonenal were the main aroma components with contributions that over 70%. Differentiation of jujube varieties was conducted by cluster analysis of GC-MS data and principal component analysis & linear discriminant analysis of E-nose data. Both results showed that jujubes could be mainly divided into two groups: group A (JZ, PDDZ, JSXZ and LWZZ) and group B (BZ, YZ, MZ, XZ and DZ). There were significant differences in contents of alcohols, acids and aromatic compounds between group A and B. GC-MS coupled with E-nose could be a fast and accurate method to identify the general flavor difference in different varieties of jujubes. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. [Analyze on volatile compounds of Antrodia camphorata using HS-SPME-GC-MS].

    Science.gov (United States)

    He, Zhe; Lu, Zhen-Ming; Xu, Hong-Yu; Shi, Jing-Song; Xu, Zheng-Hong

    2011-11-01

    To analyze the volatile compounds of Antrodia camphorata in solid-state and submerged cultures. A headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry(GC-MS) were used to evaluate the profile of the volatile compounds. 49 volatile compounds were identified in A. camphorata mycelia in submerged culture, while 43 volatile compounds were identified in mycelia in solid-state culture. 1-octen-3-ol, 3-octanone, 1-octen-3-ylacetate, acetic acid octyl ester and ethanol were the main volatile compounds in A. camphorata mycelia in submerged culture, while 1-octen-3-ol, 3-octanone, 3-methyl-butyraldenhyde, gamma-podecalactone and methyl 2-furozte were the most potent key volatile compounds in mycelia in solid-state culture. The volatile compounds in the mycelia of A. camphorata in solid-state and submerged cultures are similar but their relative contents are different.

  11. A New Method for the Fast Analysis of Trihalomethanes in Tap and Recycled Waters Using Headspace Gas Chromatography with Micro-Electron Capture Detection

    Directory of Open Access Journals (Sweden)

    Lydon D. Alexandrou

    2017-05-01

    Full Text Available Chemical disinfection of water supplies brings significant public health benefits by reducing microbial contamination. The process can however, result in the formation of toxic compounds through interactions between disinfectants and organic material in the source water. These new compounds are termed disinfection by-products (DBPs. The most common are the trihalomethanes (THMs such as trichloromethane (chloroform, dichlorobromomethane, chlorodibromomethane and tribromomethane (bromoform; these are commonly reported as a single value for total trihalomethanes (TTHMs. Analysis of DBPs is commonly performed via time- and solvent-intensive sample preparation techniques such as liquid–liquid and solid phase extraction. In this study, a method using headspace gas chromatography with micro-electron capture detection was developed and applied for the analysis of THMs in drinking and recycled waters from across Melbourne (Victoria, Australia. The method allowed almost complete removal of the sample preparation step whilst maintaining trace level detection limits (>1 ppb. All drinking water samples had TTHM concentrations below the Australian regulatory limit of 250 µg/L but some were above the U.S. EPA limit of 60 µg/L. The highest TTHM concentration was 67.2 µg/L and lowest 22.9 µg/L. For recycled water, samples taken directly from treatment plants held significantly higher concentrations (153.2 µg/L TTHM compared to samples from final use locations (4.9–9.3 µg/L.

  12. Head-Space Solid Phase Micro-extraction Followed by GC/MS Analysis of the Volatile Components in Seeds of Cinnamonum camphora

    OpenAIRE

    Yang Yong; Tao Wenyi

    2005-01-01

    The volatile components in seeds of Cinnamomum camphora were analyzed by Solid Phase Micro-extraction (SPME) combined with GC/MS. Twenty four main kinds of volatile compounds, among which the Sesquiterpene (29%), 3-Hexen-2-one (25%) and Monoterpene (10.22%), were separated and analyzed.

  13. Non-destructive profiling of volatile organic compounds using HS-SPME/GC–MS and its application for the geographical discrimination of white rice

    Directory of Open Access Journals (Sweden)

    Dong Kyu Lim

    2018-01-01

    Full Text Available The authenticity determination of white rice is crucial to prevent deceptive origin labeling and dishonest trading. However, a non-destructive and comprehensive method for rapidly discriminating the geographical origins of white rice between countries is still lacking. In the current study, we developed a volatile organic compound based geographical discrimination method using headspace solid-phase microextraction coupled to gas chromatography–mass spectrometry (HS-SPME/GC–MS to discriminate rice samples from Korea and China. A partial least squares discriminant analysis (PLS-DA model exhibited a good classification of white rice between Korea and China (accuracy = 0.958, goodness of fit = 0.937, goodness of prediction = 0.831, and permutation test p-value = 0.043. Combining the PLS-DA based feature selection with the differentially expressed features from the unpaired t-test and significance analysis of microarrays, 12 discriminatory biomarkers were found. Among them, hexanal and 1-hexanol have been previously known to be associated with the cultivation environment and storage conditions. Other hydrocarbon biomarkers are novel, and their impact on rice production and storage remains to be elucidated. In conclusion, our findings highlight the ability to rapidly discriminate white rice from Korea and China. The developed method maybe useful for the authenticity and quality control of white rice.

  14. Stable isotope dilution assay (SIDA) and HS-SPME-GCMS quantification of key aroma volatiles for fruit and sap of Australian mango cultivars.

    Science.gov (United States)

    San, Anh T; Joyce, Daryl C; Hofman, Peter J; Macnish, Andrew J; Webb, Richard I; Matovic, Nicolas J; Williams, Craig M; De Voss, James J; Wong, Siew H; Smyth, Heather E

    2017-04-15

    Reported herein is a high throughput method to quantify in a single analysis the key volatiles that contribute to the aroma of commercially significant mango cultivars grown in Australia. The method constitutes stable isotope dilution analysis (SIDA) in conjunction with headspace (HS) solid-phase microextraction (SPME) coupled with gas-chromatography mass spectrometry (GCMS). Deuterium labelled analogues of the target analytes were either purchased commercially or synthesised for use as internal standards. Seven volatiles, hexanal, 3-carene, α-terpinene, p-cymene, limonene, α-terpinolene and ethyl octanoate, were targeted. The resulting calibration functions had determination coefficients (R 2 ) ranging from 0.93775 to 0.99741. High recovery efficiencies for spiked mango samples were also achieved. The method was applied to identify the key aroma volatile compounds produced by 'Kensington Pride' and 'B74' mango fruit and by 'Honey Gold' mango sap. This method represents a marked improvement over current methods for detecting and measuring concentrations of mango fruit and sap volatiles. Copyright © 2016 Elsevier Ltd. All rights reserved.

  15. Prediction of Partition Coefficients of Organic Compounds for SPME/PDMS

    Directory of Open Access Journals (Sweden)

    Liao Hsuan-Yu

    2016-01-01

    Full Text Available The partition coefficients of 51 organic compounds between SPME/PDMS and gas were compiled from the literature sources in this study. The effect of physicochemical properties and descriptors on the partitioning process of partition coefficients was explicated by the correlation analysis. The PDMS-gas partition coefficients were well correlated to the molecular weight of organic compounds (r = 0.832, p < 0.05. An empirical model, consisting of the molecular weight and the polarizability, was developed to appropriately predict the partition coefficients of organic compounds. The empirical model for estimating the PDMS-gas partition coefficient will contribute to the practical applications of the SPME technique.

  16. Quantitative Determination of Caffeine in Beverages Using a Combined SPME-GC/MS Method

    Science.gov (United States)

    Pawliszyn, Janusz; Yang, Min J.; Orton, Maureen L.

    1997-09-01

    Solid-phase microextraction (SPME) combined with gas chromatography/mass spectrometry (GC/MS) has been applied to the analysis of various caffeinated beverages. Unlike the current methods, this technique is solvent free and requires no pH adjustments. The simplicity of the SPME-GC/MS method lends itself to a good undergraduate laboratory practice. This publication describes the analytical conditions and presents the data for determination of caffeine in coffee, tea, and coke. Quantitation by isotopic dilution is also illustrated.

  17. Full evaporation dynamic headspace and gas chromatography-mass spectrometry for uniform enrichment of odor compounds in aqueous samples.

    Science.gov (United States)

    Ochiai, Nobuo; Sasamoto, Kikuo; Hoffmann, Andreas; Okanoya, Kazunori

    2012-06-01

    A method for analysis of a wide range of odor compounds in aqueous samples at sub-ng mL⁻¹ to μg mL⁻¹ levels was developed by full evaporation dynamic headspace (FEDHS) and gas chromatography-mass spectrometry (GC-MS). Compared to conventional DHS and headspace solid phase microextraction (HS-SPME), FEDHS provides more uniform enrichment over the entire polarity range for odor compounds in aqueous samples. FEDHS at 80°C using 3 L of purge gas allows complete vaporization of 100 μL of an aqueous sample, and trapping and drying it in an adsorbent packed tube, while providing high recoveries (85-103%) of the 18 model odor compounds (water solubility at 25°C: log0.54-5.65 mg L⁻¹, vapor pressure at 25°C: 0.011-3.2 mm Hg) and leaving most of the low volatile matrix behind. The FEDHS-GC-MS method showed good linearity (r²>0.9909) and high sensitivity (limit of detection: 0.21-5.2 ng mL⁻¹) for the model compounds even with the scan mode in the conventional MS. The feasibility and benefit of the method was demonstrated with analyses of key odor compounds including hydrophilic and less volatile characteristics in beverages (whiskey and green tea). In a single malt whiskey sample, phenolic compounds including vanillin could be determined in the range of 0.92-5.1 μg mL⁻¹ (RSDfuraneol, indole, maltol, and pyrazine congeners) were determined in the range of 0.21-110 ng mL⁻¹ (RSD<10%, n=6). Copyright © 2012 Elsevier B.V. All rights reserved.

  18. Headspace versus direct immersion solid phase microextraction in complex matrixes: investigation of analyte behavior in multicomponent mixtures.

    Science.gov (United States)

    Gionfriddo, Emanuela; Souza-Silva, Érica A; Pawliszyn, Janusz

    2015-08-18

    This work aims to investigate the behavior of analytes in complex mixtures and matrixes with the use of solid-phase microextraction (SPME). Various factors that influence analyte uptake such as coating chemistry, extraction mode, the physicochemical properties of analytes, and matrix complexity were considered. At first, an aqueous system containing analytes bearing different hydrophobicities, molecular weights, and chemical functionalities was investigated by using commercially available liquid and solid porous coatings. The differences in the mass transfer mechanisms resulted in a more pronounced occurrence of coating saturation in headspace mode. Contrariwise, direct immersion extraction minimizes the occurrence of artifacts related to coating saturation and provides enhanced extraction of polar compounds. In addition, matrix-compatible PDMS-modified solid coatings, characterized by a new morphology that avoids coating fouling, were compared to their nonmodified analogues. The obtained results indicate that PDMS-modified coatings reduce artifacts associated with coating saturation, even in headspace mode. This factor, coupled to their matrix compatibility, make the use of direct SPME very practical as a quantification approach and the best choice for metabolomics studies where wide coverage is intended. To further understand the influence on analyte uptake on a system where additional interactions occur due to matrix components, ex vivo and in vivo sampling conditions were simulated using a starch matrix model, with the aim of mimicking plant-derived materials. Our results corroborate the fact that matrix handling can affect analyte/matrix equilibria, with consequent release of high concentrations of previously bound hydrophobic compounds, potentially leading to coating saturation. Direct immersion SPME limited the occurrence of the artifacts, which confirms the suitability of SPME for in vivo applications. These findings shed light into the implementation of in

  19. Effect of hot air drying on volatile compounds of Flammulina velutipes detected by HS-SPME-GC-MS and electronic nose.

    Science.gov (United States)

    Yang, Wenjian; Yu, Jie; Pei, Fei; Mariga, Alfred Mugambi; Ma, Ning; Fang, Yong; Hu, Qiuhui

    2016-04-01

    Volatile compounds are important factors that affect the flavor quality of Flammulina velutipes, but the changes occurring during hot air drying is still unclear. To clarify the dynamic changes of flavor components during hot air drying, comprehensive flavor characterization and volatile compounds of F. velutipes were evaluated using electronic nose technology and headspace solid phase micro-extraction combined with gas chromatography-mass spectrometry (HS-SPME-GC-MS), respectively. Results showed that volatile components in F. velutipes significantly changed during hot air drying according to the principal component analysis and radar fingerprint chart of electronic nose. Volatile compounds of fresh F. velutipes consisted mainly of ketones, aldehydes and alcohols, and 3-octanone was the dominant compound. Drying process could significantly decrease the relative content of ketones and promoted the generation of alcohols, acids, and esters, which became the main volatile compounds of dried F. velutipes. These may provide a theoretical basis for the formation mechanism of flavor substances in dried F. velutipes. Copyright © 2015 Elsevier Ltd. All rights reserved.

  20. 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

    International Nuclear Information System (INIS)

    Jiao, Jiao; Ma, Dan-Hui; Gai, Qing-Yan; Wang, Wei; Luo, Meng; Fu, Yu-Jie; Ma, Wei

    2013-01-01

    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 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

  1. 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.

  2. 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

  3. Sol-gel-based SPME fiber as a reliable sampling technique for studying biogenic volatile organic compounds released from Clostridium tetani.

    Science.gov (United States)

    Ghader, Masoud; Shokoufi, Nader; Es-Haghi, Ali; Kargosha, Kazem

    2017-11-01

    A novel and efficient headspace solid-phase microextraction (HS-SPME) method, followed by gas chromatography mass spectrometry (GC-MS), was developed to study volatile organic compounds (VOCs) emerging from microorganisms. Two homemade SPME fibers, a semi-polar poly (dimethylsiloxane) (PDMS) fiber, and a polar polyethylene glycol (PEG) fiber, along with two commercial fibers (PDMS and PDMS/DVB) were used to collect VOCs emerging from Clostridium tetani which was cultured in different media. The adsorbed VOCs were desorbed and identified, in vitro, using GC-MS. The adsorption efficiency was improved by optimizing the time duration of adsorption and desorption. About 50 components were identified by the proposed method. The main detected compounds appeared to be sulfur containing compounds such as butanethioic acid S-methyl ester, dimethyl trisulfide, and dimethyl tetrasulfide. These volatile sulfur containing compounds are derived from amino acids containing the sulfur element, which probably coexist in the mentioned bacterium or are added to the culture media. The developed HS-SPME-GC-MS method allowed the determination of the chemical fingerprint of Clostridium tetani volatile constituents, and thus provides a new, simple, and reliable tool for studying the growth of microorganisms. Graphical abstract Investigation of biogenic VOCs released from Clostridium tetani using SPME-GC-MS.

  4. Rapid differentiation of Chinese hop varieties (Humulus lupulus) using volatile fingerprinting by HS-SPME-GC-MS combined with multivariate statistical analysis.

    Science.gov (United States)

    Liu, Zechang; Wang, Liping; Liu, Yumei

    2018-01-18

    Hops impart flavor to beer, with the volatile components characterizing the various hop varieties and qualities. Fingerprinting, especially flavor fingerprinting, is often used to identify 'flavor products' because inconsistencies in the description of flavor may lead to an incorrect definition of beer quality. Compared to flavor fingerprinting, volatile fingerprinting is simpler and easier. We performed volatile fingerprinting using head space-solid phase micro-extraction gas chromatography-mass spectrometry combined with similarity analysis and principal component analysis (PCA) for evaluating and distinguishing between three major Chinese hops. Eighty-four volatiles were identified, which were classified into seven categories. Volatile fingerprinting based on similarity analysis did not yield any obvious result. By contrast, hop varieties and qualities were identified using volatile fingerprinting based on PCA. The potential variables explained the variance in the three hop varieties. In addition, the dendrogram and principal component score plot described the differences and classifications of hops. Volatile fingerprinting plus multivariate statistical analysis can rapidly differentiate between the different varieties and qualities of the three major Chinese hops. Furthermore, this method can be used as a reference in other fields. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

  5. 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...

  6. Comparative analysis of different methods of extraction of present hydrocarbons in industrial residual waters

    International Nuclear Information System (INIS)

    Santa, Judith Rocio; Serrano, Martin; Stashenko, Elena

    2002-01-01

    A comparison among four extraction techniques such as: liquid - liquid (LLE) continuous and for lots, solid phase extraction (SPE), solid phase micro extraction (SPME) and static headspace (S-HS) was carried out. The main purpose of this research was to determine the highest recovery efficiencies and how reproducible the tests are while varying parameters such as time, extraction technique, type of solvents and others. Chromatographic parameters were optimized in order to carry out the analyses. Hydrocarbon's quantification of residual waters was achieved by using a high-resolution gas chromatography with a gas flame ionization detector (HRGC-FID). Validation of the method was carried out by analyzing real samples taken in different sampling places of the residual waters treatment plant of Ecopetrol - Barrancabermeja. The use of extraction methods that require big solvent quantities and long time for analysis are losing validity day by day. Techniques such as the HS-SPME and static HS are offered as alternatives for quantifying hydrocarbons. They show total lack of solvents, high sensibility, selectivity and the techniques are reproducible. Solid phase micro extraction (SPME) and static headspace (static HS) techniques were chosen as the extraction techniques to validate the method in real samples. Both techniques showed similar results for the determination of total hydrocarbons (in the gasoline range)

  7. Glass bottle sampling solid phase microextraction gas chromatography mass spectrometry for breath analysis of drug metabolites.

    Science.gov (United States)

    Lu, Yan; Niu, Wenqi; Zou, Xue; Shen, Chengyin; Xia, Lei; Huang, Chaoqun; Wang, Hongzhi; Jiang, Haihe; Chu, Yannan

    2017-05-05

    Breath analysis is a non-invasive approach which may be applied to disease diagnosis and pharmacokinetic study. In the case of offline analysis, the exhaled gas needs to be collected and the sampling bag is often used as the storage vessel. However, the sampling bag usually releases some extra compounds, which may interfere with the result of the breath test. In this study, a novel breath sampling glass bottle was developed with a syringe needle sampling port for solid phase microextraction (SPME). Such a glass bottle scarcely liberates compounds and can be used to collect exhaled gas for ensuing analysis by gas chromatography-mass spectrometry (GC-MS). The glass bottle sampling SPME-GC-MS analysis was carried out to investigate the breath metabolites of myrtol, a multicompound drug normally used in the treatment of bronchitis and sinusitis. Four compounds, α-pinene, 2,3-dehydro-1,8-cineole, d-limonene and 1,8-cineole were found in the exhaled breath of all eight volunteers who had taken the myrtol. While for other ten subjects who had not used the myrtol, these compounds were undetectable. In the SPME-GC-MS analysis of the headspace of myrtol, three compounds were detected including α-pinene, d-limonene and 1,8-cineole. Comparing the results of breath and headspace analysis, it indicates that 2,3-dehydro-1,8-cineole in the breath is the metabolite of 1,8-cineole. It is the first time that this metabolite was identified in human breath. The study demonstrates that the glass bottle sampling SPME-GC-MS method is applicable to exhaled gas analysis including breath metabolites investigation of drugs like myrtol. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Simultaneous analysis of organochlorine pesticides and polychlorinated biphenyls in air samples by using accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) coupled to gas chromatography dual electron capture detection.

    Science.gov (United States)

    Mokbel, Haifaa; Al Dine, Enaam Jamal; Elmoll, Ahmad; Liaud, Céline; Millet, Maurice

    2016-04-01

    An analytical method associating accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) in immersion mode combined with gas chromatography dual electrons capture detectors (SPME-GC-2ECD) has been developed and studied for the simultaneous determination of 19 organochlorine pesticides (OCPs) and 22 polychlorinated biphenyls (PCBs) in air samples (active and XAD-2 passive samplers). Samples were extracted with ASE with acetonitrile using the following conditions: temperature, 150 °C; pressure, 1500 psi; static, 15 min; cycles, 3; purge, 300 s; flush, 100 %. Extracts were reduced to 1 mL, and 500 μL of this extract, filled with deionised water, was subject to SPME extraction. Experimental results indicated that the proposed method attained the best extraction efficiency under the optimised conditions: extraction of PCB-OCP mixture using 100-μm PDMS fibre at 80 °C for 40 min with no addition of salt. The performance of the proposed ASE-SPME-GC-2ECD methodology with respect to linearity, limit of quantification and detection was evaluated by spiking of XAD-2 resin with target compounds. The regression coefficient (R (2)) of most compounds was found to be high of 0.99. limits of detection (LODs) are between 0.02 and 4.90 ng m(-3), and limits of quantification (LOQs) are between 0.05 and 9.12 ng m(-3) and between 0.2 and 49 ng/sampler and 0.52 and 91 ng/sampler, respectively, for XAD-2 passive samplers. Finally, a developed procedure was applied to determine selected PCBs and OCPs in the atmosphere.

  9. Thermodynamic functions of hydrogen bonding of amines in methanol derived from solution calorimetry data and headspace analysis

    International Nuclear Information System (INIS)

    Zaitseva, Ksenia V.; Varfolomeev, Mikhail A.; Solomonov, Boris N.

    2012-01-01

    Highlights: ► Solution enthalpies and activity coefficients of amines in methanol were measured. ► Thermodynamic functions of H-bonding of amines with methanol were determined. ► Specific interaction entropy of amines in methanol can be about zero or positive. ► Cooperativity of H-bonds in methanol media is smaller than in water solutions. ► A new view on analysis of specific interaction of solute with methanol is presented. - Abstract: Reactivity and equilibrium properties of organic molecules in self-associated liquids greatly depend on the hydrogen bonding with solvent. This work contains comprehensive thermodynamic analysis of hydrogen bonding of aliphatic and aromatic amines in self-associated solvent methanol. Enthalpies of solution at infinite dilution and limiting activity coefficients for the studied systems were measured experimentally. Enthalpies and Gibbs energies of hydrogen bonding of amines with neat methanol were determined. These values were found to be decreased compared with hydrogen bond energy in equimolar complexes “methanol–amine” determined in inert solvent or base media. A linear dependence between enthalpies and Gibbs energies of hydrogen bonding of amines with neat methanol was observed. It was firstly revealed that the entropy of specific interactions of amines with neat methanol can be about zero or positive. Disruption of solvent–solvent hydrogen bonds can be regarded as the most important step during dissolution of amine in methanol. It was found that the cooperative effect influences on the Gibbs energies of hydrogen bonding of amines in methanol, but in a lesser extent than in aqueous solutions. The new results show that the hydrogen bonding process in the self-associated solvents differs significantly from equimolar complexation in aprotic media.

  10. Phytotoxic volatiles in the roots and shoots of Artemisia tridentata as detected by headspace solid-phase microextraction and gas chromatographic-mass spectrometry analysis.

    Science.gov (United States)

    Jassbi, Amir Reza; Zamanizadehnajari, Simin; Baldwin, Ian Thomas

    2010-12-01

    In the vicinity of big sagebrush (Artemisia tridentata), the growth of Nicotiana attenuata is negatively affected, in part due to the alleopathic effect of methyl jasmonate (MeJA) which is produced in large quantities by the aerial parts of sagebrush. Preliminary experiments suggested that growth-inhibiting substances were being emitted from the sagebrush roots. To identify the allelochemical secondary metabolites, we tested different root extracts in seedling growth bioassays with the naturally co-occurring native tobacco, Nicotiana attenuata, in a two-chamber Petri dish assay, optimized for tests of volatiles. Fractions rich in volatile compounds were particularly phytotoxic. We analyzed the volatiles emitted from the roots of intact Artemisia tridentata plants grown in soil, sand, and hydroponic cultures by using dynamic headspace extraction, headspace solvent-microextraction (HSME) and headspace solid-phase microextraction (HSPME), and GC-MS. Camphor, 1,8-cineol, nerol, and neryl isovalerate were phytotoxic and released as the major constituents. In addition to the phytotoxic monoterpenes, himachalenes, longifolene, caryophyllene, and acetylenic spiroethers, were found as characteristic components in the root's volatiles. The allelopathic potential of these root volatiles was compared with that of methyl jasmonate (MeJA), one of the most active compounds emitted from above-ground parts of the plant.

  11. The GC/MS Analysis of Volatile Components Extracted by Different Methods from Exocarpium Citri Grandis

    Directory of Open Access Journals (Sweden)

    Zhisheng Xie

    2013-01-01

    Full Text Available Volatile components from Exocarpium Citri Grandis (ECG were, respectively, extracted by three methods, that is, steam distillation (SD, headspace solid-phase microextraction (HS-SPME, and solvent extraction (SE. A total of 81 compounds were identified by gas chromatography-mass spectrometry including 77 (SD, 56 (HS-SPME, and 48 (SE compounds, respectively. Despite of the extraction method, terpenes (39.98~57.81% were the main volatile components of ECG, mainly germacrene-D, limonene, 2,6,8,10,14-hexadecapentaene, 2,6,11,15-tetramethyl-, (E,E,E-, and trans-caryophyllene. Comparison was made among the three methods in terms of extraction profile and property. SD relatively gave an entire profile of volatile in ECG by long-time extraction; SE enabled the analysis of low volatility and high molecular weight compounds but lost some volatiles components; HS-SPME generated satisfactory extraction efficiency and gave similar results to those of SD at analytical level when consuming less sample amount, shorter extraction time, and simpler procedure. Although SD and SE were treated as traditionally preparative extractive techniques for volatiles in both small batches and large scale, HS-SPME coupled with GC/MS could be useful and appropriative for the rapid extraction and qualitative analysis of volatile components from medicinal plants at analytical level.

  12. Poly(o-anisidine)/graphene oxide nanosheets composite as a coating for the headspace solid-phase microextraction of benzene, toluene, ethylbenzene and xylenes.

    Science.gov (United States)

    Behzadi, Mansoureh; Mirzaei, Mohammad

    2016-04-22

    A poly(o-anisidine)/graphene oxide nanosheets (PoA/GONSs) coating is fabricated by a simple and efficient electrochemical deposition method on steel wire. The incorporation of PoA and GONSs allows preparing a nanocomposite that can successfully integrate the advantages of both. Then, the prepared fiber is applied to the headspace solid-phase microextraction (HS-SPME) and gas chromatographic analysis of benzene, toluene, ethylbenzene and xylenes. In order to obtain an adherent, stable and efficient fiber to extract target analytes, experimental parameters related to the coating process such as deposition potential, deposition time, concentration of the monomer and concentration of GONSs were studied. The prepared composite fiber were characterized by Fourier transform infrared spectroscopy, powder X-ray diffraction and scanning electron microscopy. The effect of various parameters on the efficiency of HS-SPME process consisting of desorption temperature and time, extraction temperature and time and ionic strength were also optimized. Under the optimal conditions, the method was linear for orders of magnitude with correlation coefficients varying from 0.9888 to 0.9993. Intra- and inter-day precisions of the method were determined from mixed aqueous solutions containing 5.0 ng mL(-1) of each BTEX. The intra-day precisions varied from 3.1% for toluene to 5.7% for ethylbenzene, while the inter-day precisions varied from 4.9% for o-xylene to 7.3% for m,p-xylene. Limits of detection were in the range 0.01-0.06 ng mL(-1). The proposed method was applied to monitor BTEX compounds in some water samples and the accuracies found through spiking river water samples showed high recoveries between 92.0 and 101.2%. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Determination of Methyl tert-Butyl Ether and tert-Butyl Alcohol in Water by Solid-Phase Microextraction/Head Space Analysis in Comparison to EPA Method 5030/8260B

    Energy Technology Data Exchange (ETDEWEB)

    Oh, Keun-Chan; Stringfellow, William T.

    2003-10-02

    Methyl tert-butyl ether (MTBE) is now one of the most common groundwater contaminants in the United States. Groundwater contaminated with MTBE is also likely to be contaminated with tert-butyl alcohol (TBA), because TBA is a component of commercial grade MTBE, TBA can also be used as a fuel oxygenate, and TBA is a biodegradation product of MTBE. In California, MTBE is subject to reporting at concentrations greater than 3 {micro}g/L. TBA is classified as a ''contaminant of current interest'' and has a drinking water action level of 12 {micro}g/L. In this paper, we describe the development and optimization of a simple, automated solid phase microextraction (SPME) method for the analysis of MTBE and TBA in water and demonstrate the applicability of this method for monitoring MTBE and TBA contamination in groundwater, drinking water, and surface water. In this method, the headspace (HS) of a water sample is extracted with a carboxen/polydimethylsiloxane SPME fiber, the MTBE and TBA are desorbed into a gas chromatograph (GC), and detected using mass spectrometry (MS). The method is optimized for the routine analysis of MTBE and TBA with a level of quantitation of 0.3 {micro}g/L and 4 {micro}g/L, respectively, in water. MTBE quantitation was linear for over two orders of concentration (0.3 {micro}g/L -80 {micro}g/L). TBA was found to be linear within the range of 4 {micro}g/L-7,900 {micro}g/L. The lower level of detection for MTBE is 0.03 {micro}g/L using this method. This SPME method using headspace extraction was found to be advantageous over SPME methods requiring immersion of the fiber into the water samples, because it prolonged the life of the fiber by up to 400 sample analyses. This is the first time headspace extraction SPME has been shown to be applicable to the measurement of both MTBE and TBA at concentrations below regulatory action levels. This method was compared with the certified EPA Method 5030/8260B (purge-and-trap/GC/MS) using split

  14. Volatile phytochemical composition of rhizome of ginger after extraction by headspace solid-phase microextraction, petrol ether extraction and steam distillation extraction

    Directory of Open Access Journals (Sweden)

    Zhan-nan Yang

    2009-06-01

    Full Text Available The sampling techniques headspace solid-phase microextraction (HS-SPME, petrol ether extraction (PEE and steam distillation extraction (SDE were compared for the GC-MS of volatile constituents present in ginger (Zingiber officinale. The effects of different parameters, such as extraction fibers, extraction time, extraction temperature and particle size ranges, on the HSSPME of rhizome of ginger were investigated. Zingiberene (53.12% were predominant components of ginger samples obtained by HS-SPME whereas those levels were 39.01% in the same samples by PEE and 35.05% in those by SDE, respectively. HS-SPME with polydimethylsiloxane (PDMS fiber was more selective and particularly efficient for the isolation of volatile phytochemical composition and afforded a higher yield of total compounds than PEE and SDE. The specifically compound isolated by SPME, which due to effective fiber, was much larger than that isolated by PEE or SDE. HS-SPME is a powerful tool for determining the volatile constitutes present in the traditional Chinese medicines.

  15. An automated headspace solid-phasemicroextraction followed by gas chromatography–mass spectrometry method to determine macrocyclic musk fragrances in wastewater samples.

    Science.gov (United States)

    Vallecillos, Laura; Borrull, Francesc; Pocurull, Eva

    2013-11-01

    A fully automated method has been developed for determining eight macrocyclic musk fragrances in wastewater samples. The method is based on headspace solid-phase microextraction (HS-SPME) followed by gas chromatography–mass spectrometry (GC-MS). Five different fibres (PDMS 7 μm, PDMS 30 μm, PDMS 100 μm, PDMS/DVB 65 μm and PA 85 μm) were tested. The best conditions were achieved when a PDMS/DVB 65 μm fibre was exposed for 45 min in the headspace of 10 mL water samples at 100 °C. Method detection limits were found in the low ng L−1 range between 0.75 and 5 ng L−1 depending on the target analytes. Moreover, under optimized conditions, the method gave good levels of intra-day and inter-day repeatabilities in wastewater samples with relative standard deviations (n =5, 1,000 ng L−1) less than 9 and 14 %, respectively. The applicability of the method was tested with influent and effluent urban wastewater samples from different wastewater treatment plants (WWTPs). The analysis of influent urban wastewater revealed the presence of most of the target macrocyclic musks with, most notably, the maximum concentration of ambrettolide being obtained in WWTP A (4.36 μg L−1) and WWTP B (12.29 μg L−1), respectively. The analysis of effluent urban wastewater showed a decrease in target analyte concentrations, with exaltone and ambrettolide being the most abundant compounds with concentrations varying between below method quantification limit (MQL) and 2.46 μg L−1.

  16. Comparison of SPME Methods for Determining Volatile Compounds in Milk, Cheese, and Whey Powder

    Directory of Open Access Journals (Sweden)

    Michael H. Tunick

    2013-11-01

    Full Text Available Solid phase microextraction and gas chromatography-mass spectrometry (SPME-GC-MS are commonly used for qualitative and quantitative analysis of volatile compounds in various dairy products, but conditions have to be adjusted to maximize release while not generating new compounds that are absent in the original sample. Queso Fresco, a fresh non-melting cheese, may be heated at 60 °C for 30 min; in contrast, compounds are produced in milk when exposed to light and elevated temperatures, so milk samples are heated as little as possible. Products such as dehydrated whey protein are more stable and can be exposed to longer periods (60 min of warming at lower temperature (40 °C without decomposition, allowing for capture and analysis of many minor components. The techniques for determining the volatiles in dairy products by SPME and GC-MS have to be optimized to produce reliable results with minimal modifications and analysis times.

  17. Analysis of enantiomeric and non-enantiomeric monoterpenes in plant emissions using portable dynamic air sampling/solid-phase microextraction (PDAS-SPME) and chiral gas chromatography/mass spectrometry

    Science.gov (United States)

    Yassaa, Noureddine; Williams, Jonathan

    A portable dynamic air sampler (PDAS) using a porous polymer solid-phase microextraction (SPME) fibre has been validated for the determination of biogenic enantiomeric and non-enantiomeric monoterpenes in air. These compounds were adsorbed in the field, and then thermally desorbed at 250 °C in a gas chromatograph injector port connected via a β-cyclodextrin capillary separating column to a mass spectrometer. The optimized method has been applied for investigating the emissions of enantiomeric monoterpenes from Pseudotsuga menziesii (Douglas-fir), Rosmarinus officinalis (Rosemary) and Lavandula lanata (Lavender) which were selected as representative of coniferous trees and aromatic plants, respectively. The enantiomers of α-pinene, sabinene, camphene, δ-3-carene, β-pinene, limonene, β-phellandrene, 4-carene and camphor were successfully determined in the emissions from the three plants. While Douglas-fir showed a strong predominance toward (-)-enantiomers, Rosemary and Lavender demonstrated a large variation in enantiomeric distribution of monoterpenes. The simplicity, rapidity and sensitivity of dynamic sampling with porous polymer coated SPME fibres coupled to chiral capillary gas chromatography/mass spectrometry (GC/MS) makes this method potentially useful for in-field investigations of atmosphere-biosphere interactions and studies of optically explicit atmospheric chemistry.

  18. Analysis of class 1 residual solvents in pharmaceuticals using headspace-programmed temperature vaporization-fast gas chromatography-mass spectrometry.

    Science.gov (United States)

    Pérez Pavón, José Luis; Del Nogal Sánchez, Miguel; Fernández Laespada, M A Esther; García Pinto, Carmelo; Moreno Cordero, Bernardo

    2007-02-02

    A sensitive method is presented for the fast screening and determination of residual class 1 solvents (1,1-dichloroethene, 1,2-dichloroethane, 1,1,1-trichloroethane, carbon tetrachloride and benzene) in pharmaceutical products. The applicability of a headspace (HS) autosampler in combination with GC equipped with a programmed temperature vaporizer (PTV) and a MS detector is explored. Different injection techniques were compared. The benefits of using solvent vent injection instead of split or splitless-hot injection for the measurement of volatile compounds are shown: better peak shapes, better signal-to-noise ratios, and hence better detection limits. The proposed method is extremely sensitive. The limits of detection ranged from 4.9 ppt (benzene) to 7.9 ppt (1,2-dichloroethane) and precision (measured as the relative standard deviation) was equal to or lower than 12% in all cases. The method was applied to the determination of residual solvents in nine different pharmaceutical products. The analytical performance of the method shows that it is appropriate for the determination of residual class 1 solvents and has much lower detection limits than the concentration limits proposed by the International Conference on Harmonization (ICH) of Technical Requirements for the Registration of Pharmaceuticals for Human Use. The proposed method achieves a clear improvement in sensitivity with respect to conventional headspace methods due to the use of the PTV.

  19. In-situ methylation of strongly polar organic acids in natural waters supported by ion-pairing agents for headspace GC-MSD analysis

    Energy Technology Data Exchange (ETDEWEB)

    Neitzel, P.L.; Walther, W. [Dresden University of Technology, Institute for Groundwater Managemant, Dresden (Germany); Nestler, W. [Institute for Technology and Economics, Department of Civil Engineering and Architecture, Dresden (Germany)

    1998-06-01

    Strongly polar organic substances like halogenated acetic acids have been analyzed in surface water and groundwater in the catchment area of the upper Elbe river in Saxony since 1992. Coming directly from anthropogenic sources like industry, agriculture and indirectly by rainfall, their concentrations can increase up to 100 {mu}g/L in the aquatic environment of this catchment area. A new static headspace GC-MSD method without a manual pre-concentration step is presented to analyze the chlorinated acetic acids relevant to the Elbe river as their volatile methyl esters. Using an ion-pairing agent as modifier for the in-situ methylation of the analytes by dimethylsulfate, a minimal detection limit of 1 {mu}g/L can be achieved. Problems like the thermal degradation of chlorinated acetic acids to halogenated hydrocarbons and changing reaction yields during the headspace methylation, could be effectively reduced. The method has been successfully applied to monitoring bank infiltrate, surface water, groundwater and water works pumped raw water according to health provision principles. (orig.) With 3 figs., 2 tabs., 29 refs.

  20. Some recent developments in headspace gas chromatography

    Science.gov (United States)

    J.Y. Zhu; X.-S. Chai

    2005-01-01

    In this study, recent developments in headspace gas chromatography (HSGC) are briefly reviewed. Several novel HSGC techniques developed recently are presented in detail. These techniques were developed using the unique characteristics of the headspace sampling process implemented in commercial HSGC systems and therefore can be easily applied in laboratory and...

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

    Science.gov (United States)

    Conde, Francisco J; Afonso, Ana M; González, Venerando; Ayala, Juan H

    2006-08-01

    A sampling and analysis method for the determination of 21 phenolic compounds in smoke samples from biomass combustion has been developed. The smoke is used to make smoked foods, following an artisanal procedure used in some parts of the Canary Islands. The sampling system consists of a Bravo H air sampler, two impingers, each one containing an aqueous solution of sodium hydroxide 0.1 mol L(-1), followed by a silica gel trap. The variables optimized to reach the best sampling conditions were volume of absorbent solution and sampling flow. Under the optimum conditions, 100 mL of absorbent solution of NaOH 0.10 mol L(-1) and 2 L min(-1) for the sampling flow, sampling efficiencies are higher than 80%. Analysis of phenolic compounds was carried out by headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). Five different fiber coatings were employed in this study. By means of a central composite design, extraction time, salt concentration, and pH of the solution were optimized: 65-microm carbowax-divinylbenzene, extraction time 90 min, concentration in NaCl of 35% (m/v), and pH 2 yielded the highest response. Detection limits of phenol and their alkyl derivatives, guaiacol and eugenol, are between 1.13 and 4.60 ng mL(-1). 3-Methoxyphenol, 2,6-dimethoxyphenol, and vanillin have detection limits considerably higher. Good linearity (R2 > or = 0.98) was observed for all calibration curves in the established ranges. The reproducibility of the method (RSD, relative standard deviation) was found to oscillate between 7 and 18% (generally close or lower than 10%).

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-08-15

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

  3. 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.

  4. SPME as a promising tool in translational medicine and drug discovery: From bench to bedside.

    Science.gov (United States)

    Goryński, Krzysztof; Goryńska, Paulina; Górska, Agnieszka; Harężlak, Tomasz; Jaroch, Alina; Jaroch, Karol; Lendor, Sofia; Skobowiat, Cezary; Bojko, Barbara

    2016-10-25

    Solid phase microextraction (SPME) is a technology where a small amount of an extracting phase dispersed on a solid support is exposed to the sample for a well-defined period of time. The open-bed geometry and biocompatibility of the materials used for manufacturing of the devices makes it very convenient tool for direct extraction from complex biological matrices. The flexibility of the formats permits tailoring the method according the needs of the particular application. Number of studies concerning monitoring of drugs and their metabolites, analysis of metabolome of volatile as well as non-volatile compounds, determination of ligand-protein binding, permeability and compound toxicity was already reported. All these applications were performed in different matrices including biological fluids and tissues, cell cultures, and in living animals. The low invasiveness of in vivo SPME, ability of using very small sample volumes and analysis of cell cultures permits to address the rule of 3R, which is currently acknowledged ethical standard in R&D labs. In the current review systematic evaluation of the applicability of SPME to studies required to be conduct at different stages of drug discovery and development and translational medicine is presented. The advantages and challenges are discussed based on the examples directly showing given experimental design or on the studies, which could be translated to the models routinely used in drug development process. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Study of flavour compounds from orange juices by HS-SPME and GC-MS

    Science.gov (United States)

    Schmutzer, G.; Avram, V.; Covaciu, F.; Feher, I.; Magdas, A.; David, L.; Moldovan, Z.

    2013-11-01

    The flavour of the orange juices, which gives the taste and odour of the product, is an important criterion about the products quality for consumers. A fresh single strength and two commercial orange juices (obtained from concentrate) flavour profile were studied using a selective and sensitive gas chromatography - mass spectrometry (GC-MS) analytical system, after a solvent free, single step preconcentration and extraction technique, the headspace solid phase microextraction (HP-SPME). In the studied orange juices 55 flavour compounds were detected and classified as belonging to the esters, alcohols, ketones, monoterpenes and sesquiterpenes chemical families. The fresh single strength orange juice was characterized by high amount of esters, monoterpenes and sesquiterpenes. Limonene and valencene were the most abundant flavours in this fresh natural orange juice. Alcohols and ketones were found in higher concentration in the commercial orange juices made from concentrate, than in the single strength products. Nevertheless, in commercial juices the most abundant flavour was limonene and α-terpineol. The results highlight clear differences between fresh singles strength orange juice and juice from concentrate. The orange juices reconstructed from concentrate, made in Romania, present low quantity of flavour compounds, suggesting the absence or a low rearomatization process, but extraneous components were not detected.

  6. Volatile emerging contaminants in melon fruits, analysed by HS-SPME-GC-MS.

    Science.gov (United States)

    Cincotta, Fabrizio; Verzera, Antonella; Tripodi, Gianluca; Condurso, Concetta

    2018-03-01

    The aim of this research was to develop and validate a headspace-solid phase micro-extraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) method for the determination of volatile emerging contaminants in fruit. The method showed good precision (RSD ≤ 14%) and satisfactory recoveries (99.1-101.7%) and LOD and LOQ values ranging between 0.011-0.033 μg kg -1 and 0.037-0.098 μg kg -1 , respectively. The method was applied to investigate the content of volatile emerging contaminants in two varieties of melon fruit (Cucumis melo L.) cultivated adjoining high-risk areas. Glycol ethers, BHT, BHA and BTEX (benzene, toluene, ethylbenzene and xylene) were determined in melon fruit pulps for the first time, with different sensitivities depending on sample and variety. Although the amount of the volatile contaminants in the melon samples were in the order of µg kg -1 , the safety of vegetable crops cultivated near risk areas should be more widely considered. The results showed that this accurate and reproducible method can be useful for routine safety control of fruits and vegetables.

  7. Simultaneous determination of Hg(II) and alkylated Hg, Pb, and Sn species in human body fluids using SPME-GC/MS-MS

    Energy Technology Data Exchange (ETDEWEB)

    Dunemann, L.; Hajimiragha, H.; Begerow, J. [Department of Analytical Chemistry, Medizinisches Inst. fuer Umwelthygiene, Duesseldorf (Germany)

    1999-03-01

    A GC/MS-MS method for the determination of Hg(II) and alkylated Hg, Pb, and Sn species in human urine is described. Separation and identification of the metal species are performed by capillary gas chromatography coupled with an ion-trap mass spectrometer with electron impact ionization in the tandem-MS mode. For sample preparation a very promising technique was applied that is based on a derivatization with sodium tetraethylborate followed by headspace solid phase microextraction (SPME). Operation of the used ion trap in the tandem-MS mode yields in improved detection limits because of a signal-to-noise ratio that is at least one order of magnitude better than in the MS mode. The detection limits in real matrices like urine are between 7 and 22 ng/L for all species investigated. Urinary levels of inorganic Hg in non-occupationally exposed persons with and without dental amalgam were found to be between 0.1 and 1.4 {mu}g/L. A reference material (``ClinRep, Level I``) was used for quality assurance. Compared to the coupling of GC with ICP-MS (``inorganic`` MS), the advantage of the proposed method using an ``organic`` MS is that (i) the species can be directly identified via their precursor and daughter ions and (ii) analysis can be performed with a commercially available hyphenated technique at moderate costs and needs no lab-made interfacing. Moreover, it offers a real multi-element/multi-species capability with low detection limits and a minimum of sample preparation. (orig.) With 1 fig., 1 tab., 9 refs.

  8. NMR investigation of acrolein stability in hydroalcoholic solution as a foundation for the valid HS-SPME/GC-MS quantification of the unsaturated aldehyde in beverages.

    Science.gov (United States)

    Kächele, Martin; Monakhova, Yulia B; Kuballa, Thomas; Lachenmeier, Dirk W

    2014-04-11

    Acrolein (propenal) is found in many foods and beverages and may pose a health hazard due to its cytotoxicity. Considerable knowledge gaps regarding human exposure to acrolein exist, and there is a lack of reliable analytical methods. Hydroalcoholic dilutions prepared for calibration purposes from pure acrolein show considerable degradation of the compound and nuclear magnetic resonance (NMR) spectroscopy showed that 1,3,3-propanetriol and 3-hydroxypropionaldehyde are formed. The degradation can be prevented by addition of hydroquinone as stabilizer to the calibration solutions, which then show linear concentration-response behaviour required for quantitative analysis. The stabilized calibration solutions were used for quantitative headspace solid-phase microextraction/gas chromatography-mass spectrometry (HS-SPME/GC-MS) determination of acrolein in alcoholic beverages with a detection limit of 14 μg L(-1). Of 117 tested alcoholic beverages, 64 were tested positive with the highest incidence in grape marc spirits and whiskey (100%, mean 252 μg L(-1)), followed by fruit spirits (86%, mean 591 μg/L(-1)), tequila (86%, mean 404 μg L(-1)), Asian spirits (43%, mean 54 μg L(-1)) and wine (9%, mean 0.7 μg L(-1)). Acrolein could not be detected in beer, vodka, absinthe and bottled water. Six of the fruit and grape marc spirits had acrolein levels above the World Health Organization (WHO) provisional tolerable concentration of 1.5 mg L(-1). Copyright © 2014 Elsevier B.V. All rights reserved.

  9. Volatile Compound Profiling by HS-SPME/GC-MS-FID of a Core Olive Cultivar Collection as a Tool for Aroma Improvement of Virgin Olive Oil.

    Science.gov (United States)

    García-Vico, Lourdes; Belaj, Angjelina; Sánchez-Ortiz, Araceli; Martínez-Rivas, José M; Pérez, Ana G; Sanz, Carlos

    2017-01-14

    Virgin olive oil (VOO) is the only food product requiring official sensory analysis to be classified in commercial categories, in which the evaluation of the aroma plays a very important role. The selection of parents, with the aim of obtaining new cultivars with improved oil aroma, is of paramount importance in olive breeding programs. We have assessed the volatile fraction by headspace-solid-phase microextraction/gas chromatography-mass spectrometry-flame ionization detection (HS-SPME/GC-MS-FID) and the deduced aroma properties of VOO from a core set of olive cultivars (Core-36) which possesses most of the genetic diversity found in the World Olive Germplasm Collection (IFAPA Alameda del Obispo) located in Cordoba, Spain. The VOO volatile fractions of Core-36 cultivars display a high level of variability. It is mostly made of compounds produced from polyunsaturated fatty acids through the lipoxygenase pathway, which confirms to be a general characteristic of the olive species ( Olea europaea L.). The main group of volatile compounds in the oils was six straight-chain carbon compounds derived from linolenic acid, some of them being the main contributors to the aroma of the olive oils according to their odor activity values (OAV). The high level of variability found for the volatile fraction of the oils from Core-36 and, therefore, for the aroma odor notes, suggest that this core set may be a very useful tool for the choice of optimal parents in olive breeding programs in order to raise new cultivars with improved VOO aroma.

  10. Characterization of the Key Aroma Compounds in Proso Millet Wine Using Headspace Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Jingke Liu

    2018-02-01

    Full Text Available The volatile compounds in proso millet wine were extracted by headspace solid-phase microextraction (85 μm polyacrylate (PA, 100 μm polydimethylsiloxane (PDMS, 75 μm Carboxen (CAR/PDMS, and 50/30 μm divinylbenzene (DVB/CAR/PDMS fibers, and analyzed using gas chromatography-mass spectrometry; the odor characteristics and intensities were analyzed by the odor activity value (OAV. Different sample preparation factors were used to optimize this method: sample amount, extraction time, extraction temperature, and content of NaCl. A total of 64 volatile compounds were identified from the wine sample, including 14 esters, seven alcohols, five aldehydes, five ketones, 12 benzene derivatives, 12 hydrocarbons, two terpenes, three phenols, two acids, and two heterocycles. Ethyl benzeneacetate, phenylethyl alcohol, and benzaldehyde were the main volatile compounds found in the samples. According to their OAVs, 14 volatile compounds were determined to be odor-active compounds (OAV > 1, and benzaldehyde, benzeneacetaldehyde, 1-methyl-naphthalene, 2-methyl-naphthalene, and biphenyl were the prominent odor-active compounds (OAV > 50, having a high OAV. Principal component analysis (PCA showed the difference of distribution of the 64 volatile compounds and 14 odor-active compounds with four solid-phase microextraction (SPME fibers.

  11. Use of headspace solid-phase microextraction coupled to liquid chromatography for the analysis of polycyclic aromatic hydrocarbons in tea infusions.

    Science.gov (United States)

    Viñas, Pilar; Campillo, Natalia; Aguinaga, Nerea; Pérez-Cánovas, Eva; Hernández-Córdoba, Manuel

    2007-09-14

    A sensitive and solvent-free procedure for the determination of 11 polycyclic aromatic hydrocarbons in tea infusions using headspace solid-phase microextraction coupled to liquid chromatography with fluorimetric detection is described. A medium polarity polydimethylsiloxane-divinylbenzene 60 microm fiber was found to be suitable for extraction at 90 degrees C and with an extraction time of 60 min under continuous stirring. Desorption was carried out using the static mode for 5 min. Under the optimized conditions, when 1.75 g of tea sample were extracted with boiling water, the precision ranged from 4 to 16% (RSD) and detection limits were between 4 and 145 ngL(-1), depending on the compound. The reliability of the procedure was corroborated by means of GC-MS. The results obtained for a standard reference material were within the range indicated by the supplier.

  12. Traceability of Satsuma Mandarin (Citrus unshiu Marc.) Honey through Nectar/Honey-Sac/Honey Pathways of the Headspace, Volatiles, and Semi-Volatiles: Chemical Markers.

    Science.gov (United States)

    Jerković, Igor; Prđun, Saša; Marijanović, Zvonimir; Zekić, Marina; Bubalo, Dragan; Svečnjak, Lidija; Tuberoso, Carlo I G

    2016-09-29

    Headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE), followed by GC-MS/FID, were applied for monitoring the nectar (NE)/honey-sac (HoS)/honey (HO) pathways of the headspace, volatiles, and semi-volatiles. The major NE (4 varieties of Citrus unshiu ) headspace compounds were linalool, α-terpineol, 1 H -indole, methyl anthranilate, and phenylacetonitrile. Corresponding extracts contained, among others, 1 H -indole, methyl anthranilate, 1,3-dihydro-2 H -indol-2-one and caffeine. The major HoS headspace compounds were linalool, α-terpineol, 1,8-cineole, 1 H -indole, methyl anthranilate, and cis -jasmone. Characteristic compounds from HoS extract were caffeine, 1 H -indole, 1,3-dihydro-2 H -indol-2-one, methyl anthranilate, and phenylacetonitrile. However, HO headspace composition was significantly different in comparison to NE and HoS with respect to phenylacetaldehyde and linalool derivatives abundance that appeared as the consequence of the hive conditions and the bee enzyme activity. C. unshiu honey traceability is determined by chemical markers: phenylacetaldehyde, phenylacetonitrile, linalool and its derivatives, as well as 1 H -indole, 1,3-dihydro-2 H -indol-2-one, and caffeine.

  13. Traceability of Satsuma Mandarin (Citrus unshiu Marc. Honey through Nectar/Honey-Sac/Honey Pathways of the Headspace, Volatiles, and Semi-Volatiles: Chemical Markers

    Directory of Open Access Journals (Sweden)

    Igor Jerković

    2016-09-01

    Full Text Available Headspace solid-phase microextraction (HS-SPME and ultrasonic solvent extraction (USE, followed by GC-MS/FID, were applied for monitoring the nectar (NE/honey-sac (HoS/honey (HO pathways of the headspace, volatiles, and semi-volatiles. The major NE (4 varieties of Citrus unshiu headspace compounds were linalool, α-terpineol, 1H-indole, methyl anthranilate, and phenylacetonitrile. Corresponding extracts contained, among others, 1H-indole, methyl anthranilate, 1,3-dihydro-2H-indol-2-one and caffeine. The major HoS headspace compounds were linalool, α-terpineol, 1,8-cineole, 1H-indole, methyl anthranilate, and cis-jasmone. Characteristic compounds from HoS extract were caffeine, 1H-indole, 1,3-dihydro-2H-indol-2-one, methyl anthranilate, and phenylacetonitrile. However, HO headspace composition was significantly different in comparison to NE and HoS with respect to phenylacetaldehyde and linalool derivatives abundance that appeared as the consequence of the hive conditions and the bee enzyme activity. C. unshiu honey traceability is determined by chemical markers: phenylacetaldehyde, phenylacetonitrile, linalool and its derivatives, as well as 1H-indole, 1,3-dihydro-2H-indol-2-one, and caffeine.

  14. Screening of volatile composition of Lavandula hybrida Reverchon II honey using headspace solid-phase microextraction and ultrasonic solvent extraction.

    Science.gov (United States)

    Jerković, Igor; Marijanović, Zvonimir

    2009-03-01

    The volatiles of unifloral Lavandula hybrida Reverchon II honey were isolated by means of headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE) and analyzed by gas chromatography and mass spectrometry (GC, GC/MS). A total of 23 compounds were identified in the headspace with hexan-1-ol, hexanal, acetic acid, hotrienol, and 2-phenylacetaldehyde as the principal components. Three solvents of different polarity were used for USE, and a total of 53 compounds were identified. The extracts with pentane/Et(2)O 1 : 2 (v/v) were the most representative for USE method containing the majority of the honey floral origin compounds and potential biomarkers (hexanol, acetic acid, butane-1,3-diol, butane-2,3-diol, benzoic acid, coumarin, and 2-phenylacetic acid). The total number of identified compounds (USE and HS-SPME) was 59. In general, the comparison with volatiles of other lavandin honeys of different geographic origins indicated several similarities, while acetic and formic acids were identified with high percentages in L. hybrida Reverchon II honey.

  15. Sampling atmospheric pesticides with SPME: Laboratory developments and field study

    Energy Technology Data Exchange (ETDEWEB)

    Wang Junxia [EPCA-Institut des Sciences Moleculaires, UMR 5255 CNRS-Universite Bordeaux 1, ISM, Site universitaire, 24019 Perigueux Cedex (France); Tuduri, Ludovic [EPCA-Institut des Sciences Moleculaires, UMR 5255 CNRS-Universite Bordeaux 1, ISM, Site universitaire, 24019 Perigueux Cedex (France)], E-mail: l.tuduri@ism.u-bordeaux1.fr; Mercury, Maud [EPCA-Institut des Sciences Moleculaires, UMR 5255 CNRS-Universite Bordeaux 1, ISM, Site universitaire, 24019 Perigueux Cedex (France); Universites d' Aix-Marseille I, II et III-CNRS UMR 6264: Laboratoire Chimie Provence, Equipe Instrumentation et Reactivite Atmospherique (IRA), Universite de Provence Centre de Saint Jerome, Avenue Escadrille Normandie Niemen, 13397 Marseille Cedex 20 (France); Millet, Maurice [Centre de Geochimie de la Surface UMR 7517 CNRS-Universite Louis Pasteur (ULP), LPCA, 1 rue Blessig, 67084 Strasbourg Cedex (France); Briand, Olivier [AFSSET, 253 avenue du General Leclerc, 94701 Maisons-Alfort Cedex (France); Montury, Michel [EPCA-Institut des Sciences Moleculaires, UMR 5255 CNRS-Universite Bordeaux 1, ISM, Site universitaire, 24019 Perigueux Cedex (France)

    2009-02-15

    To estimate the atmospheric exposure of the greenhouse workers to pesticides, solid phase microextraction (SPME) was used under non-equilibrium conditions. Using Fick's law of diffusion, the concentrations of pesticides in the greenhouse can be calculated using pre-determined sampling rates (SRs). Thus the sampling rates (SRs) of two modes of SPME in the lab and in the field were determined and compared. The SRs for six pesticides in the lab were 20.4-48.3 mL min{sup -1} for the exposed fiber and 0.166-0.929 mL min{sup -1} for the retracted fiber. In field sampling, two pesticides, dichlorvos and cyprodinil were detected with exposed SPME. SR with exposed SPME for dichlorvos in the field (32.4 mL min{sup -1}) was consistent with that in the lab (34.5 mL min{sup -1}). SR for dichlorvos in the field (32.4 mL min{sup -1}) was consistent with that in the lab (34.5 mL min{sup -1}). The trends of temporal concentration and the inhalation exposure were also obtained. - SPME was proved to be a powerful and simple tool for determining pesticides' atmospheric concentration.

  16. Sampling atmospheric pesticides with SPME: Laboratory developments and field study

    International Nuclear Information System (INIS)

    Wang Junxia; Tuduri, Ludovic; Mercury, Maud; Millet, Maurice; Briand, Olivier; Montury, Michel

    2009-01-01

    To estimate the atmospheric exposure of the greenhouse workers to pesticides, solid phase microextraction (SPME) was used under non-equilibrium conditions. Using Fick's law of diffusion, the concentrations of pesticides in the greenhouse can be calculated using pre-determined sampling rates (SRs). Thus the sampling rates (SRs) of two modes of SPME in the lab and in the field were determined and compared. The SRs for six pesticides in the lab were 20.4-48.3 mL min -1 for the exposed fiber and 0.166-0.929 mL min -1 for the retracted fiber. In field sampling, two pesticides, dichlorvos and cyprodinil were detected with exposed SPME. SR with exposed SPME for dichlorvos in the field (32.4 mL min -1 ) was consistent with that in the lab (34.5 mL min -1 ). SR for dichlorvos in the field (32.4 mL min -1 ) was consistent with that in the lab (34.5 mL min -1 ). The trends of temporal concentration and the inhalation exposure were also obtained. - SPME was proved to be a powerful and simple tool for determining pesticides' atmospheric concentration

  17. Tank 241-C-103 headspace flammability

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1994-01-01

    Information regarding flammable vapors, gases, and aerosols is presented for the purpose of resolving the tank 241-C-103 headspace flammability issue. Analyses of recent vapor and liquid samples, as well as visual inspections of the tank headspace, are discussed in the context of tank dynamics. This document is restricted to issues regarding the flammability of gases, vapors, and an aerosol that may exist in the headspace of tank 241-C-103. While discussing certain information about the organic liquid present in tank 241-C-103, this document addresses neither the potential for, nor consequences of, a pool fire involving this organic liquid; they will be discussed in a separate report

  18. Tank 241-C-103 headspace flammability

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, J.L.

    1994-01-01

    Information regarding flammable vapors, gases, and aerosols is presented for the purpose of resolving the tank 241-C-103 headspace flammability issue. Analyses of recent vapor and liquid samples, as well as visual inspections of the tank headspace, are discussed in the context of tank dynamics. This document is restricted to issues regarding the flammability of gases, vapors, and an aerosol that may exist in the headspace of tank 241-C-103. While discussing certain information about the organic liquid present in tank 241-C-103, this document addresses neither the potential for, nor consequences of, a pool fire involving this organic liquid; they will be discussed in a separate report.

  19. Recent Developments and Applications of Solid Phase Microextraction (SPME in Food and Environmental Analysis—A Review

    Directory of Open Access Journals (Sweden)

    Sybille Merkle

    2015-06-01

    Full Text Available Solid-phase microextraction (SPME is a simple, sensitive, rapid and solvent-free technique for the extraction of analytes from gaseous, liquid and solid samples and takes a leading position among microextraction methods. Application of SPME in sample preparation has been increasing continuously over the last decade. It is most often used as an automatized fiber injection system coupled to chromatographic separation modules for the extraction of volatile and semivolatile organic compounds and also allows for the trace analysis of compounds in complex matrices. Since SPME was first introduced in the early 1990s, several modifications have been made to adapt the procedure to specific application requirements. More robust fiber assemblies and coatings with higher extraction efficiencies, selectivity and stability have been commercialized. Automation and on-line coupling to analytical instruments have been achieved in many applications and new derivatization strategies as well as improved calibration procedures have been developed to overcome existing limitations regarding quantitation. Furthermore, devices using tubes, needles or tips for extraction instead of a fiber have been designed. In the field of food analysis, SPME has been most often applied to fruit/vegetables, fats/oils, wine, meat products, dairy and beverages whereas environmental applications focus on the analysis of air, water, soil and sediment samples.

  20. Monitoring biogenic volatile compounds emitted by Eucalyptus citriodora using SPME.

    Science.gov (United States)

    Zini, C A; Augusto, F; Christensen, T E; Smith, B P; Caramão, E B; Pawliszy, J

    2001-10-01

    A procedure to monitor BVOC emitted by living plants using SPME technique is presented. For this purpose, a glass sampling chamber was designed. This device was employed for the characterization of biogenic volatile compounds emitted by leaves of Eucalyptus citriodora. After extraction with SPME fibers coated with PDMS/ DVB, it was possible to identify or detect 33 compounds emitted by this plant. A semiquantitative approach was applied to monitor the behavior of the emitted BVOC during 9 days. Circadian profiles of the variation in the concentration of isoprene were plotted. Using diffusion-based SPME quantitation, a recently introduced analytical approach, with extraction times as short as 15 s, it was possible to quantify subparts-per-billion amounts of isoprene emitted by this plant.

  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. Copyright © 2012 Elsevier Ltd. All rights reserved.

  2. Analysis of neutral volatile aroma components in Tilsit cheese using a combination of dynamic headspace technique, capillary gas chromatography and mass spectrometry

    International Nuclear Information System (INIS)

    Dillinger, K.H.

    2000-03-01

    Tilsit cheese is made by the influence of lab ferment and starter cultures on milk. The ripening is done by repeated inoculation of the surface of the Tilsit cheese with yeasts and read smear cultures. This surface flora forms the typical aroma of the Tilsit cheese during the ripening process. The aim of the work was to receive general knowledge about the kind and amount of the neutral volatile aroma components of Tilsit cheese. Beyond this the ability of forming aroma components by read smear cultures and the dispersion of these components in cheese was to be examined. The results were intended to evaluate the formation of aroma components in Tilsit cheese. The semi-quantitative analyses of the aroma components of all samples were done by combining dynamic headspace extraction, gas chromatography and mass spectrometry. In this process the neutral volatile aroma components were extracted by dynamic headspace technique, adsorbed on a trap, thermally desorbed, separated by gas chromatography, detected and identified by mass spectrometry. 63 components belonging to the chemical classes of esters, ketones, aldehydes, alcohols and sulfur containing substances as well as aromatic hydrocarbons, chlorinated hydrocarbons and hydrocarbons were found in the analysed cheese samples of different Austrian Tilsit manufacturing plants. All cheese samples showed a qualitative equal but quantitative varied spectrum of aroma components. The cultivation of pure cultures on a cheese agar medium showed all analysed aroma components to be involved in the biochemical metabolism of these cultures. The ability to produce aroma components greatly differed between the strains and it was not possible to correlate this ability with the taxonomic classification of the strains. The majority of the components had a non-homogeneous concentration profile in the cheese body. This was explained by effects of diffusion and temporal and spatial different forming of components by the metabolism of the

  3. Lichenysin, a cyclooctapeptide occurring in Chinese liquor jiannanchun reduced the headspace concentration of phenolic off-flavors via hydrogen-bond interactions.

    Science.gov (United States)

    Zhang, Rong; Wu, Qun; Xu, Yan

    2014-08-20

    Nonvolatile compounds play important roles in the quality of alcoholic beverages. In our previous work, a type of cyclooctapeptide lichenysin was newly identified in Chinese strong-aroma type liquor. In this work, it was found that lichenysin could selectively affect aroma volatility in strong-aroma type (Jiannanchun) liquor. Interaction of lichenysin and volatile phenolic compounds (off-odors in strong-aroma type liquor) was characterized using headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry (HS-SPME-GC-MS). HS-SPME results indicated that lichenysin very efficiently suppressed the volatility of phenolic compounds by 36-48% (P flavor and nonvolatile matrix components in Chinese liquors.

  4. Differences in microbial metabolites in urine headspace of subjects with Immune Thrombocytopenia (ITP) detected by volatile organic compound (VOC) analysis and metabolomics.

    Science.gov (United States)

    Batty, Claire A; Cauchi, Michael; Hunter, J O; Woolner, Jenny; Baglin, Trevor; Turner, Claire

    2016-10-01

    ITP is an organ-specific autoimmune disorder characterised by a low platelet count whose cause is uncertain. A possible factor is food intolerance, although much of the information linking this with ITP is anecdotal. The role of food intolerance in ITP was studied by replacing a normal diet with an elemental diet (E028), but this did not increase platelet counts. Clear differences, however, were apparent between the volatile organic compounds (VOCs) in the urine headspace of patients with ITP and those present in healthy volunteers, which leads to speculation that abnormal metabolic activity of the intestinal microbiome may be a factor causing ITP. However, further work is needed to confirm this. There were also differences between the VOCs of patients on a normal diet and those on the elemental diet, and in this case, the VOCs involved are very likely to be of bacterial origin, as their production is affected by dietary manipulation. Many of these VOCs are known to be toxic. Copyright © 2016. Published by Elsevier B.V.

  5. The application of headspace gas chromatography coupled to tandem quadrupole mass spectrometry for the analysis of furan in baby food samples.

    Science.gov (United States)

    Pugajeva, Iveta; Rozentale, Irina; Viksna, Arturs; Bartkiene, Elena; Bartkevics, Vadims

    2016-12-01

    Selective methodology employing a tandem quadrupole mass spectrometer coupled to a gas chromatograph with headspace autosampler (HS-GC-MS/MS) was elaborated in this study. Application of the elaborated procedure resulted in a limit of detection of 0.021μgkg(-1) and a limit of quantification of 0.071μgkg(-1). The mean recoveries during in-house validation ranged from 89% to 109%, and coefficients of variation for repeatability ranged from 4% to 11%. The proposed analytical method was applied for monitoring the furan content of 30 commercial baby food samples available on the Latvian retail market. The level of furan found in these samples varied from 0.45 to 81.9μgkg(-1), indicating that infants whose sole diet comprises baby food sold in jars and cans are exposed constantly to furan. Samples containing vegetables and meat had higher levels of furan than those containing only fruits. Copyright © 2016 Elsevier Ltd. All rights reserved.

  6. Analysis of the essential oils from Calendula officinalis growing in Brazil using three different extraction procedures Análise por CG-EM do óleo essencial de Calendula officinalis cultivado no Brasil utilizando-se três diferentes processos de extração

    Directory of Open Access Journals (Sweden)

    Zilda Cristina Gazim

    2008-09-01

    Full Text Available Terpenes and aroma volatiles from flowers of Calendula officinalis cultivated in southeastern Brazil were obtained by steam distillation (SD, headspace-cold finger (HS-CF extraction and headspace solid-phase microextraction (HS-SPME coupled with gas chromatography and mass spectrometric analysis. The dried flowers contained 0.1% oil. Kovats indices and mass spectra were used to identify 27 individual components in the various volatile fractions. The main components present in the volatile fractions of the C. officinalis flowers, obtained by SD, HS-SPME, and HS-CF, were δ-cadinene (22.5, 22.1, and 18.4 % and γ-cadinene (8.9, 25.4, and 24.9 % while 20.4 % of α-cadinol was seen only after SD extraction.Terpenos e aromas voláteis das flores de Calendula officinalis cultivados no sudoeste do Brasil foram isolados por arraste a vapor (SD, dedo frio (HS-CF e micro extração em fase sólida (HS-SPME acoplada à espectrometria de massas. As flores secas da C. officinalis contêm 0,1% de óleo essencial e foram identificadas 27 substâncias químicas através do cálculo do índice de Kováts e interpretação dos espectros de massas. As substâncias majoritárias presentes no óleo essencial das flores de C. officinalis, obtido por SD, HS-SPME e HS-CF foram δ-cadinene (22,5; 22,1 e 18,4 % γ-cadinene (8,9, 25,4 e 24,9 % e 20.4 % de α-cadinol foi observado apenas na extração por arraste a vapor.

  7. Analysis of Odorants in Marking Fluid of Siberian Tiger (Panthera tigris altaica) Using Simultaneous Sensory and Chemical Analysis with Headspace Solid-Phase Microextraction and Multidimensional Gas Chromatography-Mass Spectrometry-Olfactometry

    OpenAIRE

    Simone B. Soso; Jacek A. Koziel

    2016-01-01

    Scent-marking is the most effective method of communication in the presence or absence of a signaler. These complex mixtures result in a multifaceted interaction triggered by the sense of smell. The objective was to identify volatile organic compound (VOC) composition and odors emitted by total marking fluid (MF) associated with Siberian tigers (Panthera tigris altaica). Siberian tiger, an endangered species, was chosen because its MF had never been analyzed. Solid phase microextraction (SPME...

  8. Coupling of SPME with MCC/UV-IMS as a tool for rapid on-site detection of groundwater and surface water contamination

    Energy Technology Data Exchange (ETDEWEB)

    Walendzik, G.; Baumbach, J.I.; Klockow, D. [ISAS-Institute for Analytical Sciences, Dortmund (Germany)

    2005-08-01

    The combination of headspace solid phase microextraction (HS-SPME) [1] with fast chromatographic pre-separation by means of multi-capillary columns (MCC) coupled to an ion mobility spectrometer equipped with a 10.6 eV photoionisation source was applied to rapid on-site monitoring of ground and surface water contaminations. Under field conditions, water contaminants were directly detectable down to the upper {mu}g/L range. The potential of the developed method is illustrated by measurements of BTEX, naphthalene, chlorinated alkenes and chlorinated benzenes in water. Practical results from investigations of contaminated groundwater at a former gasworks site and groundwater from the site of a metal processing plant, focusing on the key substances benzene, naphthalene and tetrachloroethene, demonstrate the feasibility of the system for field studies. (orig.)

  9. Headspace-gas chromatography: an ideal technique for sampling volatiles present in non-volatile matrices.

    Science.gov (United States)

    Ettre, L S

    2001-01-01

    After a brief overview of the techniques of static and dynamic headspace sampling and examples are given for the dynamic method ("purge and trap"). With respect to static headspace-gas chromatography (HS-GC) the theoretical background of the technique and the principles of the existing instruments are outlined. Five questions related to static HS-GC are discussed in more detail: trace analysis; ultratrace analysis with cryogenic enhancement of the analytes and elimination of the possible effect of excess water vapor in the sample; sample modification by carrying out reactions in the sample vial; non-equilibrium static HS-GC; and pattern analysis by HS-GC.

  10. Headspace solid-phase microextraction-gas chromatographic-time-of-flight mass spectrometric methodology for geographical origin verification of coffee

    International Nuclear Information System (INIS)

    Risticevic, Sanja; Carasek, Eduardo; Pawliszyn, Janusz

    2008-01-01

    Increasing consumer awareness of food safety issues requires the development of highly sophisticated techniques for the authentication of food commodities. The food products targeted for falsification are either products of high commercial value or those produced in large quantities. For this reason, the present investigation is directed towards the characterization of coffee samples according to the geographical origin. The conducted research involves the development of a rapid headspace solid-phase microextraction (HS-SPME)-gas chromatography-time-of-flight mass spectrometry (GC-TOFMS) method that is utilized for the verification of geographical origin traceability of coffee samples. As opposed to the utilization of traditional univariate optimization methods, the current study employs the application of multivariate experimental designs to the optimization of extraction-influencing parameters. Hence, the two-level full factorial first-order design aided in the identification of two influential variables: extraction time and sample temperature. The optimum set of conditions for the two variables was 12 min and 55 deg. C, respectively, as directed by utilization of Doehlert matrix and response surface methodology. The high-throughput automated SPME procedure was completed by implementing a single divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) 50/30 μm metal fiber with excellent durability properties ensuring the completion of overall sequence of coffee samples. The utilization of high-speed TOFMS instrument ensured the completion of one GC-MS run of a complex coffee sample in 7.9 min and the complete list of benefits provided by ChromaTOF software including fully automated background subtraction, baseline correction, peak find and mass spectral deconvolution algorithms was exploited during the data evaluation procedure. The combination of the retention index (RI) system using C 8 -C 40 alkanes and the mass spectral library search was utilized for the

  11. Comparison of headspace techniques for sampling volatile natural products in a dynamic system.

    Science.gov (United States)

    Fäldt, J; Eriksson, M; Valterová, I; Borg-Karlson, A K

    2000-01-01

    Commonly used dynamic sorption techniques for collecting biologically active volatile compounds have been compared. Solid phase microextraction (SPME) using two types of fibers (polydimethylsiloxane, PDMS, 100 microm, and carbowax/divinylbenzene, CW/DVB, 65 microm) was compared to purge and trap methods (Porapak Q, Tenax TA and charcoal) and a technique based on absorption in methanol in a cooling bath. Sampling was done in a stream of purified air (20 ml/min) in a closed and temperature-regulated (27 degrees C) glass tube, passing over a capillary tube containing a hexane solution of tridecane, heptadecane, 1-octen-3-ol, 1-hexadecanol, ethyl tetradecanoate, alpha-pinene, linalool, terpinen-4-ol, cis-verbenol, verbenone, beta-caryophyllene, E,E-farnesol, and geranylgeraniol. With all of the methods, the sampling was performed for a period of 30 min before extraction and analysis was done on a GC-FID system. In general, SPME gave a higher response for all compounds except for alpha-pinene, which was only extracted by the CW/DVB fiber. Purge and trap methods and methanol absorption gave the same response for all substances extracted. None of the methods extracted hexadecanol and geranylgeraniol under the conditions used. However, the SPME equipped with the PDMS coating extracted heptadecane, E,E-farnesol and ethyl tetradecanoate. Our results show that SPME, when selecting the fibers to fit the polarity and volatility of the compounds, is an outstanding extraction method compared to purge and trap and methanol absorption, especially for a qualitative analysis. The best conditions for storing fibers exposed to compounds of high volatility were at low temperatures (6 degrees C) in sealed vials, while the worst way was to leave the exposed fiber unprotected at room temperature (22 degrees C). The dynamic sampling system was effectively tested on a fruiting body of a polypore fungus (Ganoderma applanatum) emitting 1-octen-3-ol, and again SPME showed to be the most

  12. Vanguard/rearguard strategy for the evaluation of the degradation of yoghurt samples based on the direct analysis of the volatiles profile through headspace-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Carrillo-Carrión, C; Cárdenas, S; Valcárcel, M

    2007-02-02

    A vanguard/rearguard analytical strategy for the monitoring of the degradation of yoghurt samples is proposed. The method is based on the headspace-gas chromatography-mass spectrometry (HS-GC-MS) instrumental coupling. In this combination, the chromatographic column is firstly used as an interface between the HS and the MS (vanguard mode) avoiding separation of the volatile components by maintaining the chromatographic oven at high, constant temperature. By changing the thermal conditions of the oven, the aldehydes can be properly separated for individual identification/quantification (rearguard mode). In the vanguard method, the quantification of the volatile aldehydes was calculated through partial least square and given as a total index. The rearguard method permits the detection of the aldehydes at concentrations between 12 and 35 ng/g. Both methods were applied to the study of the environmental factors favouring the presence of the volatile aldehydes (C(5)-C(9)) in the yoghurt samples. Principal component analysis of the total concentration of aldehydes with the time (from 0 to 30 days) demonstrates the capability of the HS-MS coupling for the estimation of the quality losses of the samples. The results were corroborated by the HS-GC-MS which also indicates that pentanal was present in the yoghurt from the beginning of the study and the combination of light/oxygen was the most negative influence for sample conservation.

  13. Headspace solid-phase microextraction and gas chromatographic analysis of low-molecular-weight sulfur volatiles with pulsed flame photometric detection and quantification by a stable isotope dilution assay.

    Science.gov (United States)

    Ullrich, Sebastian; Neef, Sylvia K; Schmarr, Hans-Georg

    2018-02-01

    Low-molecular-weight volatile sulfur compounds such as thiols, sulfides, disulfides as well as thioacetates cause a sulfidic off-flavor in wines even at low concentration levels. The proposed analytical method for quantification of these compounds in wine is based on headspace solid-phase microextraction, followed by gas chromatographic analysis with sulfur-specific detection using a pulsed flame photometric detector. Robust quantification was achieved via a stable isotope dilution assay using commercial and synthesized deuterated isotopic standards. The necessary chromatographic separation of analytes and isotopic standards benefits from the inverse isotope effect realized on an apolar polydimethylsiloxane stationary phase of increased film thickness. Interferences with sulfur-specific detection in wine caused by sulfur dioxide were minimized by addition of propanal. The method provides adequate validation data, with good repeatability and limits of detection and quantification. It suits the requirements of wine quality management, allowing the control of oenological treatments to counteract an eventual formation of excessively high concentration of such malodorous compounds. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. 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.

  15. Comparison of different extraction methods: steam distillation, simultaneous distillation and extraction and headspace co-distillation, used for the analysis of the volatile components in aged flue-cured tobacco leaves.

    Science.gov (United States)

    Peng, Fumin; Sheng, Liangquan; Liu, Baizhan; Tong, Hongwu; Liu, Shaomin

    2004-06-18

    Steam distillation (SD), simultaneous distillation and extraction (SDE) and headspace co-distillation (HCD) were compared here for their effectiveness in the extraction of volatile compounds from tobacco. The different grades of aged flue-cured tobacco leaves extracted by the three methods respectively were analyzed using GC-MS. Mass spectra or authentic compounds were used to identify around 408 components in various volatile fractions. On the one hand, the qualitative comparison showed that more compounds were detected in HCD extract (391 components) than in SDE extract (377 components), and the approximately quantitative analysis showed that the total amount of volatile components in SDE extract (445.48 microg/g) was much more than that in HCD extract (315.72 microg/g). But on the other hand, HCD was the most efficient for nearly all the highly volatile compounds among the three methods. As to low-volatile compounds such as lactones, long chain aldehydes, ketones, alcohols, and esters, more was detected in SDE extract than in HCD extract. The SD method (322 components, total amount 228.42 microg/g) was the lowest sensitive to all compounds except semi-volatile fatty acids among the three methods.

  16. Determination of some volatile compounds in alcoholic beverage by headspace solid-phase microextraction gas chromatography - mass spectrometry

    Science.gov (United States)

    Schmutzer, G.; Avram, V.; Feher, I.; David, L.; Moldovan, Z.

    2012-02-01

    The volatile composition of alcoholic beverage was studied by headspace solid-phase microextraction (HSSPME) method and gas chromatography - mass spectrometry (GC-MS). Some volatile compounds, such as alcohols, esters, terpenes and other are mainly responsible for the flavor of fortified wines and their amounts specify the quality of the alcoholic beverages. From this perspective it is interesting to develop a rapid, selective and sensitive analytical method suitable for simultaneous quantification of the main molecules being responsible for the organoleptic characteristic of alcoholic beverages. Vermouth fortified drink was analyzed in order to characterize the volatile profile. Using the HS-SPME/GC-MS a number of twenty-six volatile compounds from a commercial market alcoholic beverage were identified. The most abundant compounds were m-thymol, o-thymol and eugenol, alongside of the ethyl ester compounds.

  17. Determination of residual volatile organic compounds migrated from polystyrene food packaging into food simulant by headspace solid phase micro extraction-gas chromatography

    International Nuclear Information System (INIS)

    Mohd Marsin Sanagi; Ling, Susie Lu; Zalilah Nasir; Wan Aini Wan Ibrahim; Abu Naim, Ahmedy

    2008-01-01

    The residual styrene and other volatile organic compounds (VOCs) present in the polystyrene food packaging are of concern as these compounds have the potential to migrate into the food in contact. This work describes a method for quantitative determination of VOCs, namely styrene, toluene, ethyl benzene, iso-propylbenzene and n-propylbenzene that have migrated from polystyrene food packaging into food stimulant by gas chromatography-flame ionization detection (GC-FID). Headspace solid phase micro extraction (HS-SPME) technique was applied for migration test using water as food stimulant. The effects of extraction variables including sample volume, eluotropic strength, extraction temperature, extraction time, desorption time, sample agitation, and salt addition on the amounts of the extracted analyses were studied to obtain the optimal HS-SPME conditions. The optimized method was applied to test the VOCs migrated from polystyrene bowls and cups at storage temperatures ranging from 24 to 80 degree Celsius for 30 min. Styrene and ethyl benzene were found to migrate from the samples into the food stimulant. The migration of analyze was found to be strongly dependent upon the storage temperature. The HS-SPME is useful as an alternative method to determine the migration of VOCs from food packaging material into food stimulant. (author)

  18. First results on headspace-solid phase microextraction-gas chromatography/mass spectrometry of volatile organic compounds emitted by wax objects in museums.

    Science.gov (United States)

    Lattuati-Derieux, A; Thao, S; Langlois, J; Regert, M

    2008-04-11

    Sampling volatile organic compounds (VOCs) emitted by a large variety of materials is nowadays a very useful technique for analytical purpose. In the field of cultural heritage, it can be applied to identify some constituents of museum artefacts off-gassing VOCs without sampling on the object itself. In this study, we focused on objects made of wax. First volatiles emitted by a reference beeswax were trapped and identified by headspace-solid phase microextraction (HS-SPME)-gas chromatography and mass spectrometry (GC/MS). This allowed to identify numerous volatile biomarkers, namely saturated n-alkanes from C(10) to C(21), saturated n-carboxylic acids containing 6-12 carbon atoms, benzene and cinnamic derivatives that may be considered as volatile biomarkers of beeswax. The SPME strategy was then performed at the Orsay museum (Paris) in a showcase containing a wax sculpture "Le Mineur de la Loire" by J.-J. Carriès. The use of beeswax in this sculpture was unequivocally confirmed by the VOCs concentrated in the showcase, together with a set of characteristic molecular compounds identified by HT-GC/MS. HS-SPME-GC/MS thus appears to be a powerful in situ and non-invasive analytical technique that allows to identify natural substances in the field of cultural heritage without any sampling of solid matter from the object. The results obtained are promising for orientating the strategy of preventive conservation related to works of art characterised by important emission of VOCs.

  19. Chromatographic methods for analysis of triazine herbicides.

    Science.gov (United States)

    Abbas, Hana Hassan; Elbashir, Abdalla A; Aboul-Enein, Hassan Y

    2015-01-01

    Gas chromatography (GC) and high-performance liquid chromatography (HPLC) coupled to different detectors, and in combination with different sample extraction methods, are most widely used for analysis of triazine herbicides in different environmental samples. Nowadays, many variations and modifications of extraction and sample preparation methods such as solid-phase microextraction (SPME), hollow fiber-liquid phase microextraction (HF-LPME), stir bar sportive extraction (SBSE), headspace-solid phase microextraction (HS-SPME), dispersive liquid-liquid microextraction (DLLME), dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO), ultrasound-assisted emulsification microextraction (USAEME), and others have been introduced and developed to obtain sensitive and accurate methods for the analysis of these hazardous compounds. In this review, several analytical properties such as linearity, sensitivity, repeatability, and accuracy for each developed method are discussed, and excellent results were obtained for the most of developed methods combined with GC and HPLC techniques for the analysis of triazine herbicides. This review gives an overview of recent publications of the application of GC and HPLC for analysis of triazine herbicides residues in various samples.

  20. Tank 24-C-103 headspace flammability

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1994-05-01

    Information regarding flammable vapors, gases, and aerosols is presented and interpreted to help resolve the tank 241-C-103 headspace flammability issue. Analyses of recent vapor and liquid samples, as well as visual inspections of the tank headspace, are discussed in the context of tank dynamics. Concern that the headspace of tank 241-C-103 may contain a flammable mixture of organic vapors and an aerosol of combustible organic liquid droplets arises from the presence of a layer of organic liquid in the tank. This organic liquid is believed to have originated in the plutonium-uranium extraction (PUREX) process, having been stored initially in tank 241-C-102 and apparently transferred to tank 241-C-103 in 1975 (Carothers 1988). Analyses of samples of the organic liquid collected in 1991 and 1993 indicate that the primary constituents are tributyl phosphate (TBP) and several semivolatile hydrocarbons (Prentice 1991, Pool and Bean 1994). This is consistent with the premise that the organic waste came from the PUREX process, because the PUREX process used a solution of TBP in a diluent composed of the n-C 11 H 24 to n-C 15 H 32 normal paraffinic hydrocarbons (NPH)

  1. Análise qualitativa de compostos voláteis do headspace de carne cozida de ovinos e caprinos

    Directory of Open Access Journals (Sweden)

    Jossiê Zamperetti Donadel

    2013-11-01

    Full Text Available Este estudo teve como objetivo caracterizar qualitativamente os compostos voláteis (CV do headspace de diferentes músculos de carne cozida de ovinos e caprinos da região do Alto Camaquã, Rio Grande do Sul - Brasil. Os CV do headspace dos músculos cozidos, L. dorsi e V. lateralis de cinco ovinos machos (idade de 6 meses e cinco cabritos machos castrados (idade de 8-9 meses foram analisados pela técnica de microextração em fase sólida (HS-SPME e cromatógrafo a gás acoplado a espectrômetro de massas (GC/MS. Foram encontrados 73 compostos voláteis, dentre eles aldeídos, cetonas e compostos sulfurados, característicos de carne processada termicamente. A partir da fração volátil, foi possível encontrar marcadores que discriminassem as espécies animais estudadas, caracterizando os caprinos por apresentarem, entre outros compostos, terpenos (β-pineno, α-gurjuneno, α-muuroleno, ausentes em ovinos. Alguns compostos discriminaram V. lateralis e L. dorsi de ovinos, como álcool isopropílico, α-pineno, o-xileno, porém não foi possível obter uma diferenciação entre os músculos de caprinos.

  2. Changes in psychological distress and psychosocial functioning in young people visiting headspace centres for mental health problems.

    Science.gov (United States)

    Rickwood, Debra J; Mazzer, Kelly R; Telford, Nic R; Parker, Alexandra G; Tanti, Chris J; McGorry, Patrick D

    2015-06-01

    To examine changes in psychological distress and psychosocial functioning in young people presenting to headspace centres across Australia for mental health problems. Analysis of routine data collected from headspace clients who had commenced an episode of care between 1 April 2013 and 31 March 2014, and at 90-day follow-up. A total of 24 034 people aged 12-25 years who had first presented to one of the 55 fully established headspace centres for mental health problems during the data collection period. Main reason for presentation, types of therapeutic services provided, Kessler Psychological Distress Scale (K10) scores, and Social and Occupational Functioning Assessment Scale (SOFAS) scores. Most headspace mental health clients presented with symptoms of depression and anxiety and were likely to receive cognitive behaviour therapy (CBT). Younger males were more likely than other age- and sex-defined groups to present for anger and behavioural problems, while younger females were more likely to present for deliberate self-harm. From presentation to last assessment, over one-third of clients had significant improvements in psychological distress (K10) and a similar proportion in psychosocial functioning (SOFAS). Sixty per cent of clients showed significant improvement on one or both measures. Data regarding outcomes for young people using mental health care services similar to headspace centres are scarce, but the current results compare favourably with those reported overseas, and show positive outcomes for young people using headspace centres.

  3. Selected Ion Flow Tube-MS Analysis of Headspace Vapor from Gastric Content for the Diagnosis of Gastro-Esophageal Cancer

    Czech Academy of Sciences Publication Activity Database

    Kumar, S.; Huang, J.; Cushnir, J. R.; Španěl, Patrik; Smith, D.

    2012-01-01

    Roč. 84, č. 21 (2012), s. 9550-9557 ISSN 0003-2700 Institutional support: RVO:61388955 Keywords : SOLID-PHASE MICROEXTRACTION * TRACE GAS-ANALYSIS * CHROMATOGRAPHY -MASS SPECTROMETRY Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 5.695, year: 2012

  4. 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.

  5. Characterisation of volatile profile and sensory analysis of fresh-cut "Radicchio di Chioggia" stored in air or modified atmosphere.

    Science.gov (United States)

    Cozzolino, Rosaria; Martignetti, Antonella; Pellicano, Mario Paolo; Stocchero, Matteo; Cefola, Maria; Pace, Bernardo; De Giulio, Beatrice

    2016-02-01

    The volatile profile of two hybrids of "Radicchio di Chioggia", Corelli and Botticelli, stored in air or passive modified atmosphere (MAP) during 12 days of cold storage, was monitored by solid phase micro-extraction (SPME) GC-MS. Botticelli samples were also subjected to sensory analysis. Totally, 61 volatile organic compounds (VOCs) were identified in the headspace of radicchio samples. Principal component analysis (PCA) showed that fresh product possessed a metabolic content similar to that of the MAP samples after 5 and 8 days of storage. Projection to latent structures by partial least squares (PLS) regression analysis showed the volatiles content of the samples varied depending only on the packaging conditions. Specifically, 12 metabolites describing the time evolution and explaining the effects of the different storage conditions were highlighted. Finally, a PCA analysis revealed that VOCs profile significantly correlated with sensory attributes. Copyright © 2015 Elsevier Ltd. All rights reserved.

  6. 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

  7. Selective molecularly imprinted polymer combined with restricted access material for in-tube SPME/UHPLC-MS/MS of parabens in breast milk samples

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Israel D.; Melo, Lidervan P. [Departamento de Química, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto, SP (Brazil); Jardim, Isabel C.S.F. [Instituto de Química, Universidade Estadual de Campinas, Campinas, SP (Brazil); Monteiro, Juliana C.S.; Nakano, Ana Marcia S. [Escola de Enfermagem de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto, SP (Brazil); Queiroz, Maria Eugênia C., E-mail: mariaeqn@ffclrp.usp.br [Departamento de Química, Faculdade de Filosofia Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto, SP (Brazil)

    2016-08-17

    A new molecularly imprinted polymer modified with restricted access material (a hydrophilic external layer), (MIP-RAM) was synthesized via polymerization in situ in an open fused silica capillary. This stationary phase was used as sorbent for in-tube solid phase microextraction (in-tube SPME) to determine parabens in breast milk samples by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Scanning electron micrographs (SEM) illustrate MIP surface modification after glycerol dimethacrylate (hydrophilic monomer) incorporation. The interaction between parabens and MIP-RAM was investigated by Fourier-transform infrared (FTIR) spectroscopy. The Scatchard plot for MIP-RAM presented two linear parts with different slopes, illustrating binding sites with high- and low-affinity. Endogenous compounds exclusion from the MIP-RAM capillary was demonstrated by in-tube SPME/LC-UV assays carried out with blank milk samples. The in-tube SPME/UHPLC-MS/MS method presented linear range from 10 ng mL{sup −1} (LLOQ) to 400 ng mL{sup −1} with coefficients of determination higher than 0.99, inter-assay precision with coefficient of variation (CV) values ranging from 2 to 15%, and inter-assay accuracy with relative standard deviation (RSD) values ranging from −1% to 19%. Analytical validation parameters attested that in-tube SPME/UHPLC-MS/MS is an appropriate method to determine parabens in human milk samples to assess human exposure to these compounds. Analysis of breast milk samples from lactating women demonstrated that the proposed method is effective. - Highlights: • Molecularly imprinted polymer modified with a hydrophilic external layer (RAM-MIP) was synthesized in a silica capillary. • RAM-MIP capillary, used as sorbent for in-tube SPME, established specific interaction with parabens present in milk samples. • The matrix components that interacted only with the hydrophilic external layer (non-adsorptive network) were excluded.

  8. 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

  9. Rapid sampling of BTEX in air by SPME in the city of Nice and at the Nice-Cote d'Azur airport; Echantillonnage rapide des BTEX dans l'air par SPME dans la ville de Nice et a l'aeroport Nice-Cote d'Azur

    Energy Technology Data Exchange (ETDEWEB)

    Tumbiolo, S.; Gal, J.F.; Maria, P.Ch. [Nice Univ. Sophia Antipolis, Lab. de Radiochimie, Sciences Analytique et Environnement, Faculte des Sciences, 06 (France); Laborde, P.; Teton, S. [Qualitair, Nice Leader, 06 - Nice (France)

    2006-04-15

    This article presents the results of a tentative application of Solid Phase Micro Extraction (SPME) to the analysis of BTEX (benzene, toluene, ethyl-benzene and xylenes) at the {mu}g/m{sup 3} level in indoor and outdoor air. The salient features of the method validation are reported. Sampling by QUALITAIR using Radiello passive samplers, was carried out from 2001 to 2004 in the city of Nice and its airport. Urban traffic impact was proved, but a link between BTX concentrations and the variations of airport activities was not clearly established. During the same period, several samplings were performed using SPME. Taking into account the short (30 minutes) sampling time, rapid changes of BTEX concentrations were evidenced, as for example the start of airplane engines. As field studies have shown, SPME technique appears as a method of choice for fast qualitative analysis and quantitative determination of Volatile Organic Compounds (VOC). The small dimensions of the SPME sampling system and the short sampling time let envisage its utilisation for the rapid diagnostic and the monitoring of indoor air quality. (author)

  10. Analysis of acrylonitrile, 1,3-butadiene, and related compounds in acrylonitrile-butadiene-styrene copolymers for kitchen utensils and children's toys by headspace gas chromatography/mass spectrometry.

    Science.gov (United States)

    Ohno, Hiroyuki; Kawamura, Yoko

    2010-01-01

    A headspace gas chromatography/mass spectrometry method was developed for the simultaneous determination of the residual levels of acrylonitrile (AN), 1,3-butadiene (1,3-BD), and their related compounds containing propionitrile (PN) and 4-vinyl-1-cyclohexene (4-VC) in acrylonitrile-butadiene-styrene (ABS) copolymers for kitchen utensils and children's toys. A sample was cut into small pieces, then N,N-dimethylacetamide and an internal standard were added in a sealed headspace vial. The vial was incubated for 1 h at 90 degrees C and the headspace gas was analyzed by gas chromatography/mass spectrometry. The recovery rates of the analytes were 93.3-101.8% and the coefficients of variation were 0.3-6.5%. In ABS copolymers, the levels were 0.3-50.4 microg/g for AN, ND-4.5 microg/g for PN, 0.06-1.58 microg/g for 1,3-BD, and 1.1-295 microg/g for 4-VC. The highest level was found for 4-VC, which is a dimer of 1,3-BD, and the next highest was for AN, which is one of the monomers of the ABS copolymer. Furthermore, the method was also applied to acrylonitrile-styrene (AS) copolymers and polystyrenes (PS) for kitchen utensils, and nitrile-butadiene rubber (NBR) gloves. In AS copolymers, AN and PN were detected at 16.8-54.5 and 0.8-6.9 microg/g, respectively. On the other hand, the levels in PS and NBR samples were all low.

  11. gamma. -radiolysis experiments on the decarboxylation of methionine and related compounds. A new method of CO/sub 2/-headspace gas chromatographic analysis as applied to the. gamma. -radiolysis of biologically relevant systems in aqueous solutions which contain sulphur. gamma. -radiolytische Experimente zur Decarboxylierung des Methionins und verwandter Verbindungen. Ein neues Verfahren zur gaschromatographischen quantitativen CO/sub 2/-Headspace-Analyse mit Anwendung auf die. gamma. -Radiolyse einiger schwefelhaltiger - biochemisch relevanter - Verbindungen im waessrigen System

    Energy Technology Data Exchange (ETDEWEB)

    Masloch, B.

    1981-12-04

    The decarboxylation induced by OH radicals of the amino acid methionine containing sulphur in an aquaeous medium is examined by ..gamma..-radiolytic experiments. The following stable end products were found: carbon dioxide, methane, methanthiol, ethylene, ethane, ammonia, methionine sulphoxide and 3 methyl thiopropylamine. A gas chromatography headspace process is developed for the quantitative analysis of the gases, particularly of CO/sub 2/. The ammonia is determined by an NH/sub 3/ electrode sensitive to gas. The methionine sulphoxide was determined in a fast HPLC process, apart from other end products, which all carry the amine acid function. The formation of methionine sulphonate from the reduction of methionine induced by OH radicals can be excluded. The dependence of the radiation chemistry CO/sub 2/ yield (relative to the radiation energy absorbed) of anaerobic methionine solutions and those containing oxygen on the pH value is examined quantitatively. With increasing proton concentrations, the CO/sub 2/ yields below pH 4 decrease greatly. Higher phosphate content also decreases the CO/sub 2/ yields. At pH 4 (N/sub 2/O saturation), the yields grow with the substrate concentration. Model examination by the substrates N-acetyl methionine and 4-methyl thiobatyric acid prove that the amino group is of paramount importance for the decarboxylation induced by OH radicals. No CO/sub 2/ binding occurs in the oxidation of methionine by intermediary Tl/sup 2+/. The 2-amino butyric acid is decarboxylated intermolecularly, if dimethyl sulphide is present during irradiation. S-centred radical ions are formed in the oxidation of the dimethyl sulphide by OH radicals, which trigger the decarboxylation of the Z-amino butyric acid. All the results confirm a primary mechanism for the methionine oxidation induced by OH radicals recently postulated from pulse radiolytic data and permit one to draw a series of more precise pulse radiolytic conclusions.

  12. Comprehensive two-dimensional gas chromatography combined to multivariate data analysis for detection of disease-resistant clones of Eucalyptus.

    Science.gov (United States)

    Hantao, Leandro Wang; Toledo, Bruna Regina; Ribeiro, Fabiana Alves de Lima; Pizetta, Marilia; Pierozzi, Caroline Geraldi; Furtado, Edson Luiz; Augusto, Fabio

    2013-11-15

    In this paper it is reported the use of the chromatographic profiles from volatile fractions of plant clones - in this case, hybrids of Eucalyptus grandis×Eucalyptus urophylla - to determine specimens susceptible to rust disease. The analytes were isolated by headspace solid phase microextraction (HS-SPME) and analyzed by comprehensive two-dimensional gas chromatography combined to fast quadrupole mass spectrometry (GC×GC-qMS). Parallel Factor Analysis (PARAFAC) was employed for estimate the correlation between the chromatographic profiles and resistance against Eucalyptus rust, after preliminary variable selection performed by Fisher ratio analysis. The proposed method allowed the differentiation between susceptible and non-susceptible clones and determination of three resistance biomarkers. This approach can be a valuable alternative for the otherwise time-consuming and labor-intensive methods commonly used. © 2013 Elsevier B.V. All rights reserved.

  13. Evaluation of HS-SPME and ultrasonic solvent extraction for monitoring of plant flavours added by the bees to herbhoneys: traceability biomarkers.

    Science.gov (United States)

    Kuś, Piotr Marek; Marijanović, Zvonimir; Jerković, Igor

    2015-01-01

    The volatile composition of 21 herbhoneys (HHs) of 7 different botanical origins was characterised for the first time. Ultrasound solvent extraction (USE) and headspace solid-phase microextraction (HS-SPME) followed by GC-FID/MS were successfully applied as complementary methods for monitoring the volatile plant flavours added by the bees. HHs showed significant compositional variability related to the botanical origin and compounds that could serve as traceability biomarkers were identified. The most important compounds with high abundance were (E,extract; H, headspace): caffeine (up to 68.7%, E) and trans-linalool oxide (up to 26.0%, H) in coffee HH, α-terpineol (up to 8.2%, E; 27.1%, H) and bornyl acetate (up to 3.1, E; 11.9%, H) in pine HH, thymol (up to 3.1%, E; 55.4%, H) in thyme HH. Hawthorn HH was characterised by the presence of herniarin (up to 13.4%, E) and lemon HH contained limonene (up to 1.6%, E; 33.2%, H). Other HHs (nettle and aloe) contained lower amounts of volatiles and their profiles were not specific. In all the HHs, methyl syringate was found and it was most abundant in thyme HH (up to 17.4%, E). The volatile fraction of HHs showed some substantial similarities and differences with the composition of herbs from which they derive. It confirms the selective bee-mediated transfer of phytochemicals, including known flavour-active volatiles into the final product, but also biotransformation of several compounds. Additionally, several similarities to the corresponding natural honeys were observed, but in general HHs exhibited less rich volatile profiles.

  14. Analysis of honeybush tea (Cyclopia spp.) volatiles by comprehensive two-dimensional gas chromatography using a single-stage thermal modulator.

    Science.gov (United States)

    Ntlhokwe, Gaalebalwe; Tredoux, Andreas G J; Górecki, Tadeusz; Edwards, Matthew; Vestner, Jochen; Muller, Magdalena; Erasmus, Lené; Joubert, Elizabeth; Christel Cronje, J; de Villiers, André

    2017-07-01

    The applicability of comprehensive two-dimensional gas chromatography (GC×GC) using a single-stage thermal modulator was explored for the analysis of honeybush tea (Cyclopia spp.) volatile compounds. Headspace solid phase micro-extraction (HS-SPME) was used in combination with GC×GC separation on a non-polar × polar column set with flame ionisation (FID) detection for the analysis of fermented Cyclopia maculata, Cyclopia subternata and Cyclopia genistoides tea infusions of a single harvest season. Method optimisation entailed evaluation of the effects of several experimental parameters on the performance of the modulator, the choice of columns in both dimensions, as well as the HS-SPME extraction fibre. Eighty-four volatile compounds were identified by co-injection of reference standards. Principal component analysis (PCA) showed clear differentiation between the species based on their volatile profiles. Due to the highly reproducible separations obtained using the single-stage thermal modulator, multivariate data analysis was simplified. The results demonstrate both the complexity of honeybush volatile profiles and the potential of GC×GC separation in combination with suitable data analysis techniques for the investigation of the relationship between sensory properties and volatile composition of these products. The developed method therefore offers a fast and inexpensive methodology for the profiling of honeybush tea volatiles. Graphical abstract Surface plot obtained for the GC×GC-FID analysis of honeybush tea volatiles.

  15. Tank vapor characterization project. Tank 241-TY-103 headspace gas and vapor characterization: Results for homogeneity samples collected on November 22, 1996

    International Nuclear Information System (INIS)

    Olsen, K.B.; Pool, K.H.; Evans, J.C.; Hayes, J.C.

    1997-09-01

    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)

  16. 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.

  17. 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).

  18. Tank vapor characterization project - Tank 241-U-112 headspace gas and vapor characterization: Results for homogeneity samples collected on December 6, 1996

    International Nuclear Information System (INIS)

    Sklarew, D.S.; Pool, K.H.; Evans, J.C.; Hayes, J.C.

    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

  19. Headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry for the determination of haloanisoles in sparkling (cava and cider) and non-sparkling (wine) alcoholic beverages.

    Science.gov (United States)

    Ruiz-Delgado, Ana; Arrebola-Liébanas, Francisco Javier; Romero-González, Roberto; López-Ruiz, Rosalía; Garrido Frenich, Antonia

    2016-10-01

    A highly sensitive analytical method was developed to determine 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and 2,3,4,5,6-pentachloroanisole (PCA) in sparkling alcoholic beverages. The method was based on the use of headspace solid-phase microextraction (HS-SPME) using a polydimethylsiloxane (PDMS) fibre. It was coupled to gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS/MS) for the detection and quantification of the target haloanisoles. The method was fully automated and no sample preparation was needed. The method was validated for alcoholic beverages. The influence of CO 2 on the extraction efficiency was also evaluated for the studied sparkling drinks (cava and cider). All the calibration curves showed good linearity (R 2  > 0.98) within the tested range (1-50 ng l -1 ). Recoveries were evaluated at three different levels (1, 5 and 50 ng l -1 ) and were always between 71% and 119%. Precision was expressed as relative standard deviation (RSD), and was evaluated as intra- and inter-day precisions, with values ≤ 22% in both cases. Limits of quantitation (LOQs) were ≤ 0.91 ng l -1 , which are below the sensory threshold levels for such compounds in humans. The validated method was applied to commercial samples, 10 cavas and 10 ciders, but it was also used for the analysis of nine red wines and four white wines, demonstrating the further applicability of the proposed method to non-sparkling beverages. TCA was detected in most samples at up to 0.45 ng l -1 .

  20. Test plan for headspace gas concentration measurement and headspace ventilation rate measurement for DCRTs 241-A-244, 241-BX-244, 241-S-244, 241-TX-244

    International Nuclear Information System (INIS)

    Bauer, R.E.

    1998-01-01

    This test plan provides the directions to characterize the headspace gas concentrations and the headspace ventilation rate for double contained receiver tanks 241-A-244, 241-BX-244, 241-S-244, and 241-TX-244

  1. Forensic Analysis of Human Autopsy Tissue for the Presence of Polydimethylsiloxane (Silicone) and Volatile Cyclic Siloxanes using Macro FT-IR, FT-IR Spectroscopic Imaging and Headspace GC-MS.

    Science.gov (United States)

    Lanzarotta, Adam; Kelley, Caroline Machal

    2016-05-01

    This study describes effective and straightforward primary and secondary methods for the detection of silicone in human autopsy tissue. The primary method is polydimethylsiloxane (PDMS) specific and employs either macro-attenuated total reflection Fourier transform infrared (ATR-FT-IR) spectroscopy for samples with a high PDMS concentration (relative to that of the matrix) or micro-FT-IR spectroscopic imaging in a reflection/absorption modality for samples with a low PDMS concentration. Although the secondary method is not PDMS specific, it employs headspace gas chromatography with mass spectrometric detection (HS/GC-MS) for the detection of low molecular weight volatile cyclic siloxanes (VCS), which are characteristic marker compounds for PDMS. Overall, the combined results from the primary and secondary analyses provide reliable evidence for the presence of silicone. Published 2016. This article is a U.S. Government work and is in the public domain in the USA.

  2. Partitioning of the pesticide trifluralin between dissolved organic matter and water using automated SPME-GC/MS

    KAUST Repository

    Caupos, Emilie

    2014-10-04

    Solid-phase microextraction (SPME) was used to determine the equilibrium association constant for a pesticide, trifluralin (TFR), with dissolved organic matter (DOM). After optimization of the SPME method for the analysis of TFR, partition coefficients (K DOM) with three different sources of DOM were determined in buffered solutions at pH 7. Commercial humic acids and DOM fractions isolated from two surface waters were used. The values of log K DOMvaried from 4.3 to 5.8, depending on the nature of the organic material. A good correlation was established between log K DOMand DOM properties (as measured with the H/O atomic ratio and UV absorbance), in agreement with literature data. This is consistent with the effect of polarity and aromaticity for governing DOM-pollutant associations, regardless of the origin of DOM. This association phenomenon is relevant to better understand the behavior of pesticides in the environment since it controls part of pesticide leaching and fate in aquatic systems.

  3. Volatile profiles of Italian monovarietal extra virgin olive oils via HS-SPME-GC-MS: newly identified compounds, flavors molecular markers, and terpenic profile.

    Science.gov (United States)

    Cecchi, Teresa; Alfei, Barbara

    2013-12-01

    This study aims to contribute to the knowledge of the commercial, sensory, and analytical characteristics of extra virgin olive oil (EVOO) from Italy (Marche region), renowned since ancient times. Headspace solid-phase micro-extraction (HS-SPME) was applied for the very first time to the sampling of volatile compounds of eleven typical Italian monocultivar EVOOs. Forty-eight compounds were characterised by GC-MS, some of them were only occasionally found in other EVOOs and some other were never detected before in any EVOO. Compounds belonging mainly to alcohols, esters, aldehydes, ketones and hydrocarbons chemical classes characterised the volatile profiles. The main volatile compounds detected in the EVOOs were the C6 compounds derived from polyunsaturated fatty acids, through the lipoxygenase pathway, in different proportion according to the specific cultivar. The results suggest that genetic factors strongly influence volatile formation and terpene hydrocarbons are claimed to be suitable markers of the geographic origin and genotype of the EVOO. Correlations among sensory attributes evaluated by a panel test and the presence of specific volatile compounds were highlighted for the very first time. The significance of the presence of some newly identified volatile compounds was discussed. Copyright © 2013 Elsevier Ltd. All rights reserved.

  4. JV Task 92 - Alcoa/Retec SFE and SPME

    Energy Technology Data Exchange (ETDEWEB)

    Steven Hawthorne

    2009-02-15

    This report summarizes the work performed by the Energy & Environmental Research Center (EERC) under the U.S. Department of Energy Jointly Sponsored Research Program JV Task 92, which is a continuation of JV9. Successful studies performed in 1999 through the end of 2008 demonstrated the potential for using selective supercritical fluid extraction (SFE) and a solid-phase microextraction (SPME) method for measuring sediment pore water polycyclic aromatic hydrocarbons (PAHs) to mimic the bioavailability of PAHs from manufactured gas plant and aluminum smelter soils and sediments both in freshwater and saltwater locations. The studies that the EERC has performed with the commercial partners have continued to generate increased interest in both the regulatory communities and in the industries that have historically produced or utilized coal tar products. Both ASTM International and the U.S. Environmental Protection Agency (EPA) have accepted the pore water method developed at the EERC as standard methods. The studies have demonstrated the effectiveness of our techniques in predicting bioavailability of PAHs from ca. 250 impacted and background field sediments and soils. The field demonstrations from the final years of the project continued to build the foundation data for acceptance of our methods by the regulatory communities. The JV92 studies provide the single largest database in the world that includes measures of PAH bioavailability along with biological end points. These studies clearly demonstrated that present regulatory paradigms based on equilibrium partitioning greatly overpredict bioavailability. These investigations also laid the foundation for present (non-JV) studies being applied to PAHs and polychlorinated biphenyls (PCBs) at EPA Superfund sites, investigations into PAH and PCB bioavailability at U.S Department of Defense sites, and the application of the techniques to investigating the bioavailability of chlorinated dioxins and furans from impacted

  5. A novel polyaniline/polypyrrole/graphene oxide fiber for the determination of volatile organic compounds in headspace gas of lung cell lines.

    Science.gov (United States)

    Li, JingHong; Xu, Hui

    2017-05-15

    Exploration of volatile organic compounds (VOCs) generated by lung cell lines is a powerful and non-invasive tool for the detection of potential volatile biomarkers of lung cancer. In this study, a simple and sensitive solid phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) method was developed for the determination of VOCs in the headspace gas of lung cell lines. For the purpose of preconcentration, a novel polyaniline/polypyrrole/graphene oxide (PANI/PPy/GO) coating was prepared on the surface of stainless steel fiber via in-situ electrochemical deposition for the first time. The characteristic properties of the coating were studied and the results revealed that the coating possessed large surface area, high extraction efficiency, excellent thermal and mechanical stability as well as long lifespan. Some parameters affecting the extraction efficiency such as synthesis conditions, extraction and desorption conditions were optimized. Under the optimal conditions, the method displayed relatively wide linear range (three or four orders of magnitude) with correlation coefficients above 0.9916. Low detection limits from 1.0 to 12ngL -1 were obtained. Relative standard deviations ranged from 1.2% to 18.0% indicating good repeatability and reproducibility of the method. This method has been successfully applied to analyze VOCs in the headspace gas of lung adenocarcinoma epithelial cell line (A549) and human embryonic fibroblast cell line (MRC-5). Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Stir bar sorptive extraction-gas chromatography-mass spectrometry analysis of tetramethylene disulfotetramine in food: Method development and comparison to solid-phase microextraction.

    Science.gov (United States)

    De Jager, Lowri S; Perfetti, Gracia A; Diachenko, Gregory W

    2009-03-09

    A stir bar sorptive extraction-gas chromatography-mass spectrometry (SBSE-GC-MS) method for the determination of tetramethylene disulfotetramine is presented. The limits of detection (LOD) of the optimized method was 0.2ngg(-1) for extractions from water and 0.3-2.1ngg(-1) for extractions from foods. Recovery was highly matrix dependent (36-130%) and quantification required standard addition calibrations. Standard addition calibration lines had high linearity (R(2)>0.97) and replicate extractions had good reproducibility (R.S.D.=4.4-9.8%). A comparison of the SBSE method and a previously developed headspace (HS)-solid-phase microextraction (SPME) method was performed. Generally, SBSE provided higher sensitivity with decreased analysis time.

  7. Polypyrrole nanowire as an excellent solid phase microextraction fiber for bisphenol A analysis in food samples followed by ion mobility spectrometry.

    Science.gov (United States)

    Kamalabadi, Mahdie; Mohammadi, Abdorreza; Alizadeh, Naader

    2016-08-15

    A polypyrrole nanowire coated fiber was prepared and used in head-space solid phase microextraction coupled with ion mobility spectrometry (HS-SPME-IMS) to the analysis of bisphenol A (BPA) in canned food samples, for the first time. This fiber was synthesized by electrochemical oxidation of the monomer in aqueous solution. The fiber characterization by scanning electron microscopy (SEM) revealed that the new fiber exhibited two-dimensional structures with a nanowire morphology. The effects of important extraction parameters on the efficiency of HS-SPME were investigated and optimized. Under the optimum conditions, the linearity of 10-150ngg(-1) and limit of detection (based on S/N=3) of 1ngg(-1) were obtained in BPA analysis. The repeatability (n=5) expressed as the relative standard deviation (RSD%) was 5.8%. At the end, the proposed method was successfully applied to determine BPA in various canned food samples (peas, corns, beans). Relative recoveries were obtained 93-96%. Method validation was conducted by comparing our results with those obtained through HPLC with fluorescence detection (FLD). Compatible results indicate that the proposed method can be successfully used in BPA analysis. This method is simple and cheaper than chromatographic methods, with no need of extra organic solvent consumption and derivatization prior to sample introduction. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Analysis of volatile organic compounds in compost samples: A potential tool to determine appropriate composting time.

    Science.gov (United States)

    Zhu, Fengxiang; Pan, Zaifa; Hong, Chunlai; Wang, Weiping; Chen, Xiaoyang; Xue, Zhiyong; Yao, Yanlai

    2016-12-01

    Changes in volatile organic compound contents in compost samples during pig manure composting were studied using a headspace, solid-phase micro-extraction method (HS-SPME) followed by gas chromatography with mass spectrometric detection (GC/MS). Parameters affecting the SPME procedure were optimized as follows: the coating was carbon molecular sieve/polydimethylsiloxane (CAR/PDMS) fiber, the temperature was 60°C and the time was 30min. Under these conditions, 87 compounds were identified from 17 composting samples. Most of the volatile components could only be detected before day 22. However, benzenes, alkanes and alkenes increased and eventually stabilized after day 22. Phenol and acid substances, which are important factors for compost quality, were almost undetectable on day 39 in natural compost (NC) samples and on day 13 in maggot-treated compost (MC) samples. Our results indicate that the approach can be effectively used to determine the composting times by analysis of volatile substances in compost samples. An appropriate composting time not only ensures the quality of compost and reduces the loss of composting material but also reduces the generation of hazardous substances. The appropriate composting times for MC and NC were approximately 22days and 40days, respectively, during the summer in Zhejiang. Copyright © 2016 Elsevier Ltd. All rights reserved.

  9. Selective molecularly imprinted polymer combined with restricted access material for in-tube SPME/UHPLC-MS/MS of parabens in breast milk samples.

    Science.gov (United States)

    Souza, Israel D; Melo, Lidervan P; Jardim, Isabel C S F; Monteiro, Juliana C S; Nakano, Ana Marcia S; Queiroz, Maria Eugênia C

    2016-08-17

    A new molecularly imprinted polymer modified with restricted access material (a hydrophilic external layer), (MIP-RAM) was synthesized via polymerization in situ in an open fused silica capillary. This stationary phase was used as sorbent for in-tube solid phase microextraction (in-tube SPME) to determine parabens in breast milk samples by ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Scanning electron micrographs (SEM) illustrate MIP surface modification after glycerol dimethacrylate (hydrophilic monomer) incorporation. The interaction between parabens and MIP-RAM was investigated by Fourier-transform infrared (FTIR) spectroscopy. The Scatchard plot for MIP-RAM presented two linear parts with different slopes, illustrating binding sites with high- and low-affinity. Endogenous compounds exclusion from the MIP-RAM capillary was demonstrated by in-tube SPME/LC-UV assays carried out with blank milk samples. The in-tube SPME/UHPLC-MS/MS method presented linear range from 10 ng mL(-1) (LLOQ) to 400 ng mL(-1) with coefficients of determination higher than 0.99, inter-assay precision with coefficient of variation (CV) values ranging from 2 to 15%, and inter-assay accuracy with relative standard deviation (RSD) values ranging from -1% to 19%. Analytical validation parameters attested that in-tube SPME/UHPLC-MS/MS is an appropriate method to determine parabens in human milk samples to assess human exposure to these compounds. Analysis of breast milk samples from lactating women demonstrated that the proposed method is effective. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Efficient determination of average valence of manganese in manganese oxides by reaction headspace gas chromatography.

    Science.gov (United States)

    Xie, Wei-Qi; Gong, Yi-Xian; Yu, Kong-Xian

    2017-08-18

    This work investigates a new reaction headspace gas chromatographic (HS-GC) technique for efficient quantifying average valence of manganese (Mn) in manganese oxides. This method is on the basis of the oxidation reaction between manganese oxides and sodium oxalate under the acidic condition. The carbon dioxide (CO 2 ) formed from the oxidation reaction can be quantitatively analyzed by headspace gas chromatography. The data showed that the reaction in the closed headspace vial can be completed in 20min at 80°C. The relative standard deviation of this reaction HS-GC method in the precision testing was within 1.08%, the relative differences between the new method and the reference method (titration method) were no more than 5.71%. The new HS-GC method is automated, efficient, and can be a reliable tool for the quantitative analysis of average valence of manganese in the manganese oxide related research and applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. [Determination of olive oil content in olive blend oil by headspace gas chromatography-mass spectrometry].

    Science.gov (United States)

    Jiang, Wanfeng; Zhang, Ning; Zhang, Fengyan; Yang, Zhao

    2017-07-08

    A method for the determination of the content of olive oil in olive blend oil by headspace gas chromatography-mass spectrometry (SH-GC/MS) was established. The amount of the sample, the heating temperature, the heating time, the amount of injection, the injection mode and the chromatographic column were optimized. The characteristic compounds of olive oil were found by chemometric method. A sample of 1.0 g was placed in a 20 mL headspace flask, and heated at 180℃ for 2700 s. Then, 1.0 mL headspace gas was taken into the instrument. An HP-88 chromatographic column was used for the separation and the analysis was performed by GC/MS. The results showed that the linear range was 0-100%(olive oil content). The linear correlation coefficient ( r 2 ) was more than 0.995, and the limits of detection were 1.26%-2.13%. The deviations of olive oil contents in the olive blend oil were from -0.65% to 1.02%, with the relative deviations from -1.3% to 6.8% and the relative standard deviations from 1.18% to 4.26% ( n =6). The method is simple, rapid, environment friendly, sensitive and accurate. It is suitable for the determination of the content of olive oil in olive blend oil.

  12. Fingerprint of volatiles from plant extracts based on SPME-GC-MS

    Directory of Open Access Journals (Sweden)

    Ezequias P. Siqueira

    Full Text Available The Laboratory of Chemistry of Natural Products has an ex situ collection of extracts from organisms of the biodiversity aiming at bioprospecting. Nowadays the collection has about 4000 extracts from 1000 different species. Extracts are used to identify new bioactive compounds that could be useful for developing new drugs against neglected diseases like leishmaniosis, Chagas disease, malaria and tuberculosis. After biologic assays, the bioactive extracts need to be prepared in larger quantity to allow isolation and characterization of the bioactive component. At this time, it is important to not only confirm the bioactivity of new extract but also check if its composition is similar to the old one. It was evaluated the ability of Solid Phase Microextraction and Gas Chromatography-Mass Spectrometry analysis (SPME-GC-MS. It was used the AMDIS (Automatic Mass Spectral Deconvolution and Identification System software as tools to collect and to compare the chromatographic profiles of each extract (fingerprint. Forty six samples were analyzed, it was possible to infer from the composition of each sample and common compounds. Nine groups of samples, collected at different time, were analyzed and seasonal modifications between then could be elucidated. The results showed that this methodology can be used to monitor the composition of extracts, allowing to monitor chemical changes that may occur during storage periods and to investigate the occurrence of a determined component in different extracts.

  13. Characterization of wood plastic composites made from landfill-derived plastic and sawdust: volatile compounds and olfactometric analysis.

    Science.gov (United States)

    Félix, Juliana S; Domeño, Celia; Nerín, Cristina

    2013-03-01

    Application of wood plastic composites (WPCs) obtained from recycled materials initially intended for landfill is usually limited by their composition, mainly focused on release of volatile organic compounds (VOCs) which could affect quality or human safety. The study of the VOCs released by a material is a requirement for new composite materials. Characterization and quantification of VOCs of several WPC produced with low density polyethylene (LDPE) and polyethylene/ethylene vinyl acetate (PE/EVA) films and sawdust were carried out, in each stage of production, by solid phase microextraction in headspace mode (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). An odor profile was also obtained by HS-SPME and GC-MS coupled with olfactometry analysis. More than 140 compounds were observed in the raw materials and WPC samples. Some quantified compounds were considered WPC markers such as furfural, 2-methoxyphenol, N-methylphthalimide and 2,4-di-tert-butylphenol. Hexanoic acid, acetic acid, 2-methoxyphenol, acetylfuran, diacetyl, and aldehydes were the most important odorants. None of the VOCs were found to affect human safety for use of the WPC. Copyright © 2012 Elsevier Ltd. All rights reserved.

  14. Development of a dynamic headspace solid-phase microextraction procedure coupled to GC-qMSD for evaluation the chemical profile in alcoholic beverages

    International Nuclear Information System (INIS)

    Rodrigues, F.; Caldeira, M.; Camara, J.S.

    2008-01-01

    In the present study, a simple and sensitive methodology based on dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography with quadrupole mass detection (GC-qMSD), was developed and optimized for the determination of volatile (VOCs) and semi-volatile (SVOCs) compounds from different alcoholic beverages: wine, beer and whisky. Key experimental factors influencing the equilibrium of the VOCs and SVOCs between the sample and the SPME fibre, as the type of fibre coating, extraction time and temperature, sample stirring and ionic strength, were optimized. The performance of five commercially available SPME fibres was evaluated and compared, namely polydimethylsiloxane (PDMS, 100 μm); polyacrylate (PA, 85 μm); polydimethylsiloxane/divinylbenzene (PDMS/DVB, 65 μm); carboxen TM /polydimethylsiloxane (CAR/PDMS, 75 μm) and the divinylbenzene/carboxen on polydimethylsiloxane (DVB/CAR/PDMS, 50/30 μm) (StableFlex). An objective comparison among different alcoholic beverages has been established in terms of qualitative and semi-quantitative differences on volatile and semi-volatile compounds. These compounds belong to several chemical families, including higher alcohols, ethyl esters, fatty acids, higher alcohol acetates, isoamyl esters, carbonyl compounds, furanic compounds, terpenoids, C13-norisoprenoids and volatile phenols. The optimized extraction conditions and GC-qMSD, lead to the successful identification of 44 compounds in white wines, 64 in beers and 104 in whiskys. Some of these compounds were found in all of the examined beverage samples. The main components of the HS-SPME found in white wines were ethyl octanoate (46.9%), ethyl decanoate (30.3%), ethyl 9-decenoate (10.7%), ethyl hexanoate (3.1%), and isoamyl octanoate (2.7%). As for beers, the major compounds were isoamyl alcohol (11.5%), ethyl octanoate (9.1%), isoamyl acetate (8.2%), 2-ethyl-1-hexanol (5.9%), and octanoic acid (5.5%). Ethyl decanoate (58

  15. Determination of styrene content in Gorgonzola PDO cheese by headspace solid phase micro-extraction (HS-SPME) and gas-chromatography mass-spectrometry (GC-MS).

    Science.gov (United States)

    Chiesa, L M; Panseri, S; Soncin, S; Vallone, L; Dragoni, I

    2010-06-01

    Control of the composition of products that are intended for use as packaging material is essential, particularly when these products come into direct contact with food. It is well known that plastics are not inert and that their residual monomers, starting substances, and additives are able to migrate into the food they contact. Among plastics, styrene is a common compound found in many plastic containers that can also be produced by the oxidation of Penicillium roqueforti used in gorgonzola Protected Denomination of Origin cheese manufacturing. Therefore, solid-phase microextraction combined with gas chromatography/mass spectrometry was applied in the present work to determine the styrene content in packaged and unpackaged gorgonzola cheese samples to understand styrene migration phenomena from plastic containers.

  16. Headspace-solid phase microextraction approach for dimethylsulphoniopropionate quantification in Solanum lycopersicum plants subjected to water stress

    Directory of Open Access Journals (Sweden)

    Stefano Catola

    2016-08-01

    Full Text Available Dimethylsulphoniopropionate (DMSP and dimethyl sulphide (DMS are compounds found mainly in marine phytoplankton and in some halophytic plants. DMS is a globally important biogenic volatile in regulating of global sulphur cycle and planetary albedo, whereas DMSP is involved in the maintenance of plant-environment homeostasis. Plants emit minute amounts of DMS compared to marine phytoplankton and there is a need for hypersensitive analytic techniques to enable its quantification in plants. Solid Phase Micro Extraction from Head Space (HS-SPME is a simple, rapid, solvent-free and cost-effective extraction mode, which can be easily hyphenated with GC-MS for the analysis of volatile organic compounds (VOCs. Using tomato (Solanum lycopersicum plants subjected to water stress as a model system, we standardized a sensitive and accurate protocol for detecting and quantifying DMSP pool sizes, and potential DMS emissions, in cryoextracted leaves. The method relies on the determination of DMS free and from DMSP pools before and after the alkaline hydrolysis via HS-SPME-GC-MS. We found a significant (2.5 time increase of DMSP content in water-stressed leaves reflecting clear stress to the photosynthetic apparatus. We hypothesize that increased DMSP, and in turn DMS, in water-stressed leaves are produced by carbon sources other than direct photosynthesis, and function to protect plants either osmotically or as antioxidants. Finally, our results suggest that SPME is a powerful and suitable technique for the detection and quantification of biogenic gases in trace amounts.

  17. Direct determination of anabolic steroids in pig urine by a new SPME-GC-MS method.

    Science.gov (United States)

    Zhang, Zhuomin; Duan, Hongbin; Zhang, Lan; Chen, Xi; Liu, Wei; Chen, Guonan

    2009-05-15

    A new solid phase microextraction (SPME) method coupled with gas chromatography-mass spectrometry (GC-MS) was developed for rapid determination of four anabolic steroids such as 3alpha-hydroxy-5alpha-androstane-17-one (HA), dihydrotestosterone (DHT), androstenedione (AD) and methyltestosterone (MT) in pig urine. SPME was used to extract the four anabolic compounds directly without derivatization. The optimum SPME sampling conditions were based on the home-made carbowax-divinylbenzene (CW-DVB) fiber coating during extraction at 40 degrees C for 50 min with 0.18 g/mL NaCl solution and 750 rpm stirring speed. The linear ranges of the proposed method were in the range of 8-640 pg/mL for HA and DHT and 16-510 pg/mL for AD and MT, respectively. The detection limits (S/N=3) were from 2 to 8 pg/mL for the four anabolic steroids. This SPME method provided very high enrichment factors for the four anabolic steroids, which were 1063-fold and 965-fold for HA and DHT at the concentration of 8 pg/mL and 207-fold and 451-fold for AD and MT at the concentration of 16 pg/mL, respectively. The recoveries ranged from 71.3 to 121%, and the RSDs were lower than 12.9%. The method was sensitive and reliable for determination of trace anabolic steroids in biological samples.

  18. Measurement of mercury species in human blood using triple spike isotope dilution with SPME-GC-ICP-DRC-MS.

    Science.gov (United States)

    Sommer, Yuliya L; Verdon, Carl P; Fresquez, Mark R; Ward, Cynthia D; Wood, Elliott B; Pan, Yi; Caldwell, Kathleen L; Jones, Robert L

    2014-08-01

    The measurement of different mercury compounds in human blood can provide valuable information about the type of mercury exposure. To this end, our laboratory developed a biomonitoring method for the quantification of inorganic (iHg), methyl (MeHg), and ethyl (EtHg) mercury in whole blood using a triple-spike isotope dilution (TSID) quantification method employing capillary gas chromatography (GC) and inductively coupled dynamic reaction cell mass spectrometry (ICP-DRC-MS). We used a robotic CombiPAL(®) sample handling station featuring twin fiber-based solid-phase microextraction (SPME) injector heads. The use of two SPME fibers significantly reduces sample analysis cycle times making this method very suitable for high sample throughput, which is a requirement for large public health biomonitoring studies. Our sample preparation procedure involved solubilization of blood samples with tetramethylammonium hydroxide (TMAH) followed by the derivatization with sodium tetra(n-propyl)borate (NaBPr(4)) to promote volatility of mercury species. We thoroughly investigated mercury species stability in the blood matrix during the course of sample treatment and analysis. The method accuracy for quantifying iHg, MeHg, and EtHg was validated using NIST standard reference materials (SRM 955c level 3) and the Centre de Toxicologie du Québec (CTQ) proficiency testing (PT) samples. The limit of detection (LOD) for iHg, MeHg, and EtHg in human blood was determined to be 0.27, 0.12, and 0.16 μg/L, respectively.

  19. Tank vapor characterization project. Tank 241-S-102 temporal study headspace gas and vapor characterization results from samples collected on September 19, 1996

    International Nuclear Information System (INIS)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.; Sklarew, D.S.

    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

  20. Headspace vapor characterization of Hanford Waste Tank 241-BX-107: Results from samples collected on November 17, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Evans, J.C.; Thomas, B.L.; Pool, K.H.

    1996-06-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-BX-107 (Tank BX-107) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5080. Samples were collected by WHC on November 17, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  1. Headspace vapor characterization of Hanford Waste Tank 241-S-108: Results from samples collected on December 6, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Thomas, B.L.; Evans, J.C.; McVeety, B.D.

    1996-06-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-S-108 (Tank S-108) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5086. Samples were collected by WHC on December 6, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  2. Headspace vapor charterization of Hanford Waste Tank 241-S-110: Results from samples collected on December 5, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Thomas, B.L.; Evans, J.C.; McVeety, B.D.

    1996-06-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-S-110 (Tank S-110) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5085. Samples were collected by WHC on December 5, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  3. Headspace vapor characterization of Hanford Waste Tank 241-BY-102: Results from samples collected on November 21, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Thomas, B.L.; Evans, J.C.; Pool, K.H.

    1996-06-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-BY-102 (Tank BY-102) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5081. Samples were collected by YMC on November 21, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  4. Headspace vapor characterization of Hanford Waste Tank 241-SX-104: Results from samples collected on July 25, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Thomas, B.L.; Clauss, T.W.; Evans, J.C.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-SX-104 (Tank SX-104) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5049. Samples were collected by WHC on July 25, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  5. Headspace vapor characterization of Hanford Waste Tank 241-T-110: Results from samples collected on August 31, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    McVeety, B.D.; Thomas, B.L.; Evans, J.C.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-T-110 (Tank T-110) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5056. Samples were collected by WHC on August 31, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  6. Headspace vapor characterization of Hanford Waste Tank 241-SX-105: Results from samples collected on July 26, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Pool, K.H.; Clauss, T.W.; Evans, J.C.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-SX-105 (Tank SX-105) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5047. Samples were collected by WHC on July 26, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  7. Headspace vapor characterization of Hanford Waste Tank 241-SX-109: Results from samples collected on August 1, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Pool, K.H.; Clauss, T.W.; Evans, J.C.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-SX-109 (Tank SX-109) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5048. Samples were collected by WHC on August 1, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  8. Headspace vapor characterization of Hanford Waste Tank SX-102: Results from samples collected on July 19, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    McVeety, B.D.; Evans, J.C.; Clauss, T.W.; Pool, K.H.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-SX-102 (Tank SX-102) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed under the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5046. Samples were collected by WHC on July 19, 1995, using the vapor sampling system (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  9. Headspace vapor characterization of Hanford Waste Tank AX-103: Results from samples collected on June 21, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Ligotke, M.W.; Pool, K.H.; Clauss, T.W.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-AX-103 (Tank AX-103) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5029. Samples were collected by WHC on June 21, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  10. Headspace vapor characterization of Hanford Waste Tank AX-101: Results from samples collected on June 15, 1995. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Pool, K.H.; Clauss, T.W.; Evans, J.C.; McVeety, B.D.

    1996-05-01

    This report describes the results of vapor samples taken from the headspace of waste storage tank 241-AX-101 (Tank AX-101) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) contracted with Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for inorganic and organic analytes collected from the tank headspace and ambient air near the tank. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) under the Tank Vapor Characterization Project. Work performed was based on a sample and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Vapor Sampling and Analysis Planclose quotes, and the sample job was designated S5028. Samples were collected by WHC on June 15, 1995, using the Vapor Sampling System (VSS), a truck-based sampling method using a heated probe inserted into the tank headspace

  11. 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.

  12. Tank 241-C-107 fifth temporal study: Headspace gas and vapor characterization results from samples collected on February 7, 1997. Tank vapor characterization project

    International Nuclear Information System (INIS)

    Hayes, J.C.; Pool, K.H.; Evans, J.C.

    1997-08-01

    This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-C-107 (Tank C-107) at the Hanford Site in Washington State. Tank headspace samples collected by SGN Eurisys Services 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. No analytes were determined to be above the immediate notification limits specified by the sampling and analysis plan (SAP). Hydrogen was the principal flammable constituent of the Tank C-107 headspace, determined to be present at approximately 3.233% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <3.342% 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

  13. Tank Vapor Characterization Project: Tank 241-C-107 fourth temporal study: Headspace gas and vapor characterization results from samples collected on December 17, 1996

    International Nuclear Information System (INIS)

    Pool, K.H.; Evans, J.C.; Olsen, K.B.; Hayes, J.C.

    1997-08-01

    This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-C-107 (Tank C-107) at the Hanford Site in Washington State. Tank headspace samples 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. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by SESC. No analytes were determined to be above the immediate notification limits specified by the sampling and analysis plan (SAP). Hydrogen was the principal flammable constituent of the Tank C-107 headspace, determined to be present at approximately 2.825% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <2.935% 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

  14. 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 constituent of the Tank BX-103 headspace, determined to be present at approximately 0.385% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <0.633% if 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.

  15. 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.

  16. 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. Published by Elsevier B.V.

  17. Optimization of total vaporization solid-phase microextraction (TV-SPME) for the determination of lipid profiles of Phormia regina, a forensically important blow fly species.

    Science.gov (United States)

    Kranz, William; Carroll, Clinton; Dixon, Darren; Picard, Christine; Goodpaster, John

    2017-11-01

    A new method has been developed for the determination of fatty acids, sterols, and other lipids which naturally occur within pupae of the blow fly Phormia regina. The method relies upon liquid extraction in non-polar solvent, followed by derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) w/ 1% trimethylchlorsilane (TMCS) carried out inside the sample vial. The analysis is facilitated by total vaporization solid-phase microextraction (TV-SPME), with gas chromatography-mass spectrometry (GC-MS) serving as the instrumentation for analysis. The TV-SPME delivery technique is approximately a factor of five more sensitive than traditional liquid injection, which may alleviate the need for rotary evaporation, reconstitution, collection of high performance liquid chromatography fractions, and many of the other pre-concentration steps that are commonplace in the current literature. Furthermore, the ability to derivatize the liquid extract in a single easy step while increasing sensitivity represents an improvement over current derivatization methods. The most common lipids identified in fly pupae were various saturated and unsaturated fatty acids ranging from lauric acid (12:0) to arachinoic acid (20:4), as well as cholesterol. The concentrations of myristic acid (14:0), palmitelaidic acid (16:2), and palmitoleic acid (16:1) were the most reliable indicators of the age of the pupae. Graphical abstract Blow fly pupae were extracted prior to emerging as adults. The extracts were analyzed via total vaporization solid-phase microextraction (TV-SPME), revealing a complex mixture of lipids that could be associated with the age of the insect. This information may assist in determining a post-mortum interval (PMI) in a death investigation.

  18. Simple determination of hydrazine in waste water by headspace solid-phase micro extraction and gas chromatography-tandem mass spectrometry after derivatization with trifluoro pentanedione.

    Science.gov (United States)

    Oh, Jin-Aa; Shin, Ho-Sang

    2017-01-15

    A headspace solid-phase micro extraction (HS-SPME) and gas chromatography-tandem mass spectrometric (GC-MS/MS) method is described to detect hydrazine after derivatization with 1,1,1-trifluoro-2,4-pentanedione (1,1,1-TFPD) to 3-methyl-5-(trifluoromethyl) pyrazole in industrial waste water. The following optimal HS-SPME conditions were used: 85 μm-carboxen-polydimethylsiloxane fibre, 100 mg L -1 TFPD, saturated NaCl, an extraction/derivatization temperature of 80 °C, a heating time of 40 min, and a pH of 9.5. Under the established conditions, the detection and quantification limits were 0.002 μg L -1 and 0.007 μg L -1  by using 5 mL of waste water and the intra- and inter-day relative standard deviations were less than 10.2% at concentrations of 0.02 and 0.1 μg L -1 . The calibration curve showed good linearity, with r 2  = 0.998; the accuracy was in the range of 98.0-103%; and the precision of the assay was less than 10.2% in industrial waste water. Hydrazine was detected over a concentration range of 0.011-0.074 μg L -1 in 5 of 20 waste water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Determination of caffeine, myosmine, and nicotine in chocolate by headspace solid-phase microextraction coupled with gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Müller, Christoph; Vetter, Florian; Richter, Elmar; Bracher, Franz

    2014-02-01

    The occurrence of the bioactive components caffeine (xanthine alkaloid), myosmine and nicotine (pyridine alkaloids) in different edibles and plants is well known, but the content of myosmine and nicotine is still ambiguous in milk/dark chocolate. Therefore, a sensitive method for determination of these components was established, a simple separation of the dissolved analytes from the matrix, followed by headspace solid-phase microextraction coupled with gas chromatography-tandem mass spectrometry (HS-SPME-GC-MS/MS). This is the first approach for simultaneous determination of caffeine, myosmine, and nicotine with a convenient SPME technique. Calibration curves were linear for the xanthine alkaloid (250 to 3000 mg/kg) and the pyridine alkaloids (0.000125 to 0.003000 mg/kg). Residuals of the calibration curves were lower than 15%, hence the limits of detection were set as the lowest points of the calibration curves. The limits of detection calculated from linearity data were for caffeine 216 mg/kg, for myosmine 0.000110 mg/kg, and for nicotine 0.000120 mg/kg. Thirty samples of 5 chocolate brands with varying cocoa contents (30% to 99%) were analyzed in triplicate. Caffeine and nicotine were detected in all samples of chocolate, whereas myosmine was not present in any sample. The caffeine content ranged from 420 to 2780 mg/kg (relative standard deviation 0.1 to 11.5%) and nicotine from 0.000230 to 0.001590 mg/kg (RSD 2.0 to 22.1%). © 2014 Institute of Food Technologists®

  20. Extração em fase sólida (SPE e micro extração em fase sólida (SPME de piretróides em água Solid-phase extraction (SPE and solid-phase microextraction of pyrethroids in water

    Directory of Open Access Journals (Sweden)

    Wilma Regina Barrionuevo

    2001-04-01

    Full Text Available The pyrethroids bifenthrin, permethrin, cypermethrin and deltamethrin were extracted by solid phase extraction (SPE and solid phase microextraction (SPME. The analysis were performed on a gas chromatograph with electron capture detection (GC-ECD. Octadecil Silano-C18, Florisil and Silica stationary phases were studied for SPE. Better results were obtained for Florisil which gave recoveries from 80% to 108%. Pyrethroids extraction by SPME showed a linear response and a detection limit of 10 pg ml-1. Although the data showed that the two extraction methods were able to isolate the pesticide residues from water samples, the best results were obtained by using SPME which is more sensitive, faster, cheeper, being a more useful technique for the analysis of pyrethroids in drinking water.

  1. A platinized stainless steel fiber with in-situ coated polyaniline/polypyrrole/graphene oxide nanocomposite sorbent for headspace solid-phase microextraction of aliphatic aldehydes in rice samples.

    Science.gov (United States)

    Ghiasvand, Alireza; Nasirian, Afagh; Koonani, Samira; Nouriasl, Kolsoum

    2017-12-01

    The surface of a stainless steel fiber was made larger, porous and cohesive by platinizing for tight attachment of its coating. Then it was coated by a polyaniline/polypyrrole/graphene oxide (PANI/PP/GO) nanocomposite film using electrochemical polymerization. The prepared PANI/PP/GO fiber was used for headspace solid-phase microextraction (HS-SPME) of linear aliphatic aldehydes in rice samples followed by GC-FID determination. To achieve the highest extraction efficiency, various experimental parameters including extraction time and temperature, matrix modifier and desorption condition were studied. The linear calibration curves were obtained over the range of 0.05-20 μg g -1 (R 2  > 0.99) for C 4 -C 11 aldehydes. The limits of detection were found to be in the range of 0.01-0.04 μg g -1 . RSD values were calculated to be <7.4 and 10.7% for intra- and inter-day, respectively. The superiority of the prepared nanocomposite SPME fiber was established by comparison of its results with those obtained by polydimethylsiloxane, carbowax-divinylbenzene, divinylbenzene-carboxen-polydimethylsiloxane and polyacrylate commercial ones. Finally, the nanocomposite fiber was used to extract and determine linear aliphatic aldehydes in 18 rice samples. Copyright © 2017 John Wiley & Sons, Ltd.

  2. Cannabinoids determination in oral fluid by SPME-GC/MS and UHPLC-MS/MS and its application on suspected drivers.

    Science.gov (United States)

    Anzillotti, Luca; Castrignanò, Erika; Strano Rossi, Sabina; Chiarotti, Marcello

    2014-12-01

    The confirmation of Δ9-tetrahydrocannabinol (THC) in oral fluid (OF) is an important issue for assessing Driving Under the Influence of Drugs (DUID). The aim of this research was to develop a highly sensitive method with minimal sample pre-treatment suitable for the analysis of small OF volumes (100 μL) for the confirmation of cannabinoids in DUID cases. Two methods were compared for the confirmation of THC in residual OF samples, obtained from a preliminary on-site screening with commercial devices. An ultra high performance LC-MS (UHPLC-MS/MS) method and an SPME-GC/MS method were hence developed. 100 μL of the residual mixture OF/preservative buffer or neat OF was simply added to 10 μL of THC-D3 (1 μg/mL) and submitted to the two different analyses: A - direct injection of 10 μL in UHPLC-MS/MS in positive electrospray ionisation (ESI) mode and B - sampling for 30 min with SPME (100 μm polydimethylsiloxane or PDMS fibre) and direct injection by desorption of the fibre in the GC injection port. The lowest limit of detection (LLOD) of THC was 2 ng/mL in UHPLC-MS/MS and 0.5 ng/mL in SPME-GC/MS. In addition, cannabidiol (CBD) and cannabinol (CBN) could be detected in GC/MS equipment at 2 ng/mL, whilst in UHPLC-MS/MS the LLOD was 20 ng/mL. Both methods were applied to 70 samples coming from roadside tests. By SPME-GC/MS analysis, THC was confirmed in 42 samples, whilst CBD was detected in 21 of them, along with CBN in 14 samples. THC concentrations ranged from traces below the lowest limit of quantification or LLOQ (2 ng/mL) up to 690 ng/mL. Copyright © 2014 Forensic Science Society. Published by Elsevier Ireland Ltd. All rights reserved.

  3. Evaluation of the volatile profile of Tuber liyuanum by HS-SPME with GC-MS.

    Science.gov (United States)

    Liu, Changjiao; Li, Yu

    2017-04-01

    The volatile components of Tuber liyuanum were determined by HS-SPME with GC-MS for the first time. The effects of different fibre coating, extraction time, extraction temperature and sample amount were studied to get optimal extraction conditions. The optimal conditions were SPME fibre of Carboxen/PDMS, extraction time of 40 min, extraction temperature of 80 °C, sample amount of 2 g. Under these conditions 57 compounds in volatile of T. liyuanum were detected with a resemblance percentage above 80%. Aldehydes and aromatics were the main chemical families identified. The contribution of 3-Octanone(11.67%), phenylethyl alcohol (10.60%), isopentana (9.29%) and methylbutana (8.06%) for the total volatile profile were more significant in T. liyuanum than other compounds.

  4. Critical evaluation of fiber coatings for organotin determination by using solid phase microextraction in headspace mode.

    Science.gov (United States)

    Bravo, Manuel M; Valenzuela, Aníbal S; Fuentes, Edwar P; Quiroz, Waldo V

    2012-02-03

    In the present work three different SPME fibers have been investigated for simultaneous determination of methyl-, butyl- and phenyltins by using gas chromatography-pulsed flame photometer detection (GC-PFPD). The optimal experimental conditions for each fiber were determined and the respective figures of merit were evaluated. All fiber evaluated presented similar limit of detection (sub ng L⁻¹) and requires two internal standards to reach an acceptable repeatability. However, the CAR-PDMS fiber offers the best compromise between selectivity and sensibility for determination of organotins selected. The developed method was validated for analysis of certified reference material and spiked samples, obtaining satisfactory results. Finally, some contaminated samples were analyzed demonstrating the applicability of developed method for determination of organotin compounds in the environment and for monitoring their biochemical cycle. Copyright © 2011 Elsevier B.V. All rights reserved.

  5. Determination of volatile organic compounds in water by headspace solid-phase microextraction gas chromatography coupled to tandem mass spectrometry with triple quadrupole analyzer

    Energy Technology Data Exchange (ETDEWEB)

    Cervera, M.I. [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain); Beltran, J., E-mail: joaquim.beltran@uji.es [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain); Lopez, F.J.; Hernandez, F. [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain)

    2011-10-17

    Highlights: {yields} Employing a statistical optimization improves results reducing experiments. {yields} Use of MS (QqQ) allows high sensitivity determination and improves identification capabilities. {yields} Using Q/q intensity ratios is a powerful tool to ensure compound identification. {yields} HS SPME GC-MS/MS method allows determination of VOCs in complex matrix water samples. - Abstract: 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 {mu}m fiber for 30 min at 50 deg. 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 {mu}g L{sup -1}). Recoveries between 70% and 120% were generally obtained with

  6. Headspace vapor characterization of Hanford waste tank 241-S-106: Results from samples collected on 06/13/96

    International Nuclear Information System (INIS)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-S-106 (Tank S-106) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in a table. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples are also listed in the same table. Detailed descriptions of the analytical results appear in the appendices

  7. Headspace vapor characterization of Hanford waste tank 241-B-202: Results from samples collected on 7/18/96

    International Nuclear Information System (INIS)

    Thomas, B.L.; Evans, J.C.; Pool, K.H.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-B-202 (Tank B-202) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in a table. Detailed descriptions of the analytical results appear in the appendices

  8. Headspace vapor characterization of Hanford waste Tank 241-C-202: Results from samples collected on 06/25/96

    International Nuclear Information System (INIS)

    Pool, K.H.; Evans, J.C.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-C-202 (Tank C-202) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, on sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in a table. Detailed descriptions of the analytical results appear in the appendices

  9. Headspace vapor characterization of Hanford waste Tank 241-C-201: Results from samples collected on 06/19/96

    International Nuclear Information System (INIS)

    Thomas, B.L.; Evans, J.C.; Pool, K.H.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-C-201 (Tank C-201) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, on sample volumes provided by WHC. A summary, of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in a table. Detailed descriptions of the analytical results appear in the appendices

  10. Headspace vapor characterization of Hanford waste tank 241-B-107: Results from samples collected on 7/23/96

    International Nuclear Information System (INIS)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-B-107 (Tank B-107) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwestern National Laboratory (PNNL). A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in a table. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples are also listed in the same table. Detailed descriptions of the analytical results appear in the appendices

  11. Characterization and classification of pequi trees (Caryocar brasiliense Camb. based on the profile of volatile constituents using headspace solid-phase microextraction - gas chromatography - mass spectrometry and multivariate analysis Caracterização e classificação de pequizeiros (Caryocar brasiliense Camb. baseadas no perfil de constituintes voláteis usando microextração em fase sólida no modo headspace - cromatografia a gás - espectrometria de massas e análise multivariada

    Directory of Open Access Journals (Sweden)

    Renata França Cassimiro Belo

    2013-02-01

    Full Text Available In order to determine the variability of pequi tree (Caryocar brasiliense Camb. populations, volatile compounds from fruits of eighteen trees representing five populations were extracted by headspace solid-phase microextraction and analyzed by gas chromatography-mass spectrometry. Seventy-seven compounds were identified, including esters, hydrocarbons, terpenoids, ketones, lactones, and alcohols. Several compounds had not been previously reported in the pequi fruit. The amount of total volatile compounds and the individual compound contents varied between plants. The volatile profile enabled the differentiation of all of the eighteen plants, indicating that there is a characteristic profile in terms of their origin. The use of Principal Component Analysis and Cluster Analysis enabled the establishment of markers (dendrolasin, ethyl octanoate, ethyl 2-octenoate and β-cis-ocimene that discriminated among the pequi trees. According to the Cluster Analysis, the plants were classified into three main clusters, and four other plants showed a tendency to isolation. The results from multivariate analysis did not always group plants from the same population together, indicating that there is greater variability within the populations than between pequi tree populations.A fim de determinar a variabilidade de populações de pequizeiro (Caryocar brasiliense Camb., compostos voláteis de frutos de dezoito árvores representando cinco populações foram extraídos por microextração em fase sólida no modo headspace e analisados por cromatografia a gás acoplada à espectrometria de massas. Setenta e sete compostos foram identificados, incluindo ésteres, hidrocarbonetos, terpenoides, cetonas, lactonas e álcoois. Vários compostos não haviam sido encontrados anteriormente no fruto. A quantidade total e a composição de voláteis variaram entre as plantas. O perfil volátil permitiu a diferenciação de todas as dezoito plantas, indicando que há um

  12. Tank vapor characterization report headspace vapor characterization of Hanford tank 241-S-105: results from samples collected on 12/07/95

    International Nuclear Information System (INIS)

    Pool, K.H.; Thomas, B.L.; Evans, J.C.; McVeety, B.D.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1996-06-01

    This document presents the details of the inorganic and organic analysis that was performed on samples from the headspace of Hanford waste tank 241-S-105. The results described were obtained to support the safety evaluations and tank operations. A summary of the results for the inorganic and organic analytes is included, as well as, a detailed description of the results

  13. Quantification of liquid products from the electroreduction of CO2 and CO using static headspace-gas chromatography and nuclear magnetic resonance spectroscopy

    DEFF Research Database (Denmark)

    Bertheussen, Erlend; Abghoui, Younes; Jovanov, Zarko P.

    2017-01-01

    Static headspace-gas chromatography (HS-GC) useful for ex-situ liquid product analysis. Could complement high-performance liquid chromatography and NMR spectroscopy. Particularly high sensitivity towards compounds with high vapor pressure. Detection limits below 0.5μM were shown for acetaldehyde ...

  14. Potential application of microsensor technology in radioactive waste management with emphasis on headspace gas detection

    International Nuclear Information System (INIS)

    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

    2004-01-01

    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 and 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 b ullet) 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 b ullet) 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 b ullet) 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-called 'coffee ring

  15. [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.

  16. Rapid determination of methanol in black liquors by full evaporation headspace gas chromatography.

    Science.gov (United States)

    Li, Hailong; Zhan, Huaiyu; Fu, Shiyu; Liu, Mengru; Chai, Xin-Sheng

    2007-12-14

    This paper reported a full evaporation headspace gas chromatographic (GC) technique for determination of methanol content in black liquors (pulping spent liquor). In this method, a very small volume (10-20 microL) of liquor sample is introduced into a headspace sample vial (20 mL) and heated up to a temperature of 105 degrees C. A near-complete mass transfer of methanol from the liquid phase to vapor phase (headspace), i.e., a full evaporation, can be achieved within 3 min. The methanol in the headspace of the vial is then measured by GC. The present method is simple, rapid and accurate.

  17. Comparison between solid phase microextraction (SPME) and hollow fiber liquid phase microextraction (HFLPME) for determination of extractables from post-consumer recycled PET into food simulants.

    Science.gov (United States)

    Oliveira, Éder Costa; Echegoyen, Yolanda; Cruz, Sandra Andrea; Nerin, Cristina

    2014-09-01

    Hollow fiber liquid phase microextraction (HFLPME) and solid phase microextraction (SPME) methods for pre-concentration of contaminants (toluene, benzophenone, tetracosane and chloroform) in food simulants were investigated. For HFLPME 1-heptanol, 2-octanone and dibutyl-ether were studied as extracting solvents. Analysis by gas chromatography coupled to mass spectrometry (GC-MS), flame ionization (GC-FID) and electron capture detectors (GC-ECD) were carried out. In addition, the methods were employed to evaluate the safety in use of a PET material after the recycling process (comprising washing, extrusion and solid state polymerization (SSP)) through extractability studies of the contaminants using 10% (v/v) ethanol in deionized water and 3% (w/v) acetic acid in deionized water as food simulants in different conditions: 10 days at 40°C and 2h at 70°C. The HFLPME preconcentration method provided increased sensitivity when compared to the SPME method and allowed to analyze concentration levels below 10 µg surrogate per kg food simulant. The results of the extractability studies showed considerable reductions after the extrusion and SSP processes and indicated the compliance with regulations for using recycled PET in contact with food. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Comprehensive quality evaluation of medical Cannabis sativa L. inflorescence and macerated oils based on HS-SPME coupled to GC-MS and LC-HRMS (q-exactive orbitrap®) approach.

    Science.gov (United States)

    Calvi, Lorenzo; Pentimalli, Daniela; Panseri, Sara; Giupponi, Luca; Gelmini, Fabrizio; Beretta, Giangiacomo; Vitali, Davide; Bruno, Massimo; Zilio, Emanuela; Pavlovic, Radmila; Giorgi, Annamaria

    2018-02-20

    There are at least 554 identified compounds in C. sativa L., among them 113 phytocannabinoids and 120 terpenes. Phytocomplex composition differences between the pharmaceutical properties of different medical cannabis chemotype have been attributed to strict interactions, defined as 'entourage effect', between cannabinoids and terpenes as a result of synergic action. The chemical complexity of its bioactive constituents highlight the need for standardised and well-defined analytical approaches able to characterise the plant chemotype, the herbal drug quality as well as to monitor the quality of pharmaceutical cannabis extracts and preparations. Hence, in the first part of this study an analytical procedures involving the combination of headspace-solid-phase microextraction (HS-SPME) coupled to GC-MS and High Resolution Mass-Spectrometry LC-HRMS (Orbitrap ® ) were set up, validated and applied for the in-depth profiling and fingerprinting of cannabinoids and terpenes in two authorised medical grade varieties of Cannabis sativa L. inflorescences (Bedrocan ® and Bediol ® ) and in obtained macerated oils. To better understand the trend of all volatile compounds and cannabinoids during oil storage a new procedure for cannabis macerated oil preparation without any thermal step was tested and compared with the existing conventional methods to assess the potentially detrimental effect of heating on overall product quality. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. EVALUACIÓN DE PLAGUICIDAS 0RGAN0CL0RAD0S POR HS-SPME - GC/ECD EN LECHE PASTEURIZADA COMERCIALIZADA EN LA CIUDAD DE CARTAGENA (COLOMBIA A AVALIAQÁO DOS PESTICIDAS ORGANOCLORADOS POR HS-SPME - GC/ECD EM LEITE PASTEURIZADO COMERCIALIZADAS NA CIDADE CARTAGENA (COLOMBIA EVALUATION OF PESTICIDES BY HS-SPME ORGANOCHLORINE - GC / ECD IN PASTEURIZED MILK MARKETED IN THE CITY CARTAGENA (COLOMBIA

    Directory of Open Access Journals (Sweden)

    DENILES DEL CARMEN DE ARCO R

    2011-12-01

    Full Text Available Los plaguicidas han sido utilizados en todo el mundo desde mediados del siglo XX, en campañas de Salud Pública y en prácticas agrícolas. Los Plaguicidas Organoclorados (POCs presentan mayor impacto sobre el ambiente porque no son biodegradables, son lipofílicos, tienen gran movilidad por todo el planeta y gran tendencia a la bioacumulación, através de la cadena trófica. Con el objetivo de identificar y cuantificar plaguicidas organoclorados en leche entera pasteurizada de dos marcas (A y B, que se comercializan en la ciudad de Cartagena de Indias, se realizó la presente investigación, utilizando Microextracción en Fase Sólida en Espacio de Cabeza y Cromatografía de Gases con Detector de Captura de Electrones (HS-SPME-GC/ECD. Fueron analizadas 36 muestras (n=36, 18 de cada marca. El 100% de las muestras (n=36 resultaron positivas para el plaguicida lindano (γ-HCH, superando el Límite Máximo Residual (LMR de 0,01 mg/kg, establecido por la Food and Agriculture Organization y la Organización Mundial de la Salud (FAO/OMS. Las concentraciones promedio de lindano obtenidas para la marca A fueron de 0,042 mg/kg ± 0,003 y 0,062 ± 0,0016 mg/kg (base grasa para la marca B, no superando la Ingesta Diaria Admisible (IDA de 0,001 mg/kg de peso corporal.Os pesticidas têm sido usados em todo o mundo desde meados do século XX, as campanhas de saúde pública e práticas agrícolas. Os inseticidas organoclorados (AP têm maior impacto sobre o meio ambiente porque não são biodegradáveis, são lipofílicas, têm grande mobilidade ao redor do mundo e maior tendencia para a bioacumulação através da cadeia alimentar. A fim de identificar e quantificar pesticidas organoclorados em leite integral, duas marcas (A e B, comercializada na cidade de Cartagena das Índias, a presente investigação foi realizada por cromatografia em Fase Sólida, Microextração Headspace Gás com Detector de Captura de Elétrons(HS-SPME-GC/ECD. 36 amostras foram

  20. 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.

  1. Simultaneous optimization by neuro-genetic approach of a multiresidue method for determination of pesticides in Passiflora alata infuses using headspace solid phase microextraction and gas chromatography.

    Science.gov (United States)

    da Silva, Gilmare Antônia; Augusto, Fabio; Poppi, Ronei Jesus

    2007-01-05

    A simultaneous optimization strategy based on neuro-genetic approach has been applied to a HS-SPME-GC-ECD (Headspace Solid Phase Microextraction coupled to Gas Chromatography with Electron Capture Detection) method for simultaneous determination of the pesticides chlorotalonil, methyl parathion, malathion, alpha-endosulfan and beta-endosulfan in herbal infusions of Passiflora alata (Dryander). Two types of extractive fibers were used: a home-made device coated by sol-gel process with polydimethylsiloxane-poly(vinyl alcohol) (PDMS/PVA) and a commercial PDMS. The effects of extraction parameters such as dilution of the infusion, extraction temperature and time, as well as sample ionic strength were evaluated through the Doehlert design. To find a model that could relate these extraction parameters with the extraction efficiency of all pesticide simultaneously, a Bayesian Regularized Artificial Neural Network (BRANN) approach was employed. Subsequently, Genetic Algorithm (GA) was applied to attain the optimum values from the model developed by the neural network. The use of the proposed approach allowed the determination of a single extraction condition that maximized the peak areas of all pesticides simultaneously, showing a promising and a suitable new procedure to the optimization process of complex analytical problems.

  2. Análise de fármacos em material biológico: acoplamento microextração em fase sólida "no tubo" e cromatografia líquida de alta eficiência Analysis of drugs in biological samples: automated "in-tube" solid-phase microextraction and high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Maria Eugênia C. Queiroz

    2005-10-01

    Full Text Available A new solid phase microextraction (SPME system, known as in-tube SPME, was recently developed using an open tubular fused-silica capilary column, instead of an SPME fiber, as the SPME device. On-line in-tube SPME is usually used in combination with high performance liquid chromatography. Drugs in biological samples are directly extracted and concentrated in the stationary phase of capillary columns by repeated draw/eject cycles of sample solution, and then directly transferred to the liquid chromatographic column. In-tube SPME is suitable for automation. Automated sample handling procedures not only shorten the total analysis time, but also usually provide better accuracy and precision relative to manual techniques. In-tube SPME has been demonstrated to be a very effective and highly sensitive technique to determine drugs in biological samples for various purposes such as therapeutic drug monitoring, clinical toxicology, bioavailability and pharmacokinetics.

  3. 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. Copyright © 2016 Elsevier Ltd. All rights reserved.

  4. Volatile compounds of selected strawberry varieties analyzed by purge-and-trap headspace GC-MS.

    Science.gov (United States)

    Hakala, Mari A; Lapveteläinen, Anja T; Kallio, Heikki P

    2002-02-27

    Six strawberry (Fragaria x ananassa Duch.) varieties, Senga Sengana, Jonsok, Polka, Korona, Bounty, and Honeoye, were studied in relation to composition of their volatile headspace compounds collected by dynamic purge-and-trap concentration. Also, the influence of cultivation technique on the volatile compounds was tested by comparing conventionally and organically cultivated strawberry varieties. In addition, the effect of geographical origin on strawberry volatiles was investigated. The emphasis of this study was lay in the industrial utilization of strawberry. A total of 52 different volatile compounds were determined from frozen strawberries grown in 1997 and 1998. In addition to individual compounds, total areas of chromatogram profiles were compared. The major esters were found to be methyl butanoate, ethyl butanoate, methyl hexanoate, and ethyl hexanoate. With the application of principal component analysis and analysis of variance to the data matrix, the varieties were classified into three groups. Var. Honeoye was most different from the others. Organic cultivation had no effect on strawberry volatiles.

  5. Authenticity of raspberry flavor in food products using SPME-chiral-GC-MS

    DEFF Research Database (Denmark)

    Hansen, Anne-Mette Sølvbjerg; Frandsen, Henrik Lauritz; Fromberg, Arvid

    2015-01-01

    A fast and simple method for authenticating raspberry flavors from food products was developed. The two enantiomers of the compound (E)-α-ionone from raspberry flavor were separated on a chiral gas chromatographic column. Based on the ratio of these two enantiomers the naturalness of a raspberry...... flavor can be evaluated due to the fact that a natural flavor will consist almost exclusively of the R enantiomer, while a chemical synthesis of the same compound will result in a racemic mixture. 27 food products containing raspberry flavors where investigated using SPME-chiral-GC-MS. We found raspberry...

  6. Unbiased profiling of volatile organic compounds in the headspace of Allium plants using an in-tube extraction device.

    Science.gov (United States)

    Kusano, Miyako; Kobayashi, Makoto; Iizuka, Yumiko; Fukushima, Atsushi; Saito, Kazuki

    2016-02-29

    Plants produce and emit important volatile organic compounds (VOCs), which have an essential role in biotic and abiotic stress responses and in plant-plant and plant-insect interactions. In order to study the bouquets from plants qualitatively and quantitatively, a comprehensive, analytical method yielding reproducible results is required. We applied in-tube extraction (ITEX) and solid-phase microextraction (SPME) for studying the emissions of Allium plants. The collected HS samples were analyzed by gas chromatography-time-of-flight-mass spectrometry (GC-TOF-MS), and the results were subjected to multivariate analysis. In case of ITEX-method Allium cultivars released more than 300 VOCs, out of which we provisionally identified 50 volatiles. We also used the VOC profiles of Allium samples to discriminate among groups of A. fistulosum, A. chinense (rakkyo), and A. tuberosum (Oriental garlic). As we found 12 metabolite peaks including dipropyl disulphide with significant changes in A. chinense and A. tuberosum when compared to the control cultivar, these metabolite peaks can be used for chemotaxonomic classification of A. chinense, tuberosum, and A. fistulosum. Compared to SPME-method our ITEX-based VOC profiling technique contributes to automatic and reproducible analyses. Hence, it can be applied to high-throughput analyses such as metabolite profiling.

  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. A simple headspace equilibration method for measuring dissolved methane

    Science.gov (United States)

    Magen, C; Lapham, L.L.; Pohlman, John W.; Marshall, Kristin N.; Bosman, S.; Casso, Michael; Chanton, J.P.

    2014-01-01

    Dissolved methane concentrations in the ocean are close to equilibrium with the atmosphere. Because methane is only sparingly soluble in seawater, measuring it without contamination is challenging for samples collected and processed in the presence of air. Several methods for analyzing dissolved methane are described in the literature, yet none has conducted a thorough assessment of the method yield, contamination issues during collection, transport and storage, and the effect of temperature changes and preservative. Previous extraction methods transfer methane from water to gas by either a "sparge and trap" or a "headspace equilibration" technique. The gas is then analyzed for methane by gas chromatography. Here, we revisit the headspace equilibration technique and describe a simple, inexpensive, and reliable method to measure methane in fresh and seawater, regardless of concentration. Within the range of concentrations typically found in surface seawaters (2-1000 nmol L-1), the yield of the method nears 100% of what is expected from solubility calculation following the addition of known amount of methane. In addition to being sensitive (detection limit of 0.1 ppmv, or 0.74 nmol L-1), this method requires less than 10 min per sample, and does not use highly toxic chemicals. It can be conducted with minimum materials and does not require the use of a gas chromatograph at the collection site. It can therefore be used in various remote working environments and conditions.

  9. 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).

  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. 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.

  12. 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).

  13. SPME-Based Ca-History Method for Measuring SVOC Diffusion Coefficients in Clothing Material.

    Science.gov (United States)

    Cao, Jianping; Liu, Ningrui; Zhang, Yinping

    2017-08-15

    Clothes play an important role in dermal exposure to indoor semivolatile organic compounds (SVOCs). The diffusion coefficient of SVOCs in clothing material (D m ) is essential for estimating SVOC sorption by clothing material and subsequent dermal exposure to SVOCs. However, few studies have reported the measured D m for clothing materials. In this paper, we present the solid-phase microextraction (SPME) based C a -history method. To the best of our knowledge, this is the first try to measure D m with known relative standard deviation (RSD). A thin sealed chamber is formed by a circular ring and two pieces of flat SVOC source materials that are tightly covered by the targeted clothing materials. D m is obtained by applying an SVOC mass transfer model in the chamber to the history of gas-phase SVOC concentrations (C a ) in the chamber measured by SPME. D m 's of three SVOCs, di-iso-butyl phthalate (DiBP), di-n-butyl phthalate (DnBP), and tris(1-chloro-2-propyl) phosphate (TCPP), in a cotton T-shirt can be obtained within 16 days, with RSD less than 3%. This study should prove useful for measuring SVOC D m in various sink materials. Further studies are expected to facilitate application of this method and investigate the effects of temperature, relative humidity, and clothing material on D m .

  14. Solid-phase microextraction for the analysis of biological samples

    NARCIS (Netherlands)

    Theodoridis, G; Koster, EHM; de Jong, GJ

    2000-01-01

    Solid-phase microextraction (SPME) has been introduced for the extraction of organic compounds from environmental samples. This relatively new extraction technique has now also gained a lot of interest in a broad field of analysis including food, biological and pharmaceutical samples. SPME has a

  15. Application and exploration of fast gas chromatography-surface acoustic wave sensor to the analysis of thymus species.

    Science.gov (United States)

    Oh, Se Yeon; Ko, Jae Won; Jeong, Seo-Young; Hong, Jongki

    2008-09-26

    Fast gas chromatography combined with surface acoustic wave sensor (GC/SAW) has been applied for the detection of volatile aroma compounds emanated from thymus medicinal plants such as T. quinquecostotus (Jeju and Mt. Gaya in South Korea), T. quinquecostotus var. japonica (Ulreung island in South Korea), T. mongolicus (Northeastern Asia), and T. serpyllum (Europe). The GC/SAW involving the fragrance pattern analysis provides a novel analytical method with a very fast separation and characterization of aromas caused by the delicate difference of chemical composition according to botanical and geographical origin. On the comparison of experiments, the characteristic components and analytical tendency for air-dried thymus species detected by GC/SAW appear to be quite similar to those obtained by headspace solid-phase microextraction (HS-SPME)-GC-MS, but the abundance ratios between these two methods are different. In addition to that, the discrimination of various thymus species by using VaporPrint image based on GC/SAW provides a quite reliable result. On the basis of principal component analysis (PCA) results, the ability for classification among species of completely different chemotypes by HS-SPME-GC-MS is good enough, but the classification of same chemotypes species which are from different geographical origin in same country, original species and its variety, an air-drying term for 13 days and 16 months appear much lower than GC/SAW. Interestingly, the present experiment reveals that the air-drying term influences the aroma composition: the concentration of the pharmacologically active species, monoterpene phenol (thymol), reaches its highest concentrations after it was dried for 5 days or 13 days, which is much higher than in fresh or over-dried for a long times.

  16. Modified headspace solid-phase microextraction for the determination of quantitative relationships between components of mixtures consisting of alcohols, esters, and ethers - impact of the vapor pressure difference of the compounds.

    Science.gov (United States)

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

    2017-07-01

    The quantitative relationship between analytes established by the headspace solid-phase microextraction procedure for multicomponent mixtures depends not only on the character and strength of interactions of individual components with solid-phase microextraction fiber but also on their vapor pressure in the applied headspace solid-phase microextraction system. This study proves that vapor pressure is of minor importance when the sample is dissolved/suspended in a low-volatility liquid of the same physicochemical character as that of the used solid phase microextraction fiber coating. It is demonstrated for mixtures of alcohols, esters, ethers and their selected representatives by applying a headspace solid-phase microextraction system composed of Carbowax fiber and sample solutions in polyethyleneglycol. The observed differences in quantitative relations between components of the examined mixtures established by their direct analysis and by modified headspace solid-phase microextraction are insignificant (F exp  difference between individual components of the examined mixture in the applied headspace solid phase microextraction system due to low components concentration in polyethyleneglycol suspensions (Raoult's law) and due to strong specific interactions of analyte molecules with polyethyleneglycol molecules. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Characterization of Fish Sauce Aroma Impact Compounds Using GC-MS, SPME-Osme-GCO, and Stevens' Power Law Exponents

    Science.gov (United States)

    The objectives of this study were to characterize volatile compounds and to determine the characteristic aromas associated with impact compounds in 4 fish sauces using solid-phase micro-extraction, gas chromatography-mass spectrometry, Osme, and gas chromatography olfactometry (SPME-Osme-GCO) couple...

  18. Use of solid-phase microextraction (SPME) for the determination of methadone and EDDP in human hair by GC-MS.

    Science.gov (United States)

    Lucas, A C; Bermejo, A M; Tabernero, M J; Fernández, P; Strano-Rossi, S

    2000-01-10

    Solid-phase microextraction (SPME) is a new extraction technique with many advantages: small sample volume, simplicity, quickness and solvent-free. It is mainly applied to environmental analysis, but is also useful for the extraction of drugs from biological samples. In this paper the use of SPME is proposed for the determination of methadone and its main metabolite EDDP in hair by GC-MS. The hair samples were washed, cut into 1-mm segments, and incubated with Pronase E for 12 h. A 100-micron polydimethylsiloxane (PDMS) film fibre was submerged for 30 min in a diluted solution of the hydrolysis liquid (1:4 with borax buffer) containing methadone-d3 and EDDP-d3 as internal standards. Once the microextraction was concluded the fibre was directly inserted into the CG injection port. Linearity was found for methadone and EDDP in the range studied, 1.0-50 ng/mg hair, with correlation coefficients higher than 0.99. Interassay relative standard deviation (R.S.D) was determined to be less than 13.30% for methadone and less than 8.94% for EDDP, at 3.0 and 30.0 ng/mg. Analytical recoveries were close to 100% for both compounds on spiked samples. The method was applied to the analysis of real hair samples from eight patients of a methadone maintenance programme. The concentration of methadone in hair ranged from 2.45 to 78.10 ng/mg, and for EDDP from 0.98 to 7.76 ng/mg of hair.

  19. Comparison of solid-phase microextraction, supercritical fluid extraction, steam distillation, and solvent extraction techniques for analysis of volatile consituents in Fructus Amomi.

    Science.gov (United States)

    Shen, Shun; Sha, Yunfei; Deng, Chunhui; Fu, Daxi; Chen, Jiakuan; Zhang, Xiangmin

    2005-01-01

    Four sampling techniques, solid-phase microextraction (SPME), supercritical fluid extraction (SFE), steam distillation (SD), and solvent extraction (SE), were compared for the analysis of volatile constituents from a traditional Chinese medicine (TCM) of the dried ripe fruit of Fructus Amomi (Sha Ren). A total of 38 compounds were identified by gas chromatography/mass spectrometry. Different SFE and SPME parameters (modifier content, extraction pressure, and temperature for SFE and fibers, extraction temperature, and time for SPME) were studied. The results by SFE and SPME were compared with those obtained by conventional SD and SE methods. The results showed that SFE and SPME are better sample preparation techniques than SD and SE. Due to SFE's requirement for expensive specialized instrumentation, the simplicity, low cost, and speed of SPME make it a more appropriate technique for extraction of volatile constituents in TCMs.

  20. Characterization of wood plastic composites made from landfill-derived plastic and sawdust: Volatile compounds and olfactometric analysis

    International Nuclear Information System (INIS)

    Félix, Juliana S.; Domeño, Celia; Nerín, Cristina

    2013-01-01

    Graphical abstract: This work details the characterization of VOCs of WPC, produced from residual materials which would have landfills as current destination, and evaluates their odor profile. Highlights: ► More than 140 volatile compounds were identified in raw materials and WPC products. ► Markers were related to the thermal degradation, sawdust or coupling agents. ► WPC prototype showed a characteristic odor profile of burnt, sweet and wax-like. ► Aldehydes, carboxylic acids, ketones and phenols were odor descriptors of WPC. - Abstract: Application of wood plastic composites (WPCs) obtained from recycled materials initially intended for landfill is usually limited by their composition, mainly focused on release of volatile organic compounds (VOCs) which could affect quality or human safety. The study of the VOCs released by a material is a requirement for new composite materials. Characterization and quantification of VOCs of several WPC produced with low density polyethylene (LDPE) and polyethylene/ethylene vinyl acetate (PE/EVA) films and sawdust were carried out, in each stage of production, by solid phase microextraction in headspace mode (HS-SPME) and gas chromatography–mass spectrometry (GC–MS). An odor profile was also obtained by HS-SPME and GC–MS coupled with olfactometry analysis. More than 140 compounds were observed in the raw materials and WPC samples. Some quantified compounds were considered WPC markers such as furfural, 2-methoxyphenol, N-methylphthalimide and 2,4-di-tert-butylphenol. Hexanoic acid, acetic acid, 2-methoxyphenol, acetylfuran, diacetyl, and aldehydes were the most important odorants. None of the VOCs were found to affect human safety for use of the WPC

  1. Characterization of wood plastic composites made from landfill-derived plastic and sawdust: Volatile compounds and olfactometric analysis

    Energy Technology Data Exchange (ETDEWEB)

    Félix, Juliana S., E-mail: jfelix@unizar.es [Department of Analytical Chemistry, I3A, EINA, University of Zaragoza (UNIZAR), Zaragoza 50018 (Spain); Domeño, Celia, E-mail: cdomeno@unizar.es [Department of Analytical Chemistry, I3A, EINA, University of Zaragoza (UNIZAR), Zaragoza 50018 (Spain); Nerín, Cristina, E-mail: cnerin@unizar.es [Department of Analytical Chemistry, I3A, EINA, University of Zaragoza (UNIZAR), Zaragoza 50018 (Spain)

    2013-03-15

    Graphical abstract: This work details the characterization of VOCs of WPC, produced from residual materials which would have landfills as current destination, and evaluates their odor profile. Highlights: ► More than 140 volatile compounds were identified in raw materials and WPC products. ► Markers were related to the thermal degradation, sawdust or coupling agents. ► WPC prototype showed a characteristic odor profile of burnt, sweet and wax-like. ► Aldehydes, carboxylic acids, ketones and phenols were odor descriptors of WPC. - Abstract: Application of wood plastic composites (WPCs) obtained from recycled materials initially intended for landfill is usually limited by their composition, mainly focused on release of volatile organic compounds (VOCs) which could affect quality or human safety. The study of the VOCs released by a material is a requirement for new composite materials. Characterization and quantification of VOCs of several WPC produced with low density polyethylene (LDPE) and polyethylene/ethylene vinyl acetate (PE/EVA) films and sawdust were carried out, in each stage of production, by solid phase microextraction in headspace mode (HS-SPME) and gas chromatography–mass spectrometry (GC–MS). An odor profile was also obtained by HS-SPME and GC–MS coupled with olfactometry analysis. More than 140 compounds were observed in the raw materials and WPC samples. Some quantified compounds were considered WPC markers such as furfural, 2-methoxyphenol, N-methylphthalimide and 2,4-di-tert-butylphenol. Hexanoic acid, acetic acid, 2-methoxyphenol, acetylfuran, diacetyl, and aldehydes were the most important odorants. None of the VOCs were found to affect human safety for use of the WPC.

  2. Use of solid phase microextraction (SPME) for profiling the volatile metabolites produced by Glomerella cingulata.

    Science.gov (United States)

    Miyazawa, Mitsuo; Kimura, Minako; Yabe, Yoshito; Tsukamoto, Daisuke; Sakamoto, Masaya; Horibe, Isao; Okuno, Yoshiharu

    2008-01-01

    The profile of volatile organic compounds (VOCs) released from Glomerella cingulata using solid phase microextraction (SPME) with different fibers, Polydimethylsiloxane (PDMS), Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), Carboxen/Polydimethylsiloxane (CAR/PDMS) and Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), was investigated. C4-C6 aliphatic alcohols were the predominant fraction of VOCs isolated by CAR/PDMS fiber. Sesquiterpene hydrocarbons represented 20.3% of VOCs isolated by PDMS fiber. During the growth phase, Ochracin was produced in the large majority of VOCs. 3-Methylbutanol and phenylethyl alcohol were found in the log phase of it. Alcohols were found in cultures of higher age, while sesquiterpenes were found to be characteristic of initial growth stage of G. cingulata.

  3. Volatiles in Breath and Headspace Analysis - Diagnostic Markers

    Science.gov (United States)

    2017-07-24

    Tuberculosis; Gastric Cancer; Peptic Ulcer; Atrophic Gastritis; Intestinal Metaplasia; Gastric Dysplasia; Colorectal Cancer; Colorectal Polyp; Colorectal Adenoma; Pancreatic Cancer; Pancreatitis, Chronic; Liver Cancer; Liver Cirrhosis; Flu, Human; Other Infectious Diseases; Inflammatory Bowel Diseases

  4. Usefulness of a PARAFAC decomposition in the fiber selection procedure to determine chlorophenols by means SPME-GC-MS.

    Science.gov (United States)

    Morales, Rocío; Cruz Ortiz, M; Sarabia, Luis A

    2012-05-01

    In this work, a procedure based on solid-phase microextraction and gas chromatography coupled with mass spectrometry is proposed to determine chlorophenols in water without derivatization. The following chlorophenols are studied: 2,4-dichlorophenol; 2,4,6-trichlorophenol; 2,3,4,6-tetrachlorophenol and pentachlorophenol. Three kinds of SPME fibers, polyacrylate, polydimethylsiloxane, and polydimethylsiloxane/divinylbenzene are compared to identify the most suitable one for the extraction process on the basis of two criteria: (a) to select the equilibrium time studying the kinetics of the extraction, and (b) to obtain the best values of the figures of merit. In both cases, a three-way PARAllel FACtor analysis decomposition is used. For the first step, the three-way experimental data are arranged as follows: if I extraction times are considered, the tensor of data, X, of dimensions I × J × K is generated by concatenating the I matrices formed by the abundances of the J m/z ions recorded in K elution times around the retention time for each chlorophenol. The second-order property of PARAFAC (or PARAFAC2) assesses the unequivocal identification of each chlorophenol, as consequence, the loadings in the first mode estimated by the PARAFAC decomposition are the kinetic profile. For the second step, a calibration based on a PARAFAC decomposition is used for each fiber. The best figures of merit were obtained with PDMS/DVB fiber. The values of decision limit, CCα, achieved are between 0.29 and 0.67 μg L(-1) for the four chlorophenols. The accuracy (trueness and precision) of the procedure was assessed. This procedure has been applied to river water samples.

  5. 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.

  6. Investigation of carbon-based nanomaterials as sorbents for headspace in-tube extraction of polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Osorio Barajas, Xochitli L; Hüffer, Thorsten; Mettig, Pascal; Schilling, Beat; Jochmann, Maik A; Schmidt, Torsten C

    2017-06-01

    Carbon-based nanomaterials (CNM) represent promising materials for the application as sorbents in micro- and other extraction devices. In this work, we investigate the applicability of five different CNM (multi-walled carbon nanotubes (MWCNTs), fullerenes, carboxylic acid functionalized multi-walled carbon nanotubes (MWCNTs-COOH), graphene platelets, and carbon nanohorns) for their performance on PAH extraction from the aqueous phase by headspace in-tube extraction (HS-ITEX). Optimal extraction parameters for HS-ITEX were determined using a Box-Behnken experimental design. From the extraction yield response, central point analysis, fullerenes showed the best extraction properties for the eight selected headspace compatible PAHs (naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, and pyrene). Fullerenes were used for a further method validation including the linear range, limit of detection, precision, as well as recovery. Finally, extraction yields were compared to a commercial material (Tenax GR), demonstrating that fullerene represents a better option as sorbent in ITEX for PAH analysis. Method detection limits for the PAH on fullerene ranged from 10 to 300 ng L -1 , with recoveries between 45 and 103%.

  7. Fingerprinting of the volatile fraction from selected thyme species by means of headspace gas chromatography with mass spectrometric detection.

    Science.gov (United States)

    Staszek, Dorota; Orłowska, Marta; Rzepa, Józef; Wróbel, Michał S; Kowalska, Teresa; Szymczak, Grażyna; Waksmundzka-Hajnos, Monika

    2014-01-01

    The Thymus genus has a firm position in Mediterranean folk medicine and culinary tradition, and yet certain confusion is observed in its botanical taxonomy. Therefore, chemical analysis of secondary metabolites and selection of reliable chemotaxonomic markers can prove helpful. In this study, the volatile fraction derived from 20 different thyme specimens was analyzed by means of headspace GC with MS detection. From the obtained chromatographic fingerprints, the diversity of the volatile fraction originating from the different thyme species clearly emerged. Identification of volatile components was based on a software library of mass spectra. There was only one common component derived from all 20 investigated thyme species, i.e., ß-linalool. For three different Thymus species, a comparison was made of the performance of the headspace extraction and hydrodistillation. Characteristic differences in composition of the volatile fraction obtained with use of these two techniques were discussed. Finally, the obtained chromatographic fingerprints of the volatile fraction were analyzed by means of a chemometric approach (principal component analysis), in order to trace similarities in their chemical composition.

  8. Tank Vapor Characterization Project: Headspace vapor characterization of Hanford Waste Tank 241-S-109: Results from samples collected on 06/04/96

    International Nuclear Information System (INIS)

    Pool, K.H.; Thomas, B.L.; Evans, J.C.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-S-109 (Tank S-109) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, on sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in Table S.1. Detailed descriptions of the analytical results appear in the appendices

  9. Tank Vapor Characterization Project. Headspace vapor characterization of Hanford Waste Tank AX-102: Results from samples collected on June 27, 1995

    Energy Technology Data Exchange (ETDEWEB)

    Clauss, T.W.; Pool, K.H.; Evans, J.C.; McVeety, B.D.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Ligotke, M.W.

    1995-11-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-AX-102 (Tank AX-102) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank-farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest Laboratory (PNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. Detailed descriptions of the analytical results appear in the text.

  10. Tank Vapor Characterization Project: Headspace vapor characterization of Hanford Waste Tank U-204, Results from samples collected on August 8, 1995

    International Nuclear Information System (INIS)

    Clauss, T.W.; Evans, J.C.; McVeety, B.D.; Pool, K.H.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Ligotke, M.W.

    1995-11-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-U-204 (Tank U-204) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank-farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. A summary of the results is listed. Detailed descriptions of the analytical results appear in the text

  11. Tank Vapor Characterization Project. Headspace vapor characterization of Hanford Waste Tank AX-102: Results from samples collected on June 27, 1995

    International Nuclear Information System (INIS)

    Clauss, T.W.; Pool, K.H.; Evans, J.C.; McVeety, B.D.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Ligotke, M.W.

    1995-11-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-AX-102 (Tank AX-102) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank-farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest Laboratory (PNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. Detailed descriptions of the analytical results appear in the text

  12. Quantitative analysis of free and bonded forms of volatile sulfur compouds in wine. Basic methodologies and evidences showing the existence of reversible cation-complexed forms.

    Science.gov (United States)

    Franco-Luesma, Ernesto; Ferreira, Vicente

    2014-09-12

    This paper examines first some basic aspects critical to the analysis of Volatile Sulfur Compounds (VSCs), such as the analytical characteristics of the GC-pFPD system and the stability of the different standard solutions required for a proper calibration. Following, a direct static headspace analytical method for the determination of exclusively free forms of VSCs has been developed. Method repeatability is better than 4%, detection limits for main analytes are below 0.5μgL(-1), and the method dynamic linear range (r(2)>0.99) is expanded by controlling the split ratio in the chromatographic inlet to cover the natural range of occurrence of these compounds in wines. The method gives reliable estimates of headspace concentrations but, as expected, suffers from strong matrix effects with recoveries ranging from 0 to 100% or from 60 to 100 in the cases of H2S and the other mercaptans, respectively. This demonstrates the existence of strong interactions of these compounds with different matrix components. The complexing ability of Cu(2+) and to a lower extent Fe(2+) and Zn(2+) has been experimentally checked. A previously developed method in which the wine is strongly diluted with brine and the volatiles are preconcentrated by HS-SPME, was found to give a reliable estimation of the total amount (free+complexed) of mercaptans, demonstrating that metal-mercaptan complexes are reversible. The comparative analysis of different wines by the two procedures reveals that in normal wines H2S and methanethiol can be complexed at levels above 99%, with averages around 97% for H2S and 75% for methanethiol, while thioethers such as dimethyl sulfide (DMS) are not complexed. Overall, the proposed strategy may be generalized to understand problems caused by VSCs in different matrices. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Headspace vapor characterization of Hanford Waste Tank 241-BY-108: Results from samples collected January 23, 1996. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Pool, K.H.; Evans, J.C.; Thomas, B.L.; Olsen, K.B.

    1996-07-01

    This report describes the results of vapor samples obtained to compare vapor sampling of the tank headspace using the Vapor Sampling System (VSS) and In Situ Vapor Sampling System (ISVS) with and without particulate prefiltration. Samples were collected from the headspace of waste storage tank 241-BY-108 (Tank BY-108) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) was contracted by Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for water, ammonia, permanent gases, total nonmethane hydrocarbons (TNMHCs, also known as TO-12), and organic analytes in samples collected in SUMMA trademark canisters and on triple sorbent traps (TSTs) from the tank headspace. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sampling and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Sampling and Analysis Plan for Tank Vapor Sampling Comparison Testclose quotes, and the sample jobs were designated S6004, S6005, and S6006. Samples were collected by WHC on January 23, 1996, using the VSS, a truck-based sampling method using a heated probe; and the ISVS with and without particulate prefiltration

  14. Headspace vapor characterization of Hanford Waste Tank 241-S-102: Results from samples collected on January 26, 1996. Tank Vapor Characterization Project

    International Nuclear Information System (INIS)

    Evans, J.C.; Thomas, B.L.; Pool, K.H.

    1996-07-01

    This report describes the results of vapor samples obtained to compare vapor sampling of the tank headspace using the Vapor Sampling System (VSS) and In Situ Vapor Sampling System (ISVS) with and without particulate prefiltration. Samples were collected from the headspace of waste storage tank 241-S-102 (Tank S-102) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) was contracted by Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for water, ammonia, permanent gases, total nonmethane hydrocarbons (TNMHCs, also known as TO-12), and organic analytes in samples collected in SUMMA trademark canisters and on triple sorbent traps (TSTs) from the tank headspace. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sampling and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was open-quotes Sampling and Analysis Plan for Tank Vapor Sampling Comparison Test close-quote, and the sample jobs were designated S6007, S6008, and S6009. Samples were collected by WHC on January 26, 1996, using the VSS, a truck-based sampling method using a heated probe; and the ISVS with and without particulate prefiltration

  15. Determination of residual acetone and acetone related impurities in drug product intermediates prepared as Spray Dried Dispersions (SDD) using gas chromatography with headspace autosampling (GCHS).

    Science.gov (United States)

    Quirk, Emma; Doggett, Adrian; Bretnall, Alison

    2014-08-05

    Spray Dried Dispersions (SDD) are uniform mixtures of a specific ratio of amorphous active pharmaceutical ingredient (API) and polymer prepared via a spray drying process. Volatile solvents are employed during spray drying to facilitate the formation of the SDD material. Following manufacture, analytical methodology is required to determine residual levels of the spray drying solvent and its associated impurities. Due to the high level of polymer in the SDD samples, direct liquid injection with Gas Chromatography (GC) is not a viable option for analysis. This work describes the development and validation of an analytical approach to determine residual levels of acetone and acetone related impurities, mesityl oxide (MO) and diacetone alcohol (DAA), in drug product intermediates prepared as SDDs using GC with headspace (HS) autosampling. The method development for these analytes presented a number of analytical challenges which had to be overcome before the levels of the volatiles of interest could be accurately quantified. GCHS could be used after two critical factors were implemented; (1) calculation and application of conversion factors to 'correct' for the reactions occurring between acetone, MO and DAA during generation of the headspace volume for analysis, and the addition of an equivalent amount of polymer into all reference solutions used for quantitation to ensure comparability between the headspace volumes generated for both samples and external standards. This work describes the method development and optimisation of the standard preparation, the headspace autosampler operating parameters and the chromatographic conditions, together with a summary of the validation of the methodology. The approach has been demonstrated to be robust and suitable to accurately determine levels of acetone, MO and DAA in SDD materials over the linear concentration range 0.008-0.4μL/mL, with minimum quantitation limits of 20ppm for acetone and MO, and 80ppm for DAA. Copyright

  16. Comparative analysis of volatiles difference of Yunnan sun-dried Pu-erh green tea from different tea mountains: Jingmai and Wuliang mountain by chemical fingerprint similarity combined with principal component analysis and cluster analysis.

    Science.gov (United States)

    Wu, Yuanshuang; Lv, Shidong; Wang, Chen; Gao, Xuemei; Li, Jiangbing; Meng, Qingxiong

    2016-01-01

    Modern instrumental analysis technology can provide various chemical data and information on tea samples. Unfortunately, it remains difficult to extract the useful information. We describe the use of chemical fingerprint similarities, combined with principal component and cluster analyses, to distinguish and recognize Pu-erh green teas, which from two tea mountains, Wuliang and Jingmai, in the Pu-erh district of Yunnan province. The volatile components of all 20 Pu-erh green teas (10 Wuliang and 10 Jingmai teas) were extracted and identified by headspace solid-phase micro extraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS). Sixty-three volatiles (including alcohols, hydrocarbons, ketones, and aldehydes) were identified in the 20 Pu-erh green teas, and differences in compound compositions between them were also observed. Through fingerprint similarity, combined with principal component and cluster analyses, the 20 Pu-erh green teas were differentiated successfully based on their volatile characteristics. This study demonstrates that the GC-MS combined with chemical fingerprint and unsupervised pattern recognition method is suitable for the investigation of the volatile profiling and evaluating the quality and authenticity of teas related to the different origins.Graphical abstractDifferentiate Pu-erh green teas from different tea mountains by using chemical fingerprint similarity and multivariate statistical methods.

  17. Headspace vapor characterization of Hanford waste tank 241-U-109: Results from samples collected on 8/10/95

    International Nuclear Information System (INIS)

    Evans, J.C.; Thomas, B.L.; Pool, K.H.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1996-05-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-U-109 (Tank U-109) At the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. This tank is on the Hydrogen Waste List. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases and total non-methane hydrocarbons is listed in a table. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples is also listed in the table. Detailed descriptions of the analytical results appear in the text

  18. Determination of volatile organic compounds in eucalyptus fast pyrolysis bio-oil by full evaporation headspace gas chromatography.

    Science.gov (United States)

    Kosinski Lima, Nathalya; Romualdo Lopes, André; Gimenes Guerrero, Palimecio; Itsuo Yamamoto, Carlos; Augusto Hansel, Fabricio

    2018-01-01

    This paper reports a full evaporation (FE) headspace gas chromatographic (HS-GC) method for the determination of the volatile organic compounds (VOCs) in bio-oil (i.e. methanol, ethanol, acetone, acetic acid and furfural). The method uses a 4μL sample of bio-oil in a headspace vial (ca. 20mL). Complete evaporation of the compounds was achieved after seven minutes at 90°C. The method showed good precision and accuracy for methanol, ethanol, acetone and acetic acid. The recovery of furfural was low (74.3%). The results showed that the protocol can be applied for the determination of methanol, ethanol, acetone and acetic acid in bio-oil. Detection limits ranged from 0.13 to 0.16μg. Acetic acid was the dominant analyte in the heavy bio-oil and light bio-oil analysis (113. 3 and 85.1µgmg -1 , respectively), followed by methanol, ethanol, and acetone. The polymerisation of furfural was suspected as the cause of its poor quantification. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. SPME-based air sampling method for inhalation exposure assessment studies: case study on perchlorethylene exposure in dry cleaning.

    Science.gov (United States)

    Zare Sakhvidi, Mohammad Javad; Bahrami, Abdul Rahman; Ghiasvand, Alireza; Mahjub, Hossein; Tuduri, Ludovic

    2013-06-01

    Exposure to perchlorethylene, especially for dry cleaning workers and for people living near dry cleaning shops, could lead to several diseases and disorders. This study examines the value of solid-phase microextraction (SPME) for sampling perchlorethylene in the atmosphere of dry cleaning shops. Carboxen/polydimethylsiloxane (CAR/PDMS) in 0.5-cm retracted mode was selected. There were no significant differences between sampling rates at different temperatures (range of 20 to 30 °C) and air velocities (2 to 50 cm/s). On the opposite, relative humidity (RH) had a significant effect on sampling rates. Method reproducibility was realized in the laboratory and field conditions and was 6.2 % and 7 to 11 %, respectively. Repeatability was also determined as 8.9 %. Comparison of the results according to the American Industrial Hygiene Association exposure assessment strategy showed the SPME sampler yields more conservative results in comparison with traditional standard method.

  20. 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. Copyright © 2011 Elsevier B.V. All rights reserved.

  1. Utilization of long duration high-volume sampling coupled to SPME-GC-MS/MS for the assessment of airborne pesticides variability in an urban area (Strasbourg, France) during agricultural application.

    Science.gov (United States)

    Liaud, Céline; Brucher, Michel; Schummer, Claude; Coscollà, Clara; Wolff, Hélène; Schwartz, Jean-Jacques; Yusà, Vicent; Millet, Maurice

    2016-10-02

    Atmospheric samples have been collected between 14 March and 12 September 2012 on a 2-week basis (15 days of sampling and exchange of traps each 7 days) in Strasbourg (east of France) for the analysis of 43 pesticides. Samples (particle and gas phases) were separately extracted using Accelerated Solvent Extraction (ASE) and pre-concentrated by Solid Phase Micro-Extraction (SPME) before analysis by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). Four SPME consecutive injections at distinct temperatures were made in order to increase the sensitivity of detection for the all monitored pesticides. Currently used detected pesticides can be grouped in four classes; those used in maize crops (acetochlor, benoxacor, dicamba, s-metolachlor, pendimethalin, and bromoxynil), in cereal crops (benoxacor, chlorothalonil, fenpropimorph, and propiconazole), in vineyards (tebuconazole), and as herbicides for orchards, meadows of green spaces (2,4-MCPA, trichlopyr). This is in accordance with the diversity of crops found in the Alsace region and trends observed are in accordance with the period of application of these pesticides. Variations observed permit also to demonstrate that the long time sampling duration used in this study is efficient to visualize temporal variations of airborne pesticides concentrations. Then, long time high-volume sampling could be a simple method permitting atmospheric survey of atmospheric contamination without any long analysis time and consequently low cost.

  2. Headspace single drop microextraction versus dispersive liquid-liquid microextraction using magnetic ionic liquid extraction solvents.

    Science.gov (United States)

    An, Jiwoo; Rahn, Kira L; Anderson, Jared L

    2017-05-15

    A headspace single drop microextraction (HS-SDME) method and a dispersive liquid-liquid microextraction (DLLME) method were developed using two tetrachloromanganate ([MnCl 4 2- ])-based magnetic ionic liquids (MIL) as extraction solvents for the determination of twelve aromatic compounds, including four polyaromatic hydrocarbons, by reversed phase high-performance liquid chromatography (HPLC). The analytical performance of the developed HS-SDME method was compared to the DLLME approach employing the same MILs. In the HS-SDME approach, the magnetic field generated by the magnet was exploited to suspend the MIL solvent from the tip of a rod magnet. The utilization of MILs in HS-SDME resulted in a highly stable microdroplet under elevated temperatures and long extraction times, overcoming a common challenge encountered in traditional SDME approaches of droplet instability. The low UV absorbance of the [MnCl 4 2- ]-based MILs permitted direct analysis of the analyte enriched extraction solvent by HPLC. In HS-SDME, the effects of ionic strength of the sample solution, temperature of the extraction system, extraction time, stir rate, and headspace volume on extraction efficiencies were examined. Coefficients of determination (R 2 ) ranged from 0.994 to 0.999 and limits of detection (LODs) varied from 0.04 to 1.0μgL -1 with relative recoveries from lake water ranging from 70.2% to 109.6%. For the DLLME method, parameters including disperser solvent type and volume, ionic strength of the sample solution, mass of extraction solvent, and extraction time were studied and optimized. Coefficients of determination for the DLLME method varied from 0.997 to 0.999 with LODs ranging from 0.05 to 1.0μgL -1 . Relative recoveries from lake water samples ranged from 68.7% to 104.5%. Overall, the DLLME approach permitted faster extraction times and higher enrichment factors for analytes with low vapor pressure whereas the HS-SDME approach exhibited better extraction efficiencies for

  3. Volatiles profiling in medicinal licorice roots using steam distillation and solid-phase microextraction (SPME) coupled to chemometrics.

    Science.gov (United States)

    Farag, Mohamed A; Wessjohann, Ludger A

    2012-11-01

    Licorice (Glycyrrhiza glabra L.) is a plant of considerable commercial importance in traditional medicine and for the flavor and sweets industry. Although Glycyrrhiza species are very competitive targets for phytochemical studies, very little is known about the volatiles composition within that genus, although such knowledge can be suspected to be relevant for understanding the olfactory and taste properties. To provide insight into Glycyrrhiza species aroma composition and for its use in food and pharmaceutical industry, volatile constituents from G. glabra, G. inflata, and G. echinata roots were profiled using steam distillation and solid-phase microextraction. Two phenols, thymol and carvacrol, were found exclusively in essential oil and headspace samples of G. glabra, and with highest amounts for samples that originated from Egypt. In G. echinata oil, (2E, 4E)-decadienal (21%) and β-caryophyllene oxide (24%) were found as main constituents, whereas 1α, 10α-epoxyamorpha-4-ene (13%) and β-dihydroionone (8%) predominated G. inflata. Principal component and hierarchical cluster analyses clearly separated G. echinata and G. inflata from G. glabra; with phenolics and aliphatic aldehydes contributing mostly for species segregation. Licorice (Glycyrrhiza glabra) has large economic, nutritional, and medicinal values. The data presented in this article help in licorice quality control analysis to identify G. glabra from its closely allied species. The presence of thymol and carvacrol exclusively in G. glabra suggests that these volatiles could serve as chemotaxonomic markers and also might be considered as potentially relevant for taste. © 2012 Institute of Food Technologists®

  4. 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.

  5. Analysis of volatile compounds of Ilex paraguariensis A. St. - Hil. and its main adulterating species Ilex theizans Mart. ex Reissek and Ilex dumosa Reissek Análise de compostos voláteis de Ilex paraguariensis A. St. - Hil. e suas principais espécies adulterantes Ilex theizans Mart. ex Reissek e Ilex dumosa Reissek

    Directory of Open Access Journals (Sweden)

    Rogério Marcos Dallago

    2011-12-01

    Full Text Available The adulteration of the product Ilex paraguariensis with other Ilex species is a mAjor problem for maté tea producers. In this work, three species of Ilex were evaluated for their volatile composition by headspace solid phase microextraction coupled to gas chromatography and mass spectrum detector (HS-SPME/GC-MS. The adulterating species I. dumnosa and I. theizans Mart. ex Reissek presented a different profile of volatile organic compounds when compared to I. paraguariensis. Aldehydes methyl-butanal, pentanal, hexanal, heptanal and nonanal were detected only in the adulterating species. This result suggests that such compounds are potential chemical markers for identification of adulteration and quality analysis of products based on Ilex paraguariensis.A adulteração do produto Ilex paraguariensis com outras espécies de Ilex é um dos principais problemas dos produtores de erva-mate. Neste trabalho, três espécies de Ilex foram avaliadas quanto à sua composição volátil por microextração em fase sólida acoplada à cromatografia gasosa e detector de espectro de massas (HS-SPME/GC-MS. As espécies adulterantes I. dumnosa e I. theizans Mart. ex Reissek apresentaram um perfil diferente de compostos orgânicos voláteis, quando comparadas com a I. paraguariensis. Os aldeídos metil-butanal, pentanal, hexanal, heptanal e nonanal foram detectados apenas nas espécies adulterantes. Esse resultado sugere que esses compostos químicos são marcadores potenciais para a identificação de adulteração e análise da qualidade dos produtos à base de Ilex paraguariensis.

  6. The utilisation of two detectors for the determination of water in honey using headspace gas chromatography.

    Science.gov (United States)

    Frink, Lillian A; Armstrong, Daniel W

    2016-08-15

    A headspace gas chromatography (HSGC) method was developed for the determination of water content in honey. This method was shown to work with five different honey varieties which had a range of water from 14-16%. It also utilised two different detectors, the thermal conductivity detector (TCD) and the barrier discharge ionisation detector (BID). This method needs no heating pretreatment step as in the current leading method, (i.e. the measurement of refractive index). The solvent-free procedure negates the possibility of solvent-compound interactions as well as solubility limitations, as is common with Karl Fischer titrations. It was also apparent that the classic loss on drying method consistently and substantially produced results that were lower than the correct values. This approach is shown to be rapid, with an analysis time of 4 min when using the TCD detector and under 3 min when utilising the BID detector. HSGC is feasible for the determination of water due to the new PEG-linked geminal dicationic ionic-liquid-coated GC capillary column. In addition it provides accurate and precise determinations of the water content in honey. When using the sensitive BID detector, other trace volatile compounds are observed as well. Copyright © 2016 Elsevier Ltd. All rights reserved.

  7. The analysis of volatile organic compounds biomarkers for lung cancer in exhaled breath, tissues and cell lines.

    Science.gov (United States)

    Wang, Yishan; Hu, Yanjie; Wang, Di; Yu, Kai; Wang, Ling; Zou, Yingchang; Zhao, Cong; Zhang, Xuanlang; Wang, Ping; Ying, Kejing

    2012-01-01

    Volatile organic compounds (VOCs) biomarkers in breath provide a novel, noninvasive and quick approach to diagnosis lung cancer. The aim of the proposed study was to investigate the VOCs biomarkers in exhaled breath for lung cancer. The VOCs in exhaled breath of 88 lung cancer patients, 70 lung benign disease and 85 healthy people were analyzed by Solid Phase Micro Extraction - Gas Chromatography Mass Spectrometry (SPME-GCMS). Three types of lung cancer cells and 18 lung cancer patients' tissues were cultured in vitro. The VOCs in the headspace of these cultivations were analyzed as an evidence of production mechanism of the VOCs in breath. Three lung cancer diagnosis models were constructed respectively in exhaled breath samples using Linear Discriminant Analysis (LDA). Leave one out cross validation was employed to evaluate these models. 23 VOCs, whose areas under curve (AUC) of receiver operating characteristic (ROC) > 0.60 and p < 0.01, were confirmed as the VOCs biomarkers for lung cancer. Three diagnostic models based on 23 VOCs could easily discriminate lung cancer patients from controls with 96.47% sensitivity and 97.47% specificity. However, the discrimination between early stage and later stage lung cancer was not very obvious.

  8. Kainari, a Unique Greek Traditional Herbal Tea, from the Island of Lesvos: Chemical Analysis and Antioxidant and Antimicrobial Properties

    Directory of Open Access Journals (Sweden)

    Evangelia Bampali

    2018-01-01

    Full Text Available The chemical composition, as well as the total phenolic content (TPC and the potential antioxidant and antimicrobial activity, of three Kainari-herbal tea samples from different areas of Lesvos Island (Greece was evaluated. The rich aroma of the mixtures was studied through GC-MS, as well as through Headspace Solid-Phase Microextraction (HS-SPME/GC-MS analyses. Cinnamon, clove, nutmeg, pepper, and ginger were identified as main ingredients, while, throughout the chemical analysis of the volatiles of one selected sample, several secondary metabolites have been isolated and identified on the basis of GC-MS as well as spectral evidence as eugenol, cinnamic aldehyde and myristicin, cinnamyl alcohol, alpha-terpinyl acetate, and β-caryophyllene. Furthermore, two food dyes, azorubine and amaranth, were also isolated and identified from the infusions. The total phenolic content was estimated and the free radical scavenging activity was determined by DPPH and ABTS assays and the antimicrobial activity of the extracts was tested showing a very interesting profile against all the assayed microorganisms. Due to its very pleasant aroma and taste properties as well as to its bioactivities, Kainari-herbal tea could be further proposed as functional beverage.

  9. 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

    scale tended to give a greater accuracy of scored odor intensity. The color-graded brightness scale may strengthen the repeatability of the intensity measures due to the cross-modal support in the judgment processes. The method allows the conversion of intensity judgment of a package headspace...... 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......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...

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

    International Nuclear Information System (INIS)

    He Yi; Vargas, Angelica; Kang, Youn-Jung

    2007-01-01

    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 3 PO 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 μg L -1 , repeatability of the extraction (R.S.D. -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

  11. Prediction of sensory properties of Brazilian Arabica roasted coffees by headspace solid phase microextraction-gas chromatography and partial least squares.

    Science.gov (United States)

    Ribeiro, J S; Augusto, F; Salva, T J G; Thomaziello, R A; Ferreira, M M C

    2009-02-23

    Volatile compounds in fifty-eight Arabica roasted coffee samples from Brazil were analyzed by SPME-GC-FID and SPME-GC-MS, and the results were compared with those from sensory evaluation. The main purpose was to investigate the relationships between the volatile compounds from roasted coffees and certain sensory attributes, including body, flavor, cleanliness and overall quality. Calibration models for each sensory attribute based on chromatographic profiles were developed by using partial least squares (PLS) regression. Discrimination of samples with different overall qualities was done by using partial least squares-discriminant analysis (PLS-DA). The alignment of chromatograms was performed by the correlation optimized warping (COW) algorithm. Selection of peaks for each regression model was performed by applying the ordered predictors selection (OPS) algorithm in order to take into account only significant compounds. The results provided by the calibration models are promising and demonstrate the feasibility of using this methodology in on-line or routine applications to predict the sensory quality of unknown Brazilian Arabica coffee samples. According to the PLS-DA on chromatographic profiles of different quality samples, compounds 3-methypropanal, 2-methylfuran, furfural, furfuryl formate, 5-methyl-2-furancarboxyaldehyde, 4-ethylguaiacol, 3-methylthiophene, 2-furanmethanol acetate, 2-ethyl-3,6-dimethylpyrazine, 1-(2-furanyl)-2-butanone and three others not identified compounds can be considered as possible markers for the coffee beverage overall quality.

  12. 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.

  13. Determination of Cinnamaldehyde in Cinnamon by SPME-GC-MS: An Instrumental Analysis Experiment

    Science.gov (United States)

    Wang, Yimin; Ocariz, Jessica; Hammersand, Jennifer; MacDonald, Evan; Bartczak, Ashley; Kero, Frank; Young, Vaneica Y.; Williams, Kathryn R.

    2008-01-01

    Students analyze "trans"-cinnamaldehyde in commercial cinnamon using solid-phase microextraction and GC-MS with ethyl benzoate as the internal standard. Aside from the instrumentation, the experiment utilizes readily available low hazard materials and can be completed within one four-hour laboratory period. (Contains 2 figures.)

  14. Headspace solid-phase microextraction-gas chromatography-mass spectrometry applied to quality control in multilayer-packaging manufacture.

    Science.gov (United States)

    Ezquerro, Oscar; Pons, Begoña; Tena, María Teresa

    2003-08-01

    A method based on headspace solid-phase microextraction-gas chromatography-mass spectrometry is proposed for the quality control of multilayer packaging and its manufacturing process. Volatile organic compounds (VOCs) are produced in the manufacturing process of the packaging. They can cause organoleptic problems or modify the properties of the packaging depending on the nature and the amount of the VOCs formed. The quantification using packaging samples with a known VOC concentration for the calibration is proposed in order to reduce the analysis time, and the method is validated using a statistical test. Finally, the method is applied to the determination of odour-responsible compounds in multilayer packaging samples obtained under different extrusion-coating conditions, i.e. type of extruder, type of polymer and extrusion speed.

  15. Comparação entre injeção na coluna ("on-column" e headspace dinâmico na determinação de benzeno, tolueno e xilenos (BTX em amostras de água

    Directory of Open Access Journals (Sweden)

    Gobato Elaine A. A. F.

    2001-01-01

    Full Text Available The analysis of water samples containing volatile organic compounds has become an important task in analytical chemistry. Gas chromatography has been widely used for the analysis of volatile organic compounds in water. The headspace analysis shows as a principal characteristic the possibility of determination of the volatile components in drinking water. Benzene, Toluene and Xylene (BTX are important compounds usually present in drinking water, from contamination by petroleum derivatives. Since they are toxic compounds even when present in low concentration levels, their determination is important in order to define the quality of the water. The sampling technique using headspace, coupled with gas chromatography as the separation method, showed to be suitable for BTX analysis in several samples at the mug/L (ppb level.

  16. Tank 241-U-107 headspace gas and vapor characterization results for samples collected in February 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    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. Determination of carboxyl groups in wood fibers by headspace gas chromatography

    Science.gov (United States)

    X.-S. Chai; Q.X. Hou; J.Y. Zhu; S.-L. Chen; S.F. Wang; L. Lucia

    2003-01-01

    The phase reaction conversion (PRC) headspace gas chromatographic (HSGC) technique was employed to develop a method for the determination of the content of carboxyl groups in wood fibers. Acid treatment of the wood fibers using hydrochloric was applied to convert carboxyl groups to carboxyl acids. Bicarbonate solution is then used to react with carboxyl acids on the...

  18. Tank 241-AX-102 headspace gas and vapor characterization results for samples collected in June 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-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

  20. Tank 241-B-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

  1. Tank 241-T-107 Headspace Gas and Vapor Characterization Results for Samples Collected in January 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

  2. Tank 241-C-104 headspace gas and vapor characterization results for samples collected in March 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)

    1995-09-28

    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

  3. Tank 241-C-107 headspace gas and vapor characterization results for samples collected in 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)

    1995-09-28

    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

  4. Tank 241-U-106 headspace gas and vapor characterization results for samples collected in March 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    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. Tank 241-S-102 headspace gas and vapor characterization results for samples collected in March 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    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

  6. Tank 241-U-111 headspace gas and vapor characterization results for samples collected in February 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    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

  7. Tank 241-TX-105 headspace gas and vapor characterization results for samples collected in December 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)

    1995-09-25

    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

  8. Tank 241-T-111 headspace gas and vapor characterization results for samples collected in January 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    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

  9. Tank 241-AX-102 headspace gas and vapor characterization results for samples collected in June 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    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

  10. Tank 241-A-101 headspace gas and vapor characterization results for samples collected in June 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    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

  11. Tank 241-U-203 headspace gas and vapor characterization results for samples collected in August 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    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

  12. Tank 241-C-106 headspace gas and vapor characterization results for samples collected in February 1994

    International Nuclear Information System (INIS)

    Hackaby, J.L.; Bratzel, D.R.

    1995-01-01

    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

  13. Tank 241-C-107 headspace gas and vapor characterization results for samples collected in September 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    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. Tank 241-S-111 headspace gas and vapor characterization results for samples collected in March 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    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

  15. Tank 241-BY-112 headspace gas and vapor characterization results for samples collected in November 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    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

  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-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.

  18. Tank 241-C-110 headspace gas and vapor characterization results for samples collected in August 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.

  19. Tank 241-SX-103 headspace gas and vapor characterization results for samples collected in March 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    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-U-103 headspace gas and vapor characterization results for samples collected in February 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    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

  1. Tank 241-SX-106 headspace gas and vapor characterization results for samples collected in March 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    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. Tank 241-C-102 headspace gas and vapor characterization results for samples collected in August 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    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

  3. Tank 241-TX-105 headspace gas and vapor characterization results for samples collected in December 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    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

  4. Tank 241-C-104 headspace gas and vapor characterization results for samples collected in March 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    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. Tank 241-C-110 headspace gas and vapor characterization results for samples collected in August 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    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

  6. Tank 241-B-103 headspace gas and vapor characterization results for samples collected in February 1995

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    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

  7. Tank 241-BX-104 headspace gas and vapor characterization results for samples collected in December 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    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

  8. Tank 241-C-101 headspace gas and vapor characterization results for samples collected in September 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    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

  9. Characterization of volatile components in dry chrysanthemum flowers using headspace-liquid-phase microextraction-gas chromatography.

    Science.gov (United States)

    Wang, Guoqing; Dong, Chunhong; Sun, Yu-an; Xie, Kui; Zheng, Haiyu

    2008-02-01

    A headspace-liquid-phase microextraction (HS-LPME)-GC (gas chromatography) method for the characterization of volatile components in dry chrysanthemum flowers has been developed. In the proposed method, two extraction solvents, n-hexadecane and benzyl alcohol, are used for preconcentrating volatiles in the sample. A droplet of the extraction solvent is squeezed from the GC syringe and inserted in the headspace of the sample bottle with the dry flower, immersed in deionized water, and warmed in a water bath. The optimum HS-LPME parameters in terms of extraction solvent type, droplet magnitude, equilibrium (water bath) temperature, equilibrium time, extraction time, and ionic strength are achieved using GC-FID (flame ionization detection) by varying several levels of the factors that affect the HS-LPME procedure. After extraction under the optimized conditions, the extraction droplet is retracted into the syringe and injected for GC-MS (mass spectrometry) analysis. Thirty-three volatile components are extracted and identified using this HS-LPME-GC-MS method, with the aid of chemometric methods. It is shown that the volatiles in dry chrysanthemum flowers are mainly unsaturated organic compounds, such as monoterpenes, sesquiterpenes and their oxygenous derivatives, triterpenoids, and aliphatic compounds. Several representative components, in order of precedence of the retention time, are pinene (106.3 microg/g), camphene (112.7 microg/g), eucapyptol (52.1 microg/g), camphor (29.4 microg/g), borneol (4.2 microg g), bornyl acetate (67.3 microg/g), caryophyllene (0.7 microg/g), and caryophyllene oxide (20.0 microg/g). The relative standard error and detection limit of this method is 5-9% and 0.4 microg/g, respectively.

  10. An analytical method for trifluoroacetic Acid in water and air samples using headspace gas chromatographic determination of the methyl ester.

    Science.gov (United States)

    Zehavi, D; Seiber, J N

    1996-10-01

    An analytical method has been developed for the determination of trace levels of trifluoroacetic acid (TFA), an atmospheric breakdown product of several of the hydrofluorocarbon (HFC) and hydrochlorofluorocarbon (HCFC) replacements for the chlorofluorocarbon (CFC) refrigerants, in water and air. TFA is derivatized to the volatile methyl trifluoroacetate (MTFA) and determined by automated headspace gas chromatography (HSGC) with electron-capture detection or manual HSGC using GC/MS in the selected ion monitoring (SIM) mode. The method is based on the reaction of an aqueous sample containing TFA with dimethyl sulfate (DMS) in concentrated sulfuric acid in a sealed headspace vial under conditions favoring distribution of MTFA to the vapor phase. Water samples are prepared by evaporative concentration, during which TFA is retained as the anion, followed by extraction with diethyl ether of the acidified sample and then back-extraction of TFA (as the anion) in aqueous bicarbonate solution. The extraction step is required for samples with a relatively high background of other salts and organic materials. Air samples are collected in sodium bicarbonate-glycerin-coated glass denuder tubes and prepared by rinsing the denuder contents with water to form an aqueous sample for derivatization and analysis. Recoveries of TFA from spiked water, with and without evaporative concentration, and from spiked air were quantitative, with estimated detection limits of 10 ng/mL (unconcentrated) and 25 pg/mL (concentrated 250 mL:1 mL) for water and 1 ng/m(3) (72 h at 5 L/min) for air. Several environmental air, fogwater, rainwater, and surface water samples were successfully analyzed; many showed the presence of TFA.

  11. Analysis of volatiles from irradiated yeast extract

    International Nuclear Information System (INIS)

    Liao Tao; Li Xin; Zu Xiaoyan; Chen Yuxia; Geng Shengrong

    2013-01-01

    The method for determination volatiles from irradiated yeast extract (YE) using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) was developed in this paper. The extraction conditions were optimized with reference to the peak area and number of volatiles as aldehyde, ketone, alcohol, acid, ester and sulfur compounds. The optimized conditions of HS-SPME for volatiles in irradiated YE were: divinyl benzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber, extration time 40 min, extraction temperature 40℃. The volatiles from YE irradiated by 0-19.8 kGy were detected using HS-SPME coupled with GC-MS. The results showed that only 15 volatiles were detected from no irradiated YE and main compounds were acetic acid, 2, 3-butanediol and 1-hexanol, 2-ethyl-. There were 40 volatiles detected from irradiated YE and the main compounds were acetic acid, phenylethyl alcohol, heptanal and nonanal. Compare to no irradiated yeast extract, the aldehyde, ketone, alkene and disulfide, dimethyl were produced by irradiating process. (authors)

  12. Headspace volume and percentage of carbon monoxide affects carboxymyoglobin layer development of modified atmosphere packaged beef steaks.

    Science.gov (United States)

    Raines, Christopher R; Hunt, Melvin C

    2010-01-01

    Carboxymyoglobin (COMb) development of beef Longissimus lumborum as related to molecular CO availability and package headspace volume was evaluated. Steaks from six pairs of USDA Select strip loins were packaged in modified atmosphere packages with 0.2%, 0.4%, or 0.8% CO and 30% CO(2) and balanced with N(2) to obtain meat-to-gas ratios of 0.4, 0.7, and 1.1, and CO molar concentrations of 0.07, 0.10, and 0.20 mMol. Steak redness (CIE a*), COMb layer thickness, percentage of CO in the headspace, visual display color, and bloom intensity scores were evaluated 4 and 7 d after packaging. Greater concentration of CO in a smaller headspace resulted in a thicker COMb layer compared with lesser concentration of CO in a larger headspace, regardless of moles CO available. The combined effects of concentration of CO and headspace volume had a greater impact on COMb development than millimoles of CO in the package headspace. Package headspace can be reduced and the concentration of CO can be increased without detriment to fresh beef color or consumer safety.

  13. 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. Copyright © 2012. Published by Elsevier Ltd.

  14. Determination of Pyrethroids in Tea Brew by GC-MS Combined with SPME with Multiwalled Carbon Nanotube Coated Fiber

    Directory of Open Access Journals (Sweden)

    Dongxia Ren

    2018-01-01

    Full Text Available A new method has been developed to simultaneously determine 7 pyrethroid residues in tea brew using gas chromatography-mass spectrometry (GC-MS combined with solid phase microextraction (SPME with multiwalled carbon nanotubes (MWCNTs coated fiber. The MWCNTs coated fiber of SPME was homemade by using stainless steel wire as coating carrier and polyacrylonitrile (PAN solution as adhesive glue. Under the optimized conditions, a good linearity was shown for bifenthrin, fenpropathrin, permethrin, and cyfluthrin in 1–50 ng mL−1 and for cypermethrin, fenvalerate, and deltamethrin in 5–50 ng mL−1. The correlation coefficients were in the range of 0.9948–0.9999. The average recoveries of 7 pyrethroids were 94.2%–107.3% and the relative standard deviations (RSDs were less than 15%. The detection limit of the method ranged from 0.12 to 1.65 ng mL−1. The tea brew samples made from some commercial tea samples were analyzed. Among them, bifenthrin, fenpropathrin, and permethrin were found. The results show that the method is rapid and sensitive and requires low organic reagent consumption, which can be well used for the detection of the pyrethroids in tea brew.

  15. Improving the On-Line Extraction of Polar Compounds by IT-SPME with Silica Nanoparticles Modified Phases

    Directory of Open Access Journals (Sweden)

    Pascual Serra-Mora

    2018-02-01

    Full Text Available In the present work the extraction efficiency of in-tube solid-phase microextraction (IT-SPME for polar herbicides has been evaluated using extractive capillaries coated with different polymeric sorbents. For this purpose, aqueous solutions of herbicides with a wide range of polarities, including some highly polar compounds (log Kow < 1, have been directly processed by IT-SPME coupled on-line to capillary liquid chromatography with UV-diode array detection. For extraction, commercially available capillary columns coated with polydimethylsiloxane (PDMS and polyetilenglicol (PEG-based phases have been used, and the results have been compared with those obtained with a synthesized tetraethyl orthosilicate (TEOS-trimethoxyethylsilane (MTEOS polymer, as well as the same polymer reinforced with silica nanoparticles (SiO2 NPs. The SiO2 NPs functionalized TEOS-MTEOS coating provided the best results for most herbicides, especially for the most polar compounds. On the basis of the results obtained, conditions for the quantification of the herbicides tested are described using a SiO2 NPs reinforced TEOS-MTEOS coated capillary. The proposed method provided satisfactory linearity up to concentrations of 200 μg/L. The precision was also suitable, with relative standard deviations (RSDs values ≤9% (n = 3, and the limits of detection (LODs were within the 0.5–7.5 µg/L range. The method has been applied to different water samples and the extract obtained from an agricultural soil.

  16. Development of an SPME-GC-MS/MS method for the determination of pesticides in rainwater: Laboratory and field experiments

    International Nuclear Information System (INIS)

    Sauret-Szczepanski, Nathalie; Mirabel, Philippe; Wortham, Henri

    2006-01-01

    A solid-phase microextraction - coupled to a gas chromatography - ion trap tandem mass spectrometry (SPME-GC-MS/MS) method was developed for the quantitative determination in rainwater of 8 pesticides amongst the most used in France and 3 triazines metabolites. The main factors affecting the SPME process were studied. Using a 3 mL sample, the method developed showed good linearity for concentrations ranging from 0.05 to 50 μg L -1 with correlation coefficients between 0.997 and 0.9999 and relative standard deviations (% RSD) below 14%. The study of matrix effects showed that rainwater was too diluted to have any significant influence on the extraction efficiency. To validate the method, a field campaign was carried out on the rain events, which occurred in Strasbourg during a one-year period. The rain concentrations showed patterns of high pesticide concentrations during spring months, which were correlated to the spraying periods of most of these substances. - Solid-phase microextraction efficiency of pesticides in rainwater was optimized

  17. Development of an SPME-GC-MS/MS method for the determination of pesticides in rainwater: Laboratory and field experiments

    Energy Technology Data Exchange (ETDEWEB)

    Sauret-Szczepanski, Nathalie [Equipe de Physico-chimie de l' Atmosphere, Centre de Geochimie de la Surface (UMR 7517) 1, rue Blessig, 67084 Strasbourg Cedex (France)]. E-mail: nathalie.sauret-szczepanski@alcan.com; Mirabel, Philippe [Equipe de Physico-chimie de l' Atmosphere, Centre de Geochimie de la Surface (UMR 7517) 1, rue Blessig, 67084 Strasbourg Cedex (France); Wortham, Henri [Universite de Provence, Laboratoire Chimie et Environnement, Case 29, 3 Place Victor Hugo, 13331 Marseille Cedex (France)]. E-mail: wortham@up.univ-mrs.fr

    2006-01-15

    A solid-phase microextraction - coupled to a gas chromatography - ion trap tandem mass spectrometry (SPME-GC-MS/MS) method was developed for the quantitative determination in rainwater of 8 pesticides amongst the most used in France and 3 triazines metabolites. The main factors affecting the SPME process were studied. Using a 3 mL sample, the method developed showed good linearity for concentrations ranging from 0.05 to 50 {mu}g L{sup -1} with correlation coefficients between 0.997 and 0.9999 and relative standard deviations (% RSD) below 14%. The study of matrix effects showed that rainwater was too diluted to have any significant influence on the extraction efficiency. To validate the method, a field campaign was carried out on the rain events, which occurred in Strasbourg during a one-year period. The rain concentrations showed patterns of high pesticide concentrations during spring months, which were correlated to the spraying periods of most of these substances. - Solid-phase microextraction efficiency of pesticides in rainwater was optimized.

  18. Characterization of plant diversity of pastures and volatile organic compound analysis in ewe’s milk from a typical farm system in the Alta Murgia national park (southern Italy: opportunities for a sustainable land use

    Directory of Open Access Journals (Sweden)

    Elena Ciani

    2012-04-01

    Full Text Available In recent years, there has been an increasing interest of consumers in traditional dairy products whose origin from defined geographical areas is guaranteed. These products are appreciated for the distinctive sensorial characteristics, derived by extensive grazing system on natural and artificial pastures and traditional cheese-making techniques. Moreover, a considerable public interest is also attributed to typical dairy products for their role in stimulating the economy of rural areas and in preserving environment and biodiversity. Here we present the results of a survey on the botanical composition of Alta Murgia pastures, together with the analysis of VOCs (volatile organic compounds in milk from ewes reared under a typical farm system in the Alta Murgia National Park (Apulia region, southern Italy. Data from two less ordinary farm systems are also reported as external reference. The botanical composition of pastures was estimated by three modified Whittaker plots placed in the prevailing habitat types. Milk samples were analyzed for VOC compounds by head-space SPME/GC-MS. Consumer acceptance of cheese, made from each milk sample using homogeneous traditional cheese-making techniques, was evaluated. The study provides interesting insights on the floral composition of Alta Murgia pastures and the first characterization of VOC profiles in ewe’s raw milk from Alta Murgia.

  19. Headspace vapor characterization of Hanford Waste Tank 241-U-112: Results from samples collected on 7/09/96

    International Nuclear Information System (INIS)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.; Olsen, K.B.; Fruchter, J.S.; Silvers, K.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-U-112 at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company

  20. Evaluation of in vivo solid phase microextraction for minimally invasive analysis of nonvolatile phytochemicals in Amazonian plants.

    Science.gov (United States)

    Musteata, Florin Marcel; Sandoval, Manuel; Ruiz-Macedo, Juan C; Harrison, Kathleen; McKenna, Dennis; Millington, William

    2016-08-24

    Although solid phase microextraction (SPME) has been used extensively for fingerprinting volatile compounds emitted by plants, there are very few such reports for direct insertion SPME. In this research, direct contact of SPME probes with the interstitial fluid of plants was investigated as a method for phytochemical analysis. Medicinal plants from the Amazon have been the source of numerous drugs used in western medicine. However, a large number of species used in traditional medicine have not been characterized chemically, partly due to the difficulty of field work. In this project, the phytochemical composition of plants from several genera was fingerprinted by combining convenient field sampling by solid phase microextraction (SPME) with laboratory analysis by LC-MS. The new method was compared with classical sampling followed by liquid extraction (LE). SPME probes were prepared by coating stainless steel wires with a mixture of polyacrylonitrile and either RP-amide or HS-F5 silica particles. Sampling was performed by inserting the microextraction probes into various tissues of living plants in their natural environment. After in vivo extraction, the probes were sealed under vacuum and refrigerated until analyzed. The probes were desorbed in mobile phase and analyzed on a Waters Acquity UPLC with triple quadrupole mass spectrometer in positive ion mode. Twenty Amazonian plant species were sampled and unique metabolomic fingerprints were obtained. In addition, quantitative analysis was performed for previously identified compounds in three species. Comparison of the fingerprints obtained by in vivo SPME with those obtained by LE showed that 27% of the chromatographic features were unique to SPME, 57% were unique to LE, and 16% were common to both methods. In vivo SPME caused minimal damage to the plants, was much faster than traditional liquid extraction, and provided unique fingerprints for all investigated plants. SPME revealed unique chromatographic

  1. Effectiveness of Liquid-Liquid Extraction, Solid Phase Extraction, and Headspace Technique for Determination of Some Volatile Water-Soluble Compounds of Rose Aromatic Water.

    Science.gov (United States)

    Canbay, Hale Seçilmiş

    2017-01-01

    Steam distillation is used to isolate scent of rose flowers. Rose aromatic water is commonly used in European cuisine and aromatherapy besides its use in cosmetic industry for its lovely scent. In this study, three different sampling techniques, liquid-liquid extraction (LLE), headspace technique (HS), and solid phase extraction (SPE), were compared for the analysis of volatile water-soluble compounds in commercial rose aromatic water. Some volatile water-soluble compounds of rose aromatic water were also analyzed by gas chromatography mass spectrometry (GCMS). In any case, it was concluded that one of the solid phase extraction methods led to higher recoveries for 2-phenylethyl alcohol (PEA) in the rose aromatic water than the liquid-liquid extraction and headspace technique. Liquid-liquid extraction method provided higher recovery ratios for citronellol, nerol, and geraniol than others. Ideal linear correlation coefficient values were observed by GCMS for quantitative analysis of volatile compounds ( r 2 ≥ 0.999). Optimized methods showed acceptable repeatability (RSDs 95%). For compounds such as α -pinene, linalool, β -caryophyllene, α -humulene, methyl eugenol, and eugenol, the best recovery values were obtained with LLE and SPE.

  2. Effectiveness of Liquid-Liquid Extraction, Solid Phase Extraction, and Headspace Technique for Determination of Some Volatile Water-Soluble Compounds of Rose Aromatic Water

    Directory of Open Access Journals (Sweden)

    Hale Seçilmiş Canbay

    2017-01-01

    Full Text Available Steam distillation is used to isolate scent of rose flowers. Rose aromatic water is commonly used in European cuisine and aromatherapy besides its use in cosmetic industry for its lovely scent. In this study, three different sampling techniques, liquid-liquid extraction (LLE, headspace technique (HS, and solid phase extraction (SPE, were compared for the analysis of volatile water-soluble compounds in commercial rose aromatic water. Some volatile water-soluble compounds of rose aromatic water were also analyzed by gas chromatography mass spectrometry (GCMS. In any case, it was concluded that one of the solid phase extraction methods led to higher recoveries for 2-phenylethyl alcohol (PEA in the rose aromatic water than the liquid-liquid extraction and headspace technique. Liquid-liquid extraction method provided higher recovery ratios for citronellol, nerol, and geraniol than others. Ideal linear correlation coefficient values were observed by GCMS for quantitative analysis of volatile compounds (r2≥0.999. Optimized methods showed acceptable repeatability (RSDs 95%. For compounds such as α-pinene, linalool, β-caryophyllene, α-humulene, methyl eugenol, and eugenol, the best recovery values were obtained with LLE and SPE.

  3. Essential Oil Chemical Composition and Headspace Volatiles Profile of Achillea coarctata from Serbia.

    Science.gov (United States)

    Kostevski, Ivana R; Petrović, Goran M; Stojanović, Gordana S; Stamenković, Jelena G; Zlatković, Bojan K

    2016-04-01

    This study reports the essential oil composition and headspace volatiles profile of Achillea coarctata Poir. from Serbia. The inflorescences, stems and leaves, and the aerial parts of A. coarctata were analyzed separately. Germacrene D, α-terpineol and 1,8-cineole were the main constituents of the aerial parts essential oil; 1,8-cineole, cis-cadin-4-en-7-ol and α-terpineol were the most dominant compounds in the inflorescence essential oil, while the most abundant components in the stem and leaf oil were germacrene D, cis-cadin-4-en-7-ol and ledol. The percentages of monoterpenoids and sesquiterpenoids in the aerial parts were the same, while there were differences in distribution of these compound classes in inflorescence and stem and leaf essential oils. The major components of the headspace volatiles were the same for aerial parts, inflorescence and stem and leaves: 1,8-cineole, β-pinene and α-pinene.

  4. Caracterización de los compuestos del aroma en rones colombianos por HS-SPME-GC-MS-O

    Directory of Open Access Journals (Sweden)

    Jazmín Osorio Monsalve

    2016-11-01

    Full Text Available Se identificaron por primera vez 46 compuestos volátiles olfativamente activos con actividad aromática significativa presentes en rones comerciales de Colombia. Lo anterior, mediante microextracción en fase sólida en modo espacio de cabeza (HS-SPME, acoplada a cromatografía de gases con detectores de espectrometría de masas y olfatometría (GC-MS-O. Dentro de los compuestos identificados se encuentran ésteres, compuestos aromáticos, alcoholes, acetales, lactonas y furfural. De esos 46 compuestos, nueve están presentes en todos los rones estudiados y algunos otros son característicos solo de la marca.

  5. Tank 241-C-111 headspace gas and vapor sample results - August 1993 samples

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1994-01-01

    Tank 241-C-111 is on the ferrocyanide Watch List. Gas and vapor samples were collected to assure safe conditions before planned intrusive work was performed. Sample analyses showed that hydrogen is about ten times higher in the tank headspace than in ambient air. Nitrous oxide is about sixty times higher than ambient levels. The hydrogen cyanide concentration was below 0.04 ppbv, and the average NO x concentration was 8.6 ppmv

  6. Headspace Volumetric Karl Fischer Titration for the Determination of Water Content in Finished Tobacco Products

    OpenAIRE

    Aydin N; Chardonnens F; Rotach M

    2014-01-01

    Because many physicochemical properties of tobacco are highly sensitive to its moisture content, the determination of water level is an important parameter for tobacco characterization. A headspace volumetric Karl Fischer titration (HS-V-KFT) method is presented for the quantification of water content in different finished tobacco materials. The parameters affecting the extraction of water from the tobacco materials were the sample size and the oven temperature which have been optimized. The ...

  7. 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.)

  8. 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.

  9. Determination of methanol in pulp washing filtrates by desiccated full evaporation headspace gas chromatography.

    Science.gov (United States)

    Hu, Hui-Chao; Chai, Xin-Sheng

    2012-01-27

    This paper reports on a desiccated full evaporation headspace gas chromatographic (FE HS-GC) technique for determination of the methanol content in dilute mill effluents. Anhydrous K(2)CO(3) was selected as the preferred salt for eliminating the water in the sample in the headspace sample vial. The results showed that the addition of 12 g K(2)CO(3) made it possible to introduce a larger sample size (up to 1 mL) into the FE HS-GC measurement, thereby increasing the sensitivity of the technique. At the given equilibration temperature (105°C), a near-complete mass transfer of methanol from the liquid phase to vapor phase (headspace) was achieved within 10 min. Replicate samples showed that the relative standard deviation of the method was less than 1.5%. Further, the limit of quantification (LOQ) was 0.12 μg and the recovery ranged from 95 to 104%. The present method greatly improves the methanol detection sensitivity in the FE HS-GC method and has the added advantage of being simple, rapid and accurate. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Simultaneous determination of salicylic, 3-methyl salicylic, 4-methyl salicylic, acetylsalicylic and benzoic acids in fruit, vegetables and derived beverages by SPME-LC-UV/DAD.

    Science.gov (United States)

    Aresta, Antonella; Zambonin, Carlo

    2016-03-20

    Salicylic and benzoic acid are phenolic acids occurring in plant cells, thus they can be present in fruit and vegetables at various levels. They possess anti-inflammatory and antimicrobial properties, however they may induce symptoms and health problems in a small percentage of the population. Therefore, a low phenolic acid diet may be of clinical benefit to such individuals. In order to achieve this goal, the concentration of these substances in different food and beverages should be assessed. The present work describes for the first time a new method, based on solid phase microextraction (polydimethylsiloxane-divinylbenzene fiber) coupled to liquid chromatography with UV diode array detection, for the simultaneous determination of salicylic acid, 3-methyl salicylic acid, 4-methyl salicylic acid, acetylsalicylic acid and benzoic acid in selected fruit, vegetables and beverages. All the aspects influencing fiber adsorption (time, temperature, pH, salt addition) and desorption (desorption and injection time, desorption solvent mixture composition) of the analytes have been investigated. An isocratic separation was performed using an acetonitrile-phosphate buffer (pH 2.8; 2 mM) mixture (70:30, v/v) as the mobile phase. The estimated LOD and LOQ values (μg/mL) were in the range 0.002-0.028 and 0.007-0.095. The within-day and day-to-day precision values (RSD%) were between 4.7-6.1 and 6.6-9.4, respectively. The method has been successfully applied to the analysis of fava beans, blueberries, kiwi, tangerines, lemons, oranges and fruit juice (lemon and blueberry) samples. The major advantage of the method is that it only requires simple homogenization and/or centrifugation and dilution steps prior to SPME and injection in the LC system. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Tank Vapor Characterization Project: Headspace vapor characterization of Hanford Waste Tank 241-S-103: Results from samples collected on 06/12/96

    International Nuclear Information System (INIS)

    Evans, J.C.; Pool, K.H.; Thomas, B.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-S-103 (Tank S-103) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in Table S.1. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples are also listed in Table S.1. Detailed descriptions of the analytical results appear in the appendices

  12. Tank Vapor Characterization Project: Headspace vapor characterization of Hanford Waste Tank 241-C-204: Results from samples collected on 07/02/96

    International Nuclear Information System (INIS)

    Thomas, B.L.; Evans, J.C.; Pool, K.H.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-C-204 (Tank C-204) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in Table S.1. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples are also listed in Table S.1. Detailed descriptions of the analytical results appear in the appendices

  13. Tank Vapor Characterization Project: Headspace vapor characterization of Hanford Tank 241-B-105: Results from samples collected on 07/30/96

    International Nuclear Information System (INIS)

    Pool, K.H.; Evans, J.C.; Thomas, B.L.

    1997-01-01

    This report describes the analytical results of vapor samples taken from the headspace of the waste storage tank 241-B-105 (Tank B-105) at the Hanford Site in Washington State. The results described in this report were obtained to characterize the vapors present in the tank headspace and to support safety evaluations and tank farm operations. The results include air concentrations of selected inorganic and organic analytes and grouped compounds from samples obtained by Westinghouse Hanford Company (WHC) and provided for analysis to Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volumes provided by WHC. A summary of the inorganic analytes, permanent gases, and total non-methane organic compounds is listed in Table S.1. The three highest concentration analytes detected in SUMMA trademark canister and triple sorbent trap samples are also listed in Table S.1. Detailed descriptions of the analytical results appear in the appendices

  14. Headspace thin-film microextraction onto graphene membranes for specific detection of methyl(cyclopentadienyl)-tricarbonyl manganese in water samples by total reflection X-ray fluorescence

    Science.gov (United States)

    Romero, V.; Costas-Mora, I.; Lavilla, I.; Bendicho, C.

    2016-12-01

    In this work, a novel analytical approach for determining methyl(cyclopentadienyl)-tricarbonyl (MMT) by total reflection X-ray fluorescence (TXRF) based on its trapping onto unmodified graphene membranes is described. Graphene membranes were synthesized by mild-thermal reduction of graphene oxide following drop-casting onto a glass substrate. High flexible and easy-to-handle graphene membranes with 10 mm diameter were obtained. In order to use the as-prepared membranes as extraction phases for headspace thin-solid film microextraction of MMT, they were fitted to quartz reflectors and placed onto the top of the glass vial containing the sample. Reflectors containing graphene membranes were directly used as sample carriers for TXRF analysis. Different parameters involved in the microextraction step were optimized in order to obtain the best performance. Detection and quantification limits were 18 and 60 ng L- 1 MMT, respectively. An enrichment factor of 265 was obtained. The method was successfully applied for the specific detection of MMT in different water samples and a certified reference material e.g., NWTM-27.2 fortified lake water. A recovery study was carried out on spiked water samples showing recoveries in the range 98-104% with a relative standard deviation of 4% (N = 5). In addition, speciation of manganese, i.e. MMT and Mn(II),in water samples can be accomplished since only volatile MMT is transferred to the headspace and retained onto graphene membranes.

  15. All rights reserved Development of Headspace Solid-Phase ...

    African Journals Online (AJOL)

    ADOWIE PERE

    affecting the performance of the GC-MS system and require optimization in .... subsequent analysis. The time was selected to reduce the total time of analysis, since efficient extraction can also be achieved prior to equilibrium provided all other factors are ... stirring rate can lead to the vibration of the fiber which could lead to ...

  16. SPME applied to the study of volatile organic compounds emitted by three species of Eucalyptus in situ. Solid-phase micro extraction.

    Science.gov (United States)

    Zini, Cláudia A; Augusto, Fabio; Christensen, Eva; Caramão, Elina B; Pawliszyn, Janusz

    2002-12-04

    Headspace solid-phase microextraction coupled to gas chromatography/ion trap mass spectrometry-65 microm polydimethylsiloxane/divinylbenzene (PDMS/DVB) was used to identify and monitor the emission patterns of biogenic volatile organic compounds from leaves of Eucalyptus dunnii, Eucalyptus saligna, and Eucalyptus citriodora in situ. Short extractions (1 min) were performed every 30 min for periods of 8-10 h during 24 days taking advantage of the high capacity of this porous polymer coating. Forty-two compounds were detected and 20 identified in the headspace of E. saligna leaves, and 19 of 27 compounds were identified in the headspace of E. dunnii leaves. The emission pattern of (E)-beta-ocimene and rose oxide suggests that they may play a bioactive role in Eucalyptus.

  17. Tank 241-B-103 headspace gas and vapor characterization: Results for homogeneity samples collected on October 16, 1996. Tank vapor characterization project

    International Nuclear Information System (INIS)

    Olsen, K.B.; Pool, K.H.; Evans, J.C.

    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

  18. A full evaporation headspace technique with capillary GC and ITD: a means for quantitating volatile organic compounds in biological samples.

    Science.gov (United States)

    Schuberth, J

    1996-07-01

    The full evaporation technique (FET), which is a variant of headspace analysis used to overcome matrix effects, was combined with capillary gas chromatography (GC) and ion-trap detection (ITD). The aim was to enable quantitative tests of volatile organic compounds (VOCs) in blood and postmortem tissue samples. FET was applied to sample sized less than 35 mg whose VOCs were released from the matrix at an equilibration temperature of 130 degrees C. A capillary column with a nonpolar stationary phase was used for GC, and ITD was performed with the mass spectrometer run in full-scan mode. The potential of FET-GC-ITD was studied for the analysis of blood samples spiked with low concentrations of ethanol, acetone, 2-propanol, and 2-butanone and on brain tissue that contained methyl tert-butyl ether (MTBE), Benzene, toluene, ethylbenzene, o-, m-, and p-xylene, and propylbenzene. Samples were obtained from the bodies of victims who had inhaled smoke during an arson or accidental fire. There was a linear relationship between peak area and sample size, which indicates that the conditions of full evaporation were met and that the matrix effect was negated. The total analyte amount in the test sample at the limit of quantitation was in the range of 0.4-1 nmol for polar VOCs in blood and 0.03-0.1 nmol for nonpolar VOCs in brain tissue. Data on precision and accuracy of the method are reported.

  19. Headspace-trap gas chromatography-mass spectrometry for determination of sulphur mustard and related compounds in soil.

    Science.gov (United States)

    Røen, Bent T; Unneberg, Erik; Tørnes, John Aa; Lundanes, Elsa

    2010-04-02

    Methods for trace determination of sulphur mustard (HD) and some related cyclic sulphur compounds in soil samples have been developed using headspace-trap in combination with gas chromatography-mass spectrometry (GC-MS). Two quite different types of soil were employed in the method optimisation (sandy loam and silty clay loam). Prior to analysis, water saturated with sodium chloride was added to the samples, at a water to soil ratio of 1:1. A detection limit of 3 ng/g was achieved for HD, while the cyclic sulphur compounds 1,4-thioxane, 1,3-dithiolane and 1,4-dithiane could be detected at 0.2-0.7 ng/g. The methods were validated in the concentration range from the limit of quantification (LOQ) to hundred times LOQ. The within assay precision at fifty times LOQ was 6.9-7.3% relative standard deviation (RSD) for determination of the cyclic sulphur compounds, and 15% RSD for determination of HD. Recoveries were in the range of 43-60% from the two soil types. As the technique requires very little sample preparation, the total time for sample handling and analysis was less than 1h. The technique was successfully employed for the determination of cyclic sulphur compounds in a sediment sample from an old dumping site for chemical munitions, known to contain HD degradation products. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  20. Tank 241-U-106 vapor sampling and analysis tank characterization report

    International Nuclear Information System (INIS)

    Huckaby, J.L.

    1995-01-01

    This report presents the details of the Hanford waste tank characterization study for tank 241-U-106. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedures that were presented in other reports. The vapor and headspace gas samples were collected to determine the potential risks to tank farm workers due to fugitive emissions from the tank

  1. Development of headspace solid-phase microextraction method for ...

    African Journals Online (AJOL)

    ... analysis of 14 multiclass pesticide residues in fruits and vegetable samples. The gas chromatography mass spectrometry parameters (desorption temperature and time, column flow rate, interface temperature) and solid phase microextraction parameters (fiber coating type, extraction temperature and time, pH, salt addition ...

  2. High hydrostatic pressure treatments enhance volatile components of pre-germinated brown rice revealed by aromatic fingerprinting based on HS-SPME/GC-MS and chemometric methods.

    Science.gov (United States)

    Xia, Qiang; Mei, Jun; Yu, Wenjuan; Li, Yunfei

    2017-01-01

    Germination favors to significantly enhance functional components and health attributes of whole-grain brown rice (BR), but the production of germinated BR (GBR) compromises the typical rice flavor perception due to soaking process. Simultaneously, high hydrostatic pressure (HHP) is considered as an effective processing technique to enhance micronutrients utilization efficiency of GBR and improve products flavor, but no information about the effects of HHP treatments on volatile fingerprinting of GBR has been reported. Therefore, the objective of this work was to apply HHP to improve the flavor and odor of GBR grains by exploring HHP-induced changes in aroma compounds. GBR grains were obtained by incubating at 37°C for 36h, and subsequently subjected to HHP treatments at pressures 100, 300 and 500MPa for 15min, using 0.1MPa as control. Headspace solid-phase micro extraction coupled to gas chromatography mass spectrometry was used to characterize process-induced shifts of volatile organic compounds fingerprinting, followed by multivariate analysis. Our results confirmed the significant reduction of total volatile fractions derived from germination process. Contrarily, the following HHP treatments greatly enhanced the flavor components of GBR, particularly characteristic odorants including aldehydes, ketones, and alcohols. Principal component analysis further indicated the different influence of germination and high pressure on the changes in volatile components. Partial least square-discrimination analysis suggested that 4-vinylguaiacol was closely linked to germination, whereas E,E-2,4-decadienal, E-2-hexenal, E,E-2,4-heptadienal and benzyl alcohol could be considered as volatile biomarkers of high pressure. Copyright © 2016 Elsevier Ltd. All rights reserved.

  3. Perceptual characterization and analysis of aroma mixtures using gas chromatography recomposition-olfactometry.

    Directory of Open Access Journals (Sweden)

    Arielle J Johnson

    Full Text Available This paper describes the design of a new instrumental technique, Gas Chromatography Recomposition-Olfactometry (GC-R, that adapts the reconstitution technique used in flavor chemistry studies by extracting volatiles from a sample by headspace solid-phase microextraction (SPME, separating the extract on a capillary GC column, and recombining individual compounds selectively as they elute off of the column into a mixture for sensory analysis (Figure 1. Using the chromatogram of a mixture as a map, the GC-R instrument allows the operator to "cut apart" and recombine the components of the mixture at will, selecting compounds, peaks, or sections based on retention time to include or exclude in a reconstitution for sensory analysis. Selective recombination is accomplished with the installation of a Deans Switch directly in-line with the column, which directs compounds either to waste or to a cryotrap at the operator's discretion. This enables the creation of, for example, aroma reconstitutions incorporating all of the volatiles in a sample, including instrumentally undetectable compounds as well those present at concentrations below sensory thresholds, thus correcting for the "reconstitution discrepancy" sometimes noted in flavor chemistry studies. Using only flowering lavender (Lavandula angustifola 'Hidcote Blue' as a source for volatiles, we used the instrument to build mixtures of subsets of lavender volatiles in-instrument and characterized their aroma qualities with a sensory panel. We showed evidence of additive, masking, and synergistic effects in these mixtures and of "lavender' aroma character as an emergent property of specific mixtures. This was accomplished without the need for chemical standards, reductive aroma models, or calculation of Odor Activity Values, and is broadly applicable to any aroma or flavor.

  4. Comparison of needle concentrator with SPME for GC determination of benzene, toluene, ethylbenzene, and xylenes in aqueous samples

    Energy Technology Data Exchange (ETDEWEB)

    Prikryl, P.; Sevcik, J. [Charles Univ., Prague (Czech Republic). Dept. of Analytical Chemistry; Kubinec, R.; Jurdakova, H.; Ostrovsky, I.; Sojak, L. [Comenius Univ., Bratislava (Slovakia). Chemical Inst.; Berezkin, V. [Russian Academy of Sciences, Moscow (Russian Federation). A.V. Topchiev Inst. of Petrochemical Synthesis

    2006-07-15

    A method of solventless extraction of volatile organic compounds from aqueous samples has been developed and validated. A new arrangement in which the internal volume of a needle capillary adsorption trap is completely filled with Porapak Q, as adsorbent material, and wet alumina, as a source of desorptive water vapor flow, is presented. The device has been used for head-space sampling of benzene, toluene, ethylbenzene, and xylenes (BTEX) from water samples and compared with solid-phase microextraction. Under the same sampling conditions the analytical characteristics of the device for the BTEX compounds are better than those of solid-phase microextraction. Limits of detection and quantification are below 0.5 {mu} g L{sup -1}. (orig.)

  5. Effect of eugenol and guaiacol application on tomato aroma composition determined by headspace stir bar sorptive extraction.

    Science.gov (United States)

    Pardo-García, Ana I; Martínez-Gil, Ana M; López-Córcoles, Horacio; Zalacain, Amaya; Salinas, Rosario

    2013-03-30

    The present work was carried out because there is only a small amount of literature on how the volatile composition of tomatoes can be modified by the effect of exogenous substances in contact with tomato plants. This work studies how eugenol and guaiacol, either by foliar application and/or in the surrounding atmosphere, can affect the volatile composition of this fruit. An important work of this study was also conduced to validate the analytical method [headspace stir bar sorptive extraction-gas chromatography-mass spectrometry (HS-SBSE-GC-MS)] to determine the composition of the volatiles in tomato. Analytical method validation parameters such as linearity, limit of detection, limit of quantification, and recovery proved that this method is suitable for the analysis of tomato volatiles. Their eugenol and guaiacol content changed, with an increase of 200 and 35 times, respectively, when foliar treatment was used, and an increase of 10, in both cases, when plants were in contact with the contaminated atmosphere. As consequence of the treatments other volatile compounds changed considerably. For first time, a HS-SBSE-GC-MS method was successfully validated for the study of volatiles in tomatos. Results suggests that exogenous compounds in contact with the plants, such as eugenol and guaiacol, can be absorbed changing the global volatile composition of fruits, which could produce a negative or positive effect in their aroma. © 2012 Society of Chemical Industry.

  6. Determination of physiological levels of volatile organic compounds in blood using static headspace capillary gas chromatography with serial triple detection.

    Science.gov (United States)

    Schroers, H J; Jermann, E; Begerow, J; Hajimiragha, H; Chiarotti-Omar, A M; Dunemann, L

    1998-04-01

    A static capillary gas chromatographic method using three different detectors [photoionization detector (PID), electron capture detector (ECD) and flame ionization detector (FID)] switched in series is presented for the determination of volatile organic compounds (VOCs) in sub microgram l-1 levels. The method was applied for the analysis of selected environmentally and occupationally relevant non-halogenated and chlorinated aromatic hydrocarbons (e.g., benzene, toluene, xylenes, dichlorobenzenes) as well as chlorinated aliphatic hydrocarbons (e.g., trichloroethene, tetrachloroethene) in blood samples. Detailed investigations, in respect to the figures of merit were carried out. For most of the selected VOCs detection limits (calculated as the three-fold standard deviation of low level calibration standards) in the range from 26 (benzene) to 67 ng l-1 (m/p-xylene) were achieved which are comparable with those reported for dynamic headspace techniques in combination with mass spectrometric detection. For the individual VOCs the within-series precision varied from 4 to 19% and the day-to-day precision from 11 to 28%. Regarding PID as well as FID the calibration graphs for all substances were linear up to at least 10 micrograms l-1 while the ECD response was linear up to concentrations of about 0.6 microgram l-1 for the halogenated compounds. Our method is applicable for the quantitative determination of VOCs in blood in the occupationally as well as in the physiologically relevant (normal) concentration range.

  7. [A novel vapor dynamic headspace enrichment equipment for nontarget screening of volatile organic compounds in drinking water].

    Science.gov (United States)

    Ma, Huilian; Zhang, Haijun; Tian, Yuzeng; Wang, Longxing; Chen, Jiping

    2011-09-01

    A novel vapor dynamic headspace enrichment device was set up for nontarget screening of volatile organic compounds (VOCs) in drinking water. The main operating parameters of this device, such as length of distillation tube, volume of collected condensate, and choice of absorbent, were optimized. In this device, vapor was utilized as a purge gas and water was utilized as a absorbent. With the help of the device, one liter of water sample could be concentrated to 5 mL and the sensitivity of traditional purge and trap-gas chromatography-mass spectrometry (P&T-GC-MS) could be improved 1-2 orders of magnitude. Source and disinfected water samples from a water treatment plant were analyzed with this method. Compared with the traditional P&T-GC-MS analysis without pre-enrichment, the numbers of identified VOCs were improved from 0 to 16 for source water and 5 to 35 for disinfected water samples. It is also shown that there are many halide compounds in VOCs in disinfected water which do not exist in source water.

  8. Naphthalene emissions from moth repellents or toilet deodorant blocks determined using head-space and small-chamber tests.

    Science.gov (United States)

    Jo, Wan-Kuen; Lee, Jong-Hyo; Lim, Ho-Jin; Jeong, Woo-Sik

    2008-01-01

    The present study investigated the emissions of naphthalene and other compounds from several different moth repellents (MRs) and one toilet deodorant block (TDB) currently sold in Korea, using a headspace analysis. The emission factors and emission rates of naphthalene were studied using a small-scale environmental chamber. Paper-type products emitted a higher concentration of the total volatile organic compounds (VOCs) (normalized to the weight of test piece) than ball-type products, which in turn emitted higher concentration than a gel-type product. In contrast, naphthalene was either the most or the second highest abundant compound for the four ball products, whereas for paper and gel products it was not detected or was detected at much lower levels. The abundance of naphthalene ranged between 18.4% and 37.3% for ball products. The results showed that the lower the air changes per hour (ACH) level was, the higher the naphthalene concentrations became. In general, a low ACH level suggests a low ventilation rate. The emission factor for naphthalene was nearly 100 times higher for a ball MR than for a gel or a paper MR. For the ball MR, the lower ACH level resulted in higher emission rate.

  9. 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.

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

    International Nuclear Information System (INIS)

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

    2007-01-01

    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 μL 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 μg L -1 range varying between 0.016 and 0.039 μg 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

  11. A volatile tracer-assisted headspace analytical technique for determining the swelling capacity of superabsorbent polymers.

    Science.gov (United States)

    Zhang, Shu-Xin; Jiang, Ran; Chai, Xin-Sheng

    2017-09-01

    This paper reports on a new method for the determination of swelling capacity of superabsorbent polymers by a volatile tracer-assisted headspace gas chromatography (HS-GC). Toluene was used as a tracer and added to the solution for polymers swelling test. Based on the differences of the tracer partitioned between the vapor and hydrogel phase before and after the polymer's swelling capacity, a transition point (corresponding to the material swelling capacity) can be observed when plotting the GC signal of toluene vs. the ratio of solution added to polymers. The present method has good precision (RSDpolymers at the elevated temperatures. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Determination of ketone bodies in blood by headspace gas chromatography-mass spectrometry

    DEFF Research Database (Denmark)

    Holm, Karen Marie Dollerup; Linnet, Kristian; Rasmussen, Brian Schou

    2010-01-01

    A gas chromatography-mass spectrometry (GC-MS) method for determination of ketone bodies (ß-hydroxybutyrate, acetone, and acetoacetate) in blood is presented. The method is based on enzymatic oxidation of D-ß-hydroxybutyrate to acetoacetate, followed by decarboxylation to acetone, which...... was quantified by the use of headspace GC-MS using acetone-(13)C(3) as an internal standard. The developed method was found to have intra- and total interday relative standard deviations acetone+acetoacetate levels (~25 to 8300 µM) and D-ß-hydroxybutyrate levels (~30 to 16500 µM). Recovery values varied...

  13. Magnetic headspace adsorptive extraction of chlorobenzenes prior to thermal desorption gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Vidal, Lorena, E-mail: lorena.vidal@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain); Ahmadi, Mazaher [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Fernández, Elena [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain); Madrakian, Tayyebeh [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Canals, Antonio, E-mail: a.canals@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain)

    2017-06-08

    This study presents a new, user-friendly, cost-effective and portable headspace solid-phase extraction technique based on graphene oxide decorated with iron oxide magnetic nanoparticles as sorbent, located on one end of a small neodymium magnet. Hence, the new headspace solid-phase extraction technique has been called Magnetic Headspace Adsorptive Extraction (Mag-HSAE). In order to assess Mag-HSAE technique applicability to model analytes, some chlorobenzenes were extracted from water samples prior to gas chromatography-mass spectrometry determination. A multivariate approach was employed to optimize the experimental parameters affecting Mag-HSAE. The method was evaluated under optimized extraction conditions (i.e., sample volume, 20 mL; extraction time, 30 min; sorbent amount, 10 mg; stirring speed, 1500 rpm, and ionic strength, non-significant), obtaining a linear response from 0.5 to 100 ng L{sup −1} for 1,3-DCB, 1,4-DCB, 1,2-DCB, 1,3,5-TCB, 1,2,4-TCB and 1,2,3-TCB; from 0.5 to 75 ng L{sup −1} for 1,2,4,5-TeCB, and PeCB; and from 1 to 75 ng L{sup −1} for 1,2,3,4-TeCB. The repeatability of the proposed method was evaluated at 10 ng L{sup −1} and 50 ng L{sup −1} spiking levels, and coefficients of variation ranged between 1.5 and 9.5% (n = 5). Limits of detection values were found between 93 and 301 pg L{sup −1}. Finally, tap, mineral and effluent water were selected as real water samples to assess method applicability. Relative recoveries varied between 86 and 110% showing negligible matrix effects. - Highlights: • A new extraction technique named Magnetic Headspace Adsorptive Extraction is presented. • Graphene oxide/iron oxide composite deposited on a neodymiun magnet as sorbent. • Sorbent of low cost, rapid and simple synthesis, easy manipulation and portability options. • Fast and efficient extraction and sensitive determination of chlorobenzenes in water samples.

  14. Rapid quantitative detection of glucose content in glucose injection by reaction headspace gas chromatography.

    Science.gov (United States)

    Xie, Wei-Qi; Gong, Yi-Xian; Yu, Kong-Xian

    2017-10-20

    This work investigates an automated technique for rapid detecting the glucose content in glucose injection by reaction headspace gas chromatography (HS-GC). This method is based on the oxidation reaction of glucose in glucose injection with potassium dichromate. The carbon dioxide (CO 2 ) formed from the oxidation reaction can be quantitatively detected by GC. The results show that the relative standard deviation (RSD) of the present method was within 2.91%, and the measured glucose contents in glucose injection closely match those quantified by the reference method (relative differences glucose content in glucose injection related applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Determination of maximal amount of minor gases adsorbed in a shale sample by headspace gas chromatography.

    Science.gov (United States)

    Zhang, Chun-Yun; Hu, Hui-Chao; Chai, Xin-Sheng; Pan, Lei; Xiao, Xian-Ming

    2014-02-07

    In this paper, we present a novel method for determining the maximal amount of ethane, a minor gas species, adsorbed in a shale sample. The method is based on the time-dependent release of ethane from shale samples measured by headspace gas chromatography (HS-GC). The study includes a mathematical model for fitting the experimental data, calculating the maximal amount gas adsorbed, and predicting results at other temperatures. The method is a more efficient alternative to the isothermal adsorption method that is in widespread use today. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. HS-SPME GC/MS characterization of volatiles in raw and dry-roasted almonds (Prunus dulcis).

    Science.gov (United States)

    Xiao, Lu; Lee, Jihyun; Zhang, Gong; Ebeler, Susan E; Wickramasinghe, Niramani; Seiber, James; Mitchell, Alyson E

    2014-05-15

    A robust HS-SPME and GC/MS method was developed for analyzing the composition of volatiles in raw and dry-roasted almonds. Almonds were analyzed directly as ground almonds extracted at room temperature. In total, 58 volatiles were identified in raw and roasted almonds. Straight chain aldehydes and alcohols demonstrated significant but minimal increases, while the levels of branch-chain aldehydes, alcohols, heterocyclic and sulfur containing compounds increased significantly (500-fold) in response to roasting (p<0.05). Benzaldehyde decreased from 2934.6±272.5 ng/g (raw almonds) to 315.8±70.0 ng/g (averaged across the roasting treatments evaluated i.e. 28, 33 and 38 min at 138 °C) after roasting. Pyrazines were detected in only the roasted almonds, with the exception of 2,5-dimethylpyrazine, which was also found in raw almonds. The concentration of most alcohols increased in the roasted samples with the exception of 2-methyl-1-propanol, 3-methyl-1-butanol and 2-phenylethyl alcohol, which decreased 68%, 80%, and 86%, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

  17. Analytic escrutineo for plaguicidas organofosforados in blood in forensic cases by means of SPME-GC/NPD

    International Nuclear Information System (INIS)

    Fernandez Quesada, K.; Saenz Ugalde, M. F.

    2003-01-01

    The plaguicidas organophosphorus represent one of the most important causes of intoxication in Costa Rica; 20% of the cases received in the Section of Toxicology of the Department of Forensic Sciences of the Organism of Judicial Investigation (OIJ) are related to these plaguicidas. At the present time, the employed techniques in this institution to carry out the organophosphorus analyses in blood, present important limitations in their analytic potential. As a consequence, it is necessary to look for new methodologies, with the purpose to obtain a great specificity, and to diminish the limits of detection. This would allow a more qualified service that assures the validity and reliability of the results. Besides, it is an ideal instrument for the correct administration of justice of the Judicial Authorities. In this final work of graduation, it develops a methodology for the scrutiny of pesticides organophosphorus, in which a sample of biological origin of forensic importance is used. This employs a technique of quick, simple and clean extraction, using a separation method of detection of high analytic sensibility. In the methodology's development, samples of total blood, and the microextraccion techniques in solid phase will be used (SPME), and detection with gas chromatography by a specific instrumental detector of match and nitrogen (GCINPD) [es

  18. [Difference of volatile constituents contained in female and male flowers of Trichosanthes kirilowii by HS-SPME-GC-MS].

    Science.gov (United States)

    Sun, Wen; Chao, Zhimao; Wang, Chun; Wu, Xiaoyi; Tan, Zhigao

    2012-06-01

    To compare and analyze volatile constituents from flowers of Trichosanthes kirilowii, in order to point out characteristic differences between female and male flowers. Blooming female and male flowers were collected in the same place. Volatile constituents were extracted from the flower by solid phase micro-extraction (SPME), then separated and analyzed by gas chromatography-mass-spectrometry (GC-MS). Fifty-two and forty-five chromatographic peaks were separated from the female and male flowers, respectively. Forty seven constituents were identified and their relative percentage compositions were determined with the peak area normalization method. Linalool, alpha-farnesene, benzene methanol, and (Z)-2-methylbutanal oxime were the main volatile constituents. The contents of linalool and alpha-farnesene in female flower were remarkably higher than those in male. In contrast, the content of benzene methanol in male flower was remarkably higher than that in female. In the first study on chemical constituents from flowers in genus Trichosanthes, 37 compounds are separated from T. kirilowii. Contents of linalool, alpha-farnesene and benzene methanol show the characteristic differences of volatile constituents contained in male and female flowers of T. kirilowii, which enriches the basic studies on dioecious plant.

  19. Differentiation of South American crack and domestic (US) crack cocaine via headspace-gas chromatography/mass spectrometry.

    Science.gov (United States)

    Colley, Valerie L; Casale, John F

    2015-03-01

    South American 'crack' cocaine, produced directly from coca leaf, can be distinguished from US domestically produced crack on the basis of occluded solvent profiles. In addition, analysis of domestically produced crack indicates the solvents that were used for cocaine hydrochloride (HCl) processing in South America. Samples of cocaine base (N=3) from South America and cocaine from the USA (N=157 base, N=88 HCl) were analyzed by headspace-gas chromatography-mass spectrometry (HS-GC-MS) to determine their solvent profiles. Each cocaine HCl sample was then converted to crack cocaine using the traditional crack production method and re-examined by HS-GC-MS. The resulting occluded solvent profiles were then compared to their original HCl solvent profiles. Analysis of the corresponding crack samples confirmed the same primary processing solvents found in the original HCl samples, but at reduced levels. Domestically seized crack samples also contained reduced levels of base-to-HCl conversion solvents. In contrast, analysis of South American crack samples confirmed the presence of low to high boiling hydrocarbons and no base-to-HCl conversion solvents. The presented study showed analysis of crack cocaine samples provides data on which processing solvents were originally utilized in the production of cocaine HCl in South America, prior to conversion to crack cocaine. Determination of processing solvents provides valuable information to the counter-drug intelligence community and assists the law enforcement community in determining cocaine distribution and trafficking routes throughout the world. Published 2014. This article is a U.S. Government work and is in the public domain in the USA.

  20. Rapid detection of pathogenic bacteria by volatile organic compound (VOC) analysis

    Science.gov (United States)

    Senecal, Andre G.; Magnone, Joshua; Yeomans, Walter; Powers, Edmund M.

    2002-02-01

    Developments in rapid detection technologies have made countless improvements over the years. However, because of the limited sample that these technologies can process in a single run, the chance of capturing and identifying a small amount of pathogens is difficult. The problem is further magnified by the natural random distribution of pathogens in foods. Methods to simplify pathogenic detection through the identification of bacteria specific VOC were studied. E. coli O157:H7 and Salmonella typhimurium were grown on selected agar medium to model protein, and carbohydrate based foods. Pathogenic and common spoilage bacteria (Pseudomonas and Morexella) were screened for unique VOC production. Bacteria were grown on agar slants in closed vials. Headspace sampling was performed at intervals up to 24 hours using Solid Phase Micro-Extraction (SPME) techniques followed by GC/MS analysis. Development of unique volatiles was followed to establish sensitivity of detection. E. coli produced VOC not found in either Trypticase Soy Yeast (TSY) agar blanks or spoilage organism samples were - indole, 1-decanol, and 2-nonanone. Salmonella specific VOC grown on TSY were 3-methyl-1-butanol, dimethyl sulfide, 2-undecanol, 2-pentadecanol and 1-octanol. Trials on potato dextrose agar (PDA) slants indicated VOC specific for E. coli and Salmonella when compared to PDA blanks and Pseudomonas samples. However, these VOC peaks were similar for both pathogens. Morexella did not grow on PDA slants. Work will continue with model growth mediums at various temperatures, and mixed flora inoculums. As well as, VOC production based on the dynamics of bacterial growth.

  1. Comparative Analysis of Flower Volatiles from Nine Citrus at Three Blooming Stages

    Directory of Open Access Journals (Sweden)

    Muhammad Azam

    2013-11-01

    Full Text Available Volatiles from flowers at three blooming stages of nine citrus cultivars were analyzed by headspace-solid phase microextraction (HS-SPME-GC-MS. Up to 110 volatiles were detected, with 42 tentatively identified from citrus flowers for the first time. Highest amounts of volatiles were present in fully opened flowers of most citrus, except for pomelos. All cultivars were characterized by a high percentage of either oxygenated monoterpenes or monoterpene hydrocarbons, and the presence of a high percentage of nitrogen containing compounds was also observed. Flower volatiles varied qualitatively and quantitatively among citrus types during blooming. Limonene was the most abundant flower volatile only in citrons; α-citral and β-citral ranked 2nd and 3rd only for Bergamot, and unopened flowers of Ponkan had a higher amount of linalool and β-pinene while much lower amount of γ-terpinene and p-cymene than Satsuma. Taking the average of all cultivars, linalool and limonene were the top two volatiles for all blooming stages; β-pinene ranked 3rd in unopened flowers, while indole ranked 3rd for half opened and fully opened flower volatiles. As flowers bloomed, methyl anthranilate increased while 2-hexenal and p-cymene decreased. In some cases, a volatile could be high in both unopened and fully opened flowers but low in half opened ones. Through multivariate analysis, the nine citrus cultivars were clustered into three groups, consistent with the three true citrus types. Furthermore, an influence of blooming stages on clustering was observed, especially with hybrids Satsuma and Huyou. Altogether, it was suggested that flower volatiles can be suitable markers for revealing the genetic relationships between citrus cultivars but the same blooming stage needs to be strictly controlled.

  2. New Methyltrimethoxysilane-(3-Mercaptopropyl)- Trimethoxysilane Coated Hollow Fiber-Solid Phase Micro extraction for Hexanal and Heptanal Analysis

    International Nuclear Information System (INIS)

    Siti Munirah Abd Wahib; Mohd Marsin Sanagi

    2016-01-01

    Determination of volatile organic compounds (VOCs) in various matrices is often accomplished using solid phase micro extraction (SPME) as a superior mode of extraction. Alternatively, another configuration of solid phase micro extraction (SPME) namely hollow fiber-solid phase micro extraction (HF-SPME) is a great approach to redress some limitations of the ordinary SPME fibers including fiber breakage, coating stripping and sample carry over. The HF-SPME technique highlights the use of hollow polypropylene (PP) membrane to hold and protect the adsorbent inside its lumen. Unlike the conventional SPME, the inexpensive HF device can be disposed after single use. Introducing extracting phase via sol-gel technology has gained great interest owing to its simple preparation method and promising way to obtain materials with good characteristics. In the present work, a new hybrid silica material based on methyltrimethoxysilane-(3-mercaptopropyl)trimethoxysilane (MTMOS-MPTMOS) was introduced as a new extractant of HF-SPME and the effectiveness of the proposed method was tested for analysis of hexanal and heptanal as the target VOC analytes. Preparation of the HF-SPME MTMOS-MPTMOS was simple in which the hybrid material was synthesized via sol-gel method and was self-polymerized in small segments of HF. Parameters affecting the efficiency of the HF-SPME MTMOS-MPTMOS in extracting both aldehydes were thoroughly investigated and analyzed by gas chromatography-flame ionization detection (GC-FID). It was found that the highest efficiency was achieved as the extraction was conducted in 30 min at a stirring rate of 1000 rpm in a 10 mL of sample solution whereby the back-extraction was performed via vortex for 3 min using 100 μL methanol as desorption solvent. Under the optimal conditions, linearity was observed over a range of 0.020-10.00 μg mL -1 with detection limits of 0.015 μg mL -1 and 0.010 μg mL -1 for hexanal and heptanal, respectively. The applicability of the HF-SPME

  3. Headspace single-drop microextraction coupled to microvolume UV-vis spectrophotometry for iodine determination

    International Nuclear Information System (INIS)

    Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

    2009-01-01

    Headspace single-drop microextraction has been combined with microvolume UV-vis spectrophotometry for iodine determination. Matrix separation and preconcentration of iodide following in situ volatile iodine generation and extraction into a microdrop of N,N'-dimethylformamide is performed. An exhaustive characterization of the microextraction system and the experimental variables affecting iodine generation from iodide was carried out. The procedure employed consisted of exposing 2.5 μL of N,N'-dimethylformamide to the headspace of a 10 mL acidic (H 2 SO 4 2 mol L -1 ) aqueous solution containing 1.7 mol L -1 Na 2 SO 4 for 7 min. Addition of 1 mL of H 2 O 2 1 mol L -1 for in situ iodine generation was performed. The limit of detection was determined as 0.69 μg L -1 . The repeatability, expressed as relative standard deviation, was 4.7% (n = 6). The calibration working range was from 5 to 200 μg L -1 (r 2 = 0.9991). The large preconcentration factor obtained, ca. 623 in only 7 min, compensate for the 10-fold loss in sensitivity caused by the decreased optical path, which results in improved detection limits as compared to spectrophotometric measurements carried out with conventional sample cells. The method was successfully applied to the determination of iodine in water, pharmaceutical and food samples

  4. 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.

  5. Vented spikes improve delivery from intravenous bags with no air headspace.

    Science.gov (United States)

    Galush, William J; Horst, Travis A

    2015-07-01

    Flexible plastic bags are the container of choice for most intravenous (i.v.) infusions. Under certain circumstances, however, the air-liquid interface present in these i.v. bags can lead to physical instability of protein biopharmaceuticals, resulting in product aggregation. In principle, the air headspace present in the bags can be removed to increase drug stability, but experiments described here show that this can result in incomplete draining of solution from the bag using gravity delivery, or generation of negative pressure in the bag when an infusion pump is used. It is expected that these issues could lead to incomplete delivery of medication to patients or pump-related problems, respectively. However, here it is shown that contrary to the standard pharmacy practice of using nonvented spikes with i.v. bags, the use of vented spikes with i.v. bags that lack air headspace allows complete delivery of the dose solution without impacting the physical stability of a protein-based drug. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

  6. Headspace gas chromatography-mass spectrometry of volatile compounds in murici (Byrsonima crassifolia l. Rich).

    Science.gov (United States)

    Alves, G L; Franco, M R B

    2003-01-24

    Northern and Northeastern Brazil have a natural diversity of fruits, many of which are considered exotic, presenting different flavors and aromas. The enormous diversity of fruits represents a promising area for research on aromas. There is also a great potential for the manufacture of juices, desserts or other processed products. Murici is a typical fruit from these regions presenting a different flavor, reminiscent of that of cheese. This fruit is consumed mainly as juice, ice cream or as liquor, greatly appreciated by the local population. Headspace volatile compounds of three lots of the fruit from Ceará (Fortaleza) were collected by suction on Porapak Q for 2 h and desorbed with 300 microl of acetone. The isolated volatile compounds were separated by high resolution GC. Forty-six volatile compounds were detected, of which 41 were identified by gas chromatography-mass spectrometry and Kovats indices. The most abundant compounds were ethanol (28.3%) and ethyl hexanoate (25.1%). Butanoic acid (5.1%), hexanoic acid (5.1%) and methyl butyrate (2.8%) were also detected in the headspace of the fruit and confirm its unusual cheese aroma.

  7. Data on changes in red wine phenolic compounds, headspace aroma compounds and sensory profile after treatment of red wines with activated carbons with different physicochemical characteristics.

    Science.gov (United States)

    Filipe-Ribeiro, Luís; Milheiro, Juliana; Matos, Carlos C; Cosme, Fernanda; Nunes, Fernando M

    2017-06-01

    Data in this article presents the changes on phenolic compounds, headspace aroma composition and sensory profile of a red wine spiked with 4-ethylphenol and 4-ethylguaiacol and treated with seven activated carbons with different physicochemical characteristics, namely surface area, micropore volume and mesopore volume ("Reduction of 4-ethylphenol and 4-ethylguaiacol in red wine by activated carbons with different physicochemical characteristics: impact on wine quality" Filipe-Ribeiro et al. (2017) [1]). Data on the physicochemical characteristics of the activated carbons are shown. Statistical data on the sensory expert panel consistency by General Procrustes Analysis is shown. Statistical data is also shown, which correlates the changes in chemical composition of red wines with the physicochemical characteristics of activated carbons used.

  8. Data on changes in red wine phenolic compounds, headspace aroma compounds and sensory profile after treatment of red wines with activated carbons with different physicochemical characteristics

    Directory of Open Access Journals (Sweden)

    Luís Filipe-Ribeiro

    2017-06-01

    Full Text Available Data in this article presents the changes on phenolic compounds, headspace aroma composition and sensory profile of a red wine spiked with 4-ethylphenol and 4-ethylguaiacol and treated with seven activated carbons with different physicochemical characteristics, namely surface area, micropore volume and mesopore volume (“Reduction of 4-ethylphenol and 4-ethylguaiacol in red wine by activated carbons with different physicochemical characteristics: impact on wine quality” Filipe-Ribeiro et al. (2017 [1]. Data on the physicochemical characteristics of the activated carbons are shown. Statistical data on the sensory expert panel consistency by General Procrustes Analysis is shown. Statistical data is also shown, which correlates the changes in chemical composition of red wines with the physicochemical characteristics of activated carbons used.

  9. Method development and validation for determining 1,3-butadiene in human blood by gas chromatography-mass spectrometry and head-space gas chromatography.

    Science.gov (United States)

    Zhang, Su-Jing; Shen, Bao-Hua; Zhuo, Xian-Yi

    2013-04-01

    To develop a simple, validated method for identifying and quantifying 1,3-butadiene (BD) in human blood by gas chromatography-mass spectrometry (GC-MS) and head-space gas chromatography (HS-GC). BD was identified by GC-MS and HS-GC, and quantified by HS-GC. The method showed that BD had a good linearity from 50 to 500 microg/mL (r > 0.99). The limits of detection and quantification were 10 microg/mL and 50 microg/mL, respectively. Both the intra-day precision and inter-day precision were < 6.08%, and the accuracy was 96.98%-103.81%. The method was applied to an actual case, and the concentration of BD in the case was 242 microg/mL in human blood. This simple method is found to be useful for the routine forensic analysis of acute exposure to BD.

  10. Automated headspace solid-phase microextraction and on-fiber derivatization for the determination of clenbuterol in meat products by gas chromatography coupled to mass spectrometry.

    Science.gov (United States)

    Jiang, Yong; Ni, Yongnian

    2015-02-01

    A method was developed for the determination of clenbuterol in meat using stable-isotope-dilution gas chromatography with mass spectrometry coupled with solid-phase microextraction and on-fiber derivatization. The samples were first homogenized with hydrochloric acid followed by protein deposition. After headspace solid-phase microextraction and on-fiber derivatization, the content of clenbuterol was measured with the aid of stable-isotope dilution. The condition of solid-phase microextraction was optimized by central composite design. The relative standard deviations, limit of detection, and recoveries for clenbuterol were 4.2-9.2%, 0.48 μg/kg, and 96-104%, respectively. The proposed method was satisfactory for analysis of real samples as compared with the Chinese standard method. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Having the "Headspace" for Compassion Toward Self and Others: A Qualitative Study of Medical Students' Views and Experiences.

    Science.gov (United States)

    Tierney, Stephanie; Ozer, Cameron-Tosh; Perry, Sophie

    2018-01-31

    Phenomenon: Debate about compassion exhibited by healthcare professionals has escalated, following a perceived decline over recent years. At the same time, a growing interest in self-compassion has emerged, which is seen as facilitating compassion toward others. Little research has explored, in depth, what compassion to self and others means to medical students. Therefore, a study was designed to address this gap in knowledge. A qualitative study was conducted, involving students from all 4 years of a graduate-entry medical school in the United Kingdom. Focus groups were used to obtain the views of students on compassion for self and others (patients). Care was taken to achieve variation within the sample in terms of age, gender, and year of study. Focus groups were completed between September and October 2016. An inductive thematic analysis was performed. A total of 31 students participated in 4 focus groups, each lasting between 60 and 90 minutes. Having the cognitive freedom-"headspace"-to be aware of and respond to one's own and others' difficulties and distress was identified as an overarching theme within the data. This was underpinned by the themes developed during analysis: (a) bringing humanity into the workplace; (b) compassion as a variable, innate resource; (c) zoning into an individual's current needs; and (d) collective compassion. Students talked about the importance of being adaptable and responsive to situational factors in relation to self-compassion and compassionate care. They also highlighted the contribution of role models in promoting compassion to self and others. Insights: It is important for medical educators to explore ways of enhancing students' compassion to self and others during their training and beyond. Integrating approaches to "well-being" into the curriculum can create opportunities for self-compassion development, but rigid protocols could derail these efforts.

  12. Unbiased profiling of volatile organic compounds in the headspace of Allium plants using an in-tube extraction device

    OpenAIRE

    Kusano, Miyako; Kobayashi, Makoto; Iizuka, Yumiko; Fukushima, Atsushi; Saito, Kazuki

    2016-01-01

    Background Plants produce and emit important volatile organic compounds (VOCs), which have an essential role in biotic and abiotic stress responses and in plant?plant and plant?insect interactions. In order to study the bouquets from plants qualitatively and quantitatively, a comprehensive, analytical method yielding reproducible results is required. Results We applied in-tube extraction (ITEX) and solid-phase microextraction (SPME) for studying the emissions of Allium plants. The collected H...

  13. Tank 241-TX-118 headspace gas and vapor characterization results for samples collected in September 1994 and December 1994

    International Nuclear Information System (INIS)

    Huckaby, J.L.; Bratzel, D.R.

    1995-01-01

    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. Tank 241-C-105 headspace gas and vapor characterization results for samples collected in February 1994. Revision 1

    Energy Technology Data Exchange (ETDEWEB)

    Huckaby, J.L. [Pacific Northwest Lab., Washington, DC (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.

  15. Tank 241-BY-103 headspace gas and vapor characterization results for samples collected in May 1994 and November 1994

    Energy Technology Data Exchange (ETDEWEB)

    Bratzel, D.R.

    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