Sampling volatile organic compounds using a modified solid phase microextraction device

A method was developed for the analysis of volatile polar compounds in a water matrix using open cap vials Solid Phase Micro-Extraction (SPME) and Capillary Gas Chromatography (CGC). Both SPME techniques – direct sampling and headspace – were tested. Optimization of experimental conditions – exposure time, desorption time, with headspace SPME in addition the influence of the temperature and ionic strength of the sample solution on compound sorption, and finally GC response – were investigated. The analytes were extracted by directly immersing the 85 μm polyacrylate fiber in the aqueous sample or in the headspace. The linear range of the preconcentration process and the precision were examined. The amount of polar analytes sorbed on the fiber was determined and was found to be concentration dependent; it amounted to 0.014–0.64% in the concentration range of 0.00425–425 ppm studied in aqueous solution for direct sampling SPME and to 0.011–2.76% for solutions of concentration 0.0425–255 ppm for headspace SPME. The limits of determination were ascertained. Headspace SPME was applied to the analysis of real-life samples.

To comprehensively understand the volatile compounds and assess the aroma profiles of different types of Pyrus ussuriensis Maxim. Anli, Dongmili, Huagai, Jianbali, Jingbaili, Jinxiangshui, and Nanguoli were detected via headspace solid phase microextraction (HS-SPME) coupled with two-dimensional gas chromatography/time-of-flight mass spectrometry (GC×GC-TOFMS). The aroma composition, total aroma content, proportion and number of different aroma types, and the relative quantities of each compound were analyzed and evaluated. The results showed that 174 volatile aroma compounds were detected in various cultivars, mainly including esters, alcohols, aldehydes, and alkenes: Jinxiangshui had the highest total aroma content at 2825.59 ng/g; and Nanguoli had the highest number of aroma species detected at 108. The aroma composition and content varied among pear varieties, and the pears could be divided into three groups based on principal component analysis. Twenty-four kinds of aroma scents were detected; among them, fruit and aliphatic were the main fragrance types. The proportions of aroma types also varied among different varieties, visually and quantitatively displaying changes of the whole aroma of the different varieties of pears brought by the changes in aroma composition. This study contributes to further research on volatile compound analysis, and provides useful data for the improvement of fruit sensory quality and breeding work.

P36: Évaluation of fetal exposure to environmental pollutants by quantification of volatile organic compounds, pesticides and associated metabolites in meconium

The aim of this study was to investigate the diversity of Bacillus species in dawadawa; aiding potential starter cultures selection for alkaline fermentation of bambara groundnut into dawadawa-type condiments based on their genotypic and volatile compound profiles. Bacillus species (n = 71) isolated from spontaneously fermented dawadawa were identified using matrix assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF MS) as B. cereus (35%), B. licheniformis (30%), B. pumilus (21%), B. subtilis (10%) and B. amyloliquefaciens (4%). Further molecular typing was performed using GTG5 rep-PCR typing, 16S rRNA and gyrA gene sequencing. The gyrA gene sequence analysis exhibited the highest species discriminatory power with B. subtilis subsp. subtilis, B. amyloliquefaciens subsp. plantarum, B. pumilus and B. licheniformis as the distinct clusters. Representative strains from each cluster were then used as starter cultures for the production of dawadawa from bambara groundnut. Volatile compounds analysis using headspace solid phase microextraction (SPME) and comprehensive gas chromatography coupled to time of flight mass spectrometry (GC × GC–TOF MS) identified distinct chemical profiles produced by each of the four strains. Volatile compounds produced by B. subtilis subsp. subtilis (strain SFBA3) were categorized by dimethyl disulfide, methanethiol and nonanal while B. amyloliquefaciens subsp. plantarum (strain SFBA2) produced acetic acid and hexadecanoic acid. B. cereus (strain PALB7) produced 2,5-dimethyl pyrazine and 2-butanone which were not detected in the other condiments. Hexanal was the main compound produced by B. licheniformis (strain OALB7).

The chemical compositions of the essential oils (EOs) of roots, young and old leaves and stems, and flowers of Pittosporum tobira (Thunb.) W.T. Aiton cultivated in Tunisia and of the volatile organic compounds (VOCs) emitted by the powder of each organ were identified. The EOs are extracted from fresh material by hydrodistillation, whereas the VOCs are obtained by head space solid-phase microextraction (HS-SPME) from the powdered dry tissues. Fifty-eight VOCs are identified, while, 105 components are detected for the EOs. The main EOs compounds are α-neoclovene, β-caryophyllene and limonene in roots (22.56, 12.52, and 8.59 %, respectively), viridiflorol in young stems, flowers and young leaves (34.90, 31.60, and 24.60 %, respectively), α-cadinol in young stems and leaves, and flowers (13.80, 10.40, and 9.10 %, respectively), (E)-nerolidol in flowers (13.30 %), and germacrene D in old stems (9.06 %). The major detected VOCs are n-undecane, mainly in young and old leaves (71.40 and 40.90 %, respectively), n-nonane in young leaves and flowers (31.80 and 27.10 %, respectively), α-cubebene in old stems and flowers (22.60 and 15.50 %, respectively), and α-gurjunene and β-gurjunene in roots (14.20 and 12.20 %, respectively). Principal Component Analysis (PCA) carried out on the 26 main volatile compounds (relative content exceeding 6 %) identified both by HS and in the EOs allowed their classification into two groups; compounds specific to roots and those specific to aerial parts. The later are subdivided in to two subgroups; old leaves and stems compounds subgroup, and young leaves and stems, and flowers one. We can notice that the two methods used to extract P. tobira volatile compounds and identify them are complementary. This study defines and differentiates, for the first time, the specific aroma profile of P. tobira from Tunisia. In addition to its ornamental value, all the organs of this species, could be valued as a source of volatile compounds useful in perfume, cosmetics and as food flavoring products.

Theory and protocol of dual mode unity solid-phase microextraction

Grumixama (Eugenia brasiliensis Lam.) is a native fruit of the Brazilian Atlantic Forest, belonging to the Myrtaceae family, which designatesthe most significant number of species with food potential. It stands out due to its phytochemical characteristics because of the presence of polyphenols and volatile organic compounds. Volatile compounds are substances released by foods that give off an aroma and influence flavor. Solid-phase microextraction is a technique that allows for low-cost, fast, and solvent-free extraction, has an affinity for numerous analytes, and is easily coupled to gas chromatography. The objectives of this work were to evaluate the efficiency of different fibers of SPME (solid-phase microextraction) in the extraction of volatile organic compounds from grumixama pulp; optimize a method for extraction time, temperature, and sample weight; and to determine the characteristic volatile profile of this fruit. For the extraction of volatile compounds, three fibers of different polarities were used: polar polyacrylate (PA) fibers, divinylbenzene/carboxyne/polydimethylsiloxane (DVB/CAR/PDMS) semipolar fibers, and polydimethylsiloxane/divinylbenzene (PDMS/DVB). Fourteen volatile organic compounds (VOCs) were identified by DVB/CAR/PDMS, six by PA, and seven by PDMS/DVB through solid-phase microextraction in the headspace mode (SPME-HS). Considering the total number of compounds identified, regardless of the fiber used, and the optimization of the method, Eugenia brasiliensis presented sesquiterpene fractions (85.7%, 83.3%, and 85.7% of total VOCs) higher than the monoterpene fractions (14.3%, 16.7%, and 14.3%) for DVB/CAR/PDMS, PA, and PDMS/DVB, respectively in its composition. In addition, it was possible to verify that the fiber DVB/CAR/PDMS presented a better efficiency due to the larger chromatographic area observed when the grumixama pulp was subjected to conditions of 75 °C, 2.0 g, and an adsorption time of 20 min.

Fungi and oomycetes are important plant pathogens that constantly attacked plants, thus compromising the production of foods worldwide. Streptomyces strains might be useful to control fungal pathogens by different mechanism. The in vitro antagonistic activity of non-volatile and volatile metabolites from four Streptomyces strains was evaluated over cultures of phytopathogenic fungi and oomycetes. The non-volatile compounds from Streptomyces strains significantly reduced (44.2 to 92.1%) the growth of aerial mycelium of pathogens. The volatile compounds (VOCs) from Streptomyces strains reduced both aerial mycelium (22.5 to 96.7%) and mycelium growing inside of culture medium (0.0 - 9.4%). The pathogens maintained their capacity to grow normally in fresh culture medium without antagonists after confrontations with antagonist VOCs. The analysis of VOCs by gas chromatography coupled to mass spectrometry revealed different kinds of VOCs included alcohols, aldehydes, ketones, esters, terpenes, terpenoids, thioethers, among others. The most abundant VOCs were trans-1,10-dimethyl-trans-9-decalol (geosmin), 2-methylisoborneol, 2-methyl-2-bornene, 1,4-dimethyladamantane, and 4-penten-1-ol, trifluoroacetate. The antipathogenic activity of nine pure VOCs that had been identified in cultures of the Streptomyces strains alone was evaluated in vitro against phytopathogenic fungi and oomycetes. Trans-2-hexenal was the most effective of these VOCs, inhibiting completely the growth of tested phytopathogens. The volatile and non-volatile compounds from Streptomyces strains effectively reduced the in vitro growth of phytopathogens and they might be used as biological control. Further studies are required to demonstrate this activity on open field conditions.

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

Preface Overview 1. The Significance of Volatile Sulfur Compounds in Food Flavors Robert J. McGorrin Volatile Sulfur Analysis 2. Challenges and Artifact Concerns in Analysis of Volatile Sulfur Compounds Eric Block 3. The Role of Separation in the Identification of Trace Aroma Compounds J. Lin, Y. Wang, P. L. Perry, E. Frerot, A. Rada, and J. Impellizzeri 4. Emerging Analytical Techniques for the Assessment of Aroma Relevant Sulfur Compounds in Coffee Luigi Poisson, Christine Hug, Juerg Baggenstoss, Imre Blank, and Josef Kerler 5. Progress on Volatile Sulfur Compound Analysis in Wine Peter M. Davis and Michael C. Qian Volatile Sulfur Compounds in Food Systems 6. Recent Advances in Volatile Sulfur Compounds in Cheese: Thiols and Thioesters A. M. Sourabie, H.-E. Spinnler, A. Saint-Eve, P. Bonnarme, and S. Landaud 7. Contribution of Volatile Sulfur Compounds to the Characteristic Aroma of Roasted Garlic Keith Cadwallader, David Potts, Laura Brisske-BeVier, and Samira Mirarefi 8. Analysis of Volatile Sulfur Compounds in Swiss Cheese Using Selected Ion Flow Tube Mass Spectrometry (SIFT-MS) W. James Harper, Nurdan A. Kocaoglu-Vurma, Cheryl Wick, Karen Elekes, and Vaughan Langford 9. Volatile Compounds of the Genus Allium L. (Onions) Prof. Dr. Michael Keusgen 10. Sulfur Compounds in Still and Sparkling Wines and in Grappa: Analytical and Technological Aspects Bruno Fedrizzi, Giuseppe Versini, Roberto Ferrarini, Fabio Finato, Giorgio Nicolini, and Franco Magno Volatile Sulfur Compound Formation in Food Systems 11. Determination of Volatile Sulfur Compounds Formed by the Maillard Reaction of Glutathione with Glucose Sang Mi Lee and Young-Suk Kim 12. Volatile Sulfur Compounds in Foods as a Result of Ionizing Radiation Xuetong Fan, Eun Joo Lee, and Dong Ahn 13. Volatile Compounds Formed from the Interaction between Organoselenium and Sulfur Compounds Guor-Jien Wei and Chi-Tang Ho 14. Analysis and Formation of Key Sulfur Aroma Compounds in Wine M. J. Herderich, I. L. Francis, M. Ugliano, T. E. Siebert, and D. W. Jeffery Sensory and Bioactivity of Volatile Sulfur Compounds 15. Understanding Aroma Impact of Four Important Volatile Sulfur Compounds in Oregon Pinot Noir Wine I-Min Tsai and Mina R. McDaniel 16. Antimicrobial Activity of Volatile Sulfur Compounds in Foods Kyu Hang Kyung Editors' Biographies Indexes Author Index Subject Index

Aroma is an important fruit sensory attributes that is influenced by the volatile compounds present in the fruit, and it determines whether a fruit is acceptable to consumers. The volatile compounds in 11 pear cultivars from different species were investigated by headspace solid phase microextraction and gas chromatography-mass spectrometry. In total, 70 volatile compounds, including three alcohols, six aldehydes, fifty-two esters, three acids, three terpenes and three ketones were identified and quantified. Ester was the dominant chemical class of which a total of 52 compounds were detected. Hexanal, hexyl acetate, ethyl hexanoate, ethyl 2-methylbutanoate and ethyl butanoate were the major volatile compounds. Pyrus ussuriensis Maxim showed a higher concentration of volatiles and higher ester content than in the other Asian pear species studied. Cultivars were clearly grouped into four clusters based on the concentration and number of different volatile compounds present in each cultivar. The clusters of different cultivars could be discriminated from each others using the first two principal components. The volatile profiles of the pears were qualitatively and quantitatively influenced by the cultivar. Key words: Pyrus, Asian pear, volatile compound, gas chromatography mass spectrometry (GC-MS), solid phase microextraction (SPME), multivariate analysis.

A senior-level undergraduate laboratory experiment that demonstrates the use of solid-phase microextraction (SPME) and capillary gas chromatography-mass spectrometry (GC-MS) was developed for the identification of volatile compounds in consumer products. SPME minimizes sample preparation and concentrates volatile analytes in a solvent-free manner.

Guangdong black teas have diverse flavors and aromas. To explore the molecular basis of these aromas, we extracted and analyzed the volatile flavor compounds of 31 black tea samples from 7 districts (Yingde, Luokeng, Renhua, Meizhou, Chaozhou, Lianshan, and Heyuan) in Guangdong Province with headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography–mass spectrometry (GC–MS). Then, 135 volatile flavor compounds (VFCs) were identified and grouped into 12 classes according to their chemical structure. Notably, alcohols accounted for 31.40–44.43% of total VFCs. The score plot of supervised partial least squares-discriminant analysis (PLS-DA) revealed good discrimination for most black tea samples. Additionally, 64 compounds with variable importance in projection > 1.0 were identified as differential odorants. Through an odor activity value analysis, eight volatile compounds were identified as the key active differential VFCs: linalool, methyl salicylate, phenylethyl alcohol, p-cresol, 3-methyl-butanoic acid, geraniol, benzaldehyde, and benzeneacetaldehyde. Thus, benzeneacetaldehyde and linalool in YJ-Yingde samples, benzaldehyde in Luokeng samples with an almond-like aroma, phenylethyl alcohol in the Heyuan samples, and p-cresol and 3-methyl-butanoic acid in the Chaozhou samples were the key volatile flavor compounds that could differentiate local black teas from other black teas. These findings will enrich the research in tea aroma chemistry and provide a method for identifying the origins of Guangdong black teas.

In this study, the volatile compound profiles of gurum seed oil were determined using two methods: supercritical CO2 extraction (SFE) and the screw press process (SPP). For volatile compounds extraction and identification, headspace solid-phase micro-extraction (HS-SPME) and GC–MS were used, respectively. A total number of 56 volatile compounds were revealed and identified in oil extracted by SFE, while only 40 compounds were detected in extracted oil by SPP. Acids, aldehydes, esters, ketones, furans, and other components were present in the highest ratio in oil extracted by SFE. In contrast, alcohols and alkenes were found in the highest proportion in oil extracted by SPP. In this study, it was observed that SFE showed an increase in the amounts of volatile compounds and favorably impacted the aroma of gurum seed oil. The results reveal that different extraction methods significantly impact the volatile components of gurum seed oil, and this study can help evaluate the quality of the oil extracted from gurum seeds.

Solid phase microextraction (SPME) has been shown to be an effective tool for analysing volatile compounds. The aim of this study was to optimise the conditions for the application of SPME in the analysis of volatile compounds in dry‐cured ham. The effects of exposure time and fibre coating were investigated while maintaining the dry‐cured ham at 30 °C to avoid artefact generation due to possible temperature effects. A divinylbenzene/Carboxen on polydimethylsiloxane (DVB/CAR/PDMS) coating showed the best extraction performance for medium‐ and high‐molecular‐weight analytes, whilst a Carboxen on polydimethylsiloxane (CAR/PDMS) coating gave the best results for low‐molecular‐weight compounds. A total of 70 different compounds were extracted by the two fibre coatings and identified. Sixty compounds were extracted by the DVB/CAR/PDMS fibre, whilst only 41 of these were found with the CAR/PDMS fibre. On the other hand, 10 additional volatile compounds were extracted by the CAR/PDMS coating, all of them being of low molecular weight. Two of the major compounds extracted, hexanal and 2‐pentanone, were found in high proportion in both fibre coatings. The extraction yields of dry‐cured ham volatile compounds varied according to the fibre coating used and the time of exposure. Therefore extraction conditions should be selected depending on the objective of the study.© 2002 Society of Chemical Industry