Headspace Gas Chromatography-Mass Spectrometry

In instances where the chemical identity of some or all of the volatiles present in a polymer are not known it is possible to obtain the required information by the application of this technique. 

workers at Hewlett Packard [13] using this technique identified six volatiles in styrene-acrylonitrile-maleic anhydride terpolymer (benzene, toluene, ethylbenzene, styrene, aromatics, and maleic anhydride). 

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Arabin, A., Jacobsson, S., Hagman, A., and Ostelius, J. (1986), Studies on contamination of intravenous solutions from poly(vinyl chloride) bags with dynamic headspace gas chromatography-mass spectrometry and gradient liquid chromatography diode array techniques, Int. J. Pharm., 28,211-218. 

Montesinos, I., Gallego, M. Headspace gas chromatography-mass spectrometry for rapid determination of halonitromethanes in tap and swimming pool water. Anal. Bioanal. Chem. 402, 2315-2323 (2012)... 

The most detailed smdies on the flavor of fish oil in recent years were probably those of Hsieh et al. (78, 79), Lin et al. (80), and Lin (81). In their studies, a series of alkanals, alkenals, alkadienals, and alkatrienals were determined by dynamic headspace gas chromatography-mass spectrometry in cmde menhaden oils (Table 11). Most of these aldehydes contributed to the characteristic oxidized oily odors, such as green grassy, waxy, and rancid in the crude oils. Alkatrienals, i.e., nonatrienal and decatrienals, were also found at ppb levels in the dynamic headspace of the crude oils. 2-fraM5,4-frflMi,7-cA-Decatrienal, 2-fra 5,4-d5,7-di-decatrienal,... 

LA. Wash, A.H. Al-Awadhi, Z.N. Al-Hatali, EJ. Al-Rayami, N.A.A. Katheeri, Rapid and sensitive static headspace gas chromatography-mass spectrometry method for the analysis of ethanol and abused inhalants in blood, J. Chromatogr. B, 799, 331-336 (2004). 

Accorsi, A. Valenti, S. Barbieri, A. Raffi, G.B. Violante RS. (2003) Enflurane as an internal standard in monitoring halogenated volatile aneasthesics by headspace gas chromatography - mass spectrometry. Journal of chromatography A. 985,259-264... 

Ohno H, Kawamura Y. Analysis of vinylidene chloride and 1-chlorobutane in foods packaged with polyvinylidene chloride casing films by headspace gas chromatography/mass spectrometry (GC/MS). Food Addit Contam 2006 23 (8) 839-844. 

Table 5.6. Potent volatile compounds identified in fish oil enriched milk stored at 2°C by dynamic headspace gas chromatography-mass spectrometry/gas chromatography-olfactometry ...

Karlsson, S., Hakkarainen, M. and Mbertsson, A.-C. (1994) Identification by headspace gas chromatography-mass spectrometry of in vitro degradation products of homo- and copohmers of L- and D,L-lactide and l,5-dioxepan-2-one./ Chromatography A, 688, 251-259. 

Methods for the determination of volatiles in polymers are based principally on direct gas chromatography (GC) of solutions or extracts of the polymer, high-performance liquid chromatography (HPLC), polarography of solutions or extracts of the polymer, headspace analysis, headspace-gas chromatography-mass spectrometry (MS), and purge and trap analysis. These various techniques are discussed in the following sections. 

Takahashi, Y. Onodera, S. Morita, M. and Terao, Y. A problem in the determination of trihalomethane by headspace-gas chromatography/mass spectrometry. Journal of Health Science... 

Kallio, H. and Salorinne, L. 1990. Comparison of onion varieties by headspace gas chromatography-mass spectrometry. J Agric Food Chem 36 1560 1564. 

Nyman P.J., Diachenko G.W., Perfetti G.A., McNeal T.P., Hiatt M.H., Morehous K.M. Survey results of benzene in soft drinks and other beverages by headspace gas chromatography/mass spectrometry. Journal of Agricultural and Food Chemistry, 56 571 576 (2008). 

Jacq, K., Delaney, E., Teasdale, A., Eyley, S., Taylor-Worth, K., Lipczynski, A., Reif, V. D., Elder, D. P., Facchine, K. L., Oestrich, R. S., Sandra, P. and David, F. Development and validation of an automated static headspace gas chromatography-mass spectrometry (SHS-GC-MS) method for monitoring the formation of ethyl methane sulfonate from ethanol and methane sulfonic acid. J. Pharm. Biomed. Anal. 48 1339—1344, 2008. 

D. M. Wyatt, Dynamic headspace gas chromatography/mass spectrometry technique for determining volatiles in ambient stored vegetable oils, J. Chromatogr. Sci. 25 257 (1987). 

Bianchi, F., Careri, M., and Musci, M. (2005). Volatile norisoprenoids as markers of botanical origin of Sardinian strawberry-tree (Arbutus unedo L.) honey Characterisation of aroma compounds by dynamic headspace extraction and gas chromatography-mass spectrometry. Food Chem. 89,527-532. 

A. Lattuati Derieux, S. Thao, J. Langlois, M. Regert, First results on headspace solid phase microextraction gas chromatography/mass spectrometry of volatile organic compounds emitted by wax objects in museums, Journal of Chromatography A, 1187, 239 249 (2008). 

Y. F. Sha, S. Chen, G. L. Duan, Rapid determination of tramadol in human plasma by headspace solid phase microextraction and capillary gas chromatography mass spectrometry, J. Pharrn. Biomed. Anal., 37, 143 147 (2005). 

A. Lattuati Derieux, S. Bonnassies Termes, B. Lavedrine, Characterisation of compounds emitted during natural and artificial ageing of a hook. Use of headspace solid phase microex traction/gas chromatography/mass spectrometry, J. Cult. Her., 7, 123 133 (2006). 

M. Regert, V. Alexandre, N. Thomas, A. Lattuati Derieux, Molecular characterisation of birch bark tar by headspace solid phase microextraction gas chromatography mass spectrometry A new way for identifying archaeological glues, J. Chromatogr. A, 1101, 245 253 (2006). 

S. Hamm, E. Lesellier, J. Bleton, A. Tchapla, Optimization of headspace solid phase micro extraction for gas chromatography/mass spectrometry analysis of widely different volatility and polarity terpenoids in olibanum, J. Chromatogr. A, 1018, 73 83 (2003). 

For those aldehydes and ketones which are volatile enough, gas chromatography of the headspace gases can be used, and this has been used to measure acetone, butyraldehyde, and 2-butanone in oceanic waters. In a gas chromatography-mass spectrometry analysis of a single sample of volatile materials concentrated from inshore waters onto Tenax GC, MacKinnon [ 139] reported tentative identification of methyl isopropyl ketone, bromoform, 4-methyl-2-pentanone, 2-hexanone, and 2-hexanal. 

Bianchi AP, Vamoy MS, Phillips J. 1991. Analysis of volatile organic compounds in estruarine sediments using dynamic headspace and gas chromatography mass spectrometry. J Chromatogr 542 413-450. 

Yonamine M, TawU N, Moreau RL, Silva OA. 2003. Solid-phase micro-extraction-gas chromatography-mass spectrometry and headspace-gas chromatography of tetrahydrocannabinol, amphetamine, methamphetamine, cocaine and ethanol in saliva samples. J Chromatogr B Anal Technol Biomed Life Sci 789 73. 

Schoenmakers et al. [72] analyzed two representative commercial rubbers by gas chromatography-mass spectrometry (GC-MS) and detected more than 100 different compounds. The rubbers, mixtures of isobutylene and isoprene, were analyzed after being cryogenically grinded and submitted to two different extraction procedures a Sohxlet extraction with a series of solvents and a static-headspace extraction, which entailed placing the sample in a 20-mL sealed vial in an oven at 110°C for 5,20, or 50 min. Although these are not the conditions to which pharmaceutical products are submitted, the results may give an idea of which compounds could be expected from these materials. Residual monomers, isobutylene in the dimeric or tetrameric form, and compounds derived from the scission of the polymeric chain were found in the extracts. Table 32 presents an overview of the nature of the compounds identified in the headspace and Soxhlet extracts of the polymers. While the liquid-phase extraction was able to extract less volatile compounds, the headspace technique was able to show the presence of compounds with low molecular mass... 

Fig. 5.3. Odor changes that track floral color changes. Gas chromatography-mass spectrometry total ion chromatograms of floral headspace collected from young (upper trace) and old (lower trace) flowers of Lantana montevidense. Peaks 1,8,10, and 12 are metabolites of linalool (peak 3), all of which decrease dramatically with floral age and color change. Sesquiterpene hydrocarbons (peaks 4, 5, 9, and 11) show comparable decreases over time. Peaks 2, 6, 7, 13, and 14 are oxygenated aromatics and are present only in newly opened, rewarding flowers. Insert mass spectra highlight loss of phenylacetaldehyde ( peak 7) taken from young (a) and old (b) flowers. (M. R. Weiss and R. A. Raguso, unpublished data.)...

F. Vilaplana, M. Martinez-Sanz, A. Ribes-Greus, and S. Karlsson, Emission pattern of semi-volatile organic compounds from recycled styrenic polymers using headspace solid-phase microextraction gas chromatography - mass spectrometry, J. Chromatogr. A, In Press, Accepted Manuscript -, 2010. 

Headspace analysis is the method of choice for determining volatile organic compounds in soil [178-183]. A limitation of this method is the incomplete desorption of the contaminants in soil-water mixtures, but this problem can be overcome through the addition of methanol to the sample [181]. Good recoveries of volatile organic compounds in soils were obtained via thermal vaporisation of the sample followed by Tenax GC trapping and gas chromatography-mass spectrometry. 

Headspace analysis has been employed in the extraction of dithiocarbamate insecticide in vegetables [227]. Other techniques occasionally used are vacuum distillation followed by gas chromatography-mass spectrometry in the determination of volatile organic compounds in leaves, steam distillation in the determination of organochlorine insecticides in fruit and vegetables [229], and water distillation followed by high-performance liquid chromatography in the determination of 2-aminobutane in potatoes [102,230]. 

J., Gonzalez-Castro, M.J., De La Cruz Garcia, C. Determination of volatile 4.36 components in fresh, frozen, and freeze-dried Padron-type peppers by gas chromatography-mass spectrometry using dynamic headspace sampling and 4.37 microwave desorption. J. Chromatogr. 

Camara, J. S., Alves, M. A., and Marques, J. C. (2006c). Development of headspace solid-phase microextraction-gas chromatography-mass spectrometry methodology for analysis of terpenoids in Madeira wines. Anal. Chim. Acta 555,191-200. 

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