Gas chromatography-mass spectrometric analysis

Lopez-Avila et al. [59] used microwave assisted extraction to assist the extraction of polyaromatic hydrocarbons from soils. Another extraction method was described by Hartmann [60] for the recovery of polyaromatic hydrocarbons in forest soils. The method included saponification of samples in an ultrasonic bath, partitioning of polyaromatic hydrocarbons into hexane, extract cleanup by using solid-phase extraction, and gas chromatography-mass spectrometric analysis using deuterated internal standards. Polyaromatic hydrocarbons were thermally desorbed from soils and sediments without pretreatment in another investigation [61]. 

Fig. 11.4 shows the total ion current trace and some mass chromatograms obtained by flash evaporation pyrolysis gas chromatography-mass spectrometric analysis of the polluted sediment sample. All compounds present in this complex mixture were not listed. A selection was made to exemplify several aspects of the screening approach. The peak number correspond with the numbers in Table 11.1. Identifications were based on the same criteria as mentioned above. Although several components were shown to be real pyrolysis products, all the compounds are present as such in the sample and resulted from simple thermal extraction from the wire. This was shown in separate analyses using ferromagnetic wires with a Curie temperature of 358°C. 

L. Hou, G. Shen and H. K. Lee, Automated hollow fiber-protected dynamic liquid-phase microextraction of pesticides for gas chromatography-mass spectrometric analysis. Journal of Chromatography A, 2003, 985(1-2), 107-116. 

Pardasani, D., M. Palit, A.K. Gupta, P.K. Kanaujia, K. Sikhar, and D.K. Dubey. 2006. Microemulsion mediated in situ derivatization-extraction and gas chromatography-mass spectrometric analysis of alky-Iphosphonic acids. J. Chromatogr. A 1108 166-175. 

ANALYTICAL DERIVATIZATION FOR GAS CHROMATOGRAPHY/ MASS SPECTROMETRIC ANALYSIS... 

Prouteau, C., Schneider, R., Lucchese, Y., Nepveu, F, Renard, R., and Vaca-Garda, C. (2004). Improving headspace-solid-phase microextraction of 3-isobutyl-2-methoxypyrazine by experimental design with regard to stable isotope dilution gas chromatography-mass spectrometric analysis of wine. Anal. Chim. Acta, 513, 223-227. 

Insa, S., Antico, E., and Ferreira, V. (2005). Highly selective solid-phase extraction and large volume injection for the robust gas chromatography-mass spectrometric analysis of TCA and TBA in wines, J. Chromatogr. A, 1089,235-242. 

Zuo, Y. Zhang, K. Lin, Y. Microwave-accelerated derivatization for the simultaneous gas chromatography-mass spectrometric analysis of natural and synthetic estrogenic steroids. J. Chromatogr. A, 2007,1148, 211-218. 

Pardasani, D., et al. (2005) Gas chromatography/mass spectrometric analysis of methyl esters of NJSl-dialkylaminoethane-2 sulfonic acids for verification of the Chemical Weapons Convention. Rapid Communications in Mass Spectrometry, 19, 3015-3020. 

Chiantore, O., Riedo, C., Scalarone, D. (2009) Gas chromatography-mass spectrometric analysis of products from on-hne pyrolysis/sUylation of plant gums used as binding media. International Journal of Mass Spectrometry, 284,35-41. 

Gas Chromatography-Mass Spectrometric Analysis of Organic Acids in Human Cerebrospinal Fluid Koensju - lyo Masu Kenfcy ukai 4 289-292 (1979) CA 92 193769p... 

Silyl ethers are formed with carbohydrate hydroxyl groups by reaction with chlorotrimethylsilane in pyridine with hexamethyldizilazane. Trimethylsilyl ethers are stable in neutral and basic condition but are hydrolyzed in aqueous acidic conditions [18]. The major uses of the silyl ethers is the formation of highly volatile carbohydrate derivatives that can be used in gas chromatography and gas chromatography/mass spectrometric analysis [19,20]. 

The Curie Point flash evaporation-pyrolysis gas chromatography-mass spectrometric method [32] described in section 2.2.1.2 for the analysis of aromatic hydrocarbons in soils has also been applied to the determination of heteroaromatic compounds (Table 2.2) such as methyledene, isomeric methylidenes, biphenyl and methylbenzofurans. 

Lopez-Avila et al. [36] used a stable isotope dilution gas chromatography-mass spectrometric technique to determine down to O.lppb of pentachlorophenol (also Atrazine, Diazinon and lindane) in soil. Soil samples are extracted with acetone and hexane. Analysis is performed by high-resolution gas chromatography-mass spectrometry with mass spectrometer operated in the selected ion monitoring mode. Accuracy greater than 86% and a precision better than 8% were demonstrated by use of spiked samples. 

Macleod KE, Hanisch RC, Lewis RG. 1982. Evaluation of gel permeation chromatography for clean up of human adipose tissue samples for gas chromatographic-mass spectrometric analysis of pesticides and other chemicals. J Anal Toxicol 6(1) 38-40. 

Rosel I, A., Gomez-Behnehon, J.L, and Grimalt, J.O., Gas Chromatographic-Mass Spectrometric Analysis of Urban-Related Aquatic and Airborne Volatile Organic Compounds Study of the Extracts Obtained by Water Closed-Loop Stripping and Ah Adsorption with Charcoal and Polyurethane Foam, Journal of Chromatography. Biomedical Applications, Vol. 562, p 493-506. 1991. 

The method involves chloroform extraction of acidified waste water samples and rotary evaporation without heat. After redissolving in chloroform the samples were analysed directly by high performance liquid chromatography on a microparticulate silica gel column. A number of solvent combinations are possible and 98 2 cyclohexane-acetic acid is preferred. The minimum detectable concentration is lppm (without sample concentration) and the coefficient of variation is 1-2%. The type of separation achieved with a microparticulate silica gel column is shown in Fig. 4.1. The first peak as determined by gas chromatographic-mass spectrometric analysis, consisted of a complex mixture of polychlorinated compounds, including octa-, hepta- and hexachlorodibenzo-/ -... 

Tabanca, N., Demirci, B., Ozek, T., Kirimer, N., Baser, K.H.C., Bedir, E., Khan, I.A. and Wedge, D.E. (2006) Gas chromatographic-mass spectrometric analysis of essential oils from Pimpinella species gathered from Central and Northern Turkey, Journal of Chromatography A 1 11 7(2), 194-205. 

Fig. 9.1.2. Compounds identified in the phenolic fraction of a bleach plant E effluent by gas chromatography-mass spectrometric (GC-MS) analysis...

Tsuge, K., Seto, Y. (2006). Detection of human bufyryl-cholinesterase-nerve gas adducts by liquid chromatography-mass spectrometric analysis after in gel chymotryptic digestion. J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. 838 21-30. 

Wong, J.W., Webster, M.G., Halverson, C.A., Hengel, M.J., Ngim, K.K., and Ebeler, S.E. (2003) Multiresidue pesticide analysis in wines by solid-phase extraction and capillary gas chromatography-mass spectrometric detection with selective ion monitoring,/. Agric. Food Chem., 51(5), 1148-1161. 

Ng LK, Lafontaine P, and Harnois J (2000) Gas chromatographic-mass spectrometric analysis of acids and phenols in distilled alcohol beverages - application of anion-exchange disk extraction combined with in-vial elution and silylation. Journal of Chromatography A 873 29-38. 

Our personal experience with gas chromatographic-mass spectrometric analysis of bile acids is limited to the use of a modified Atlas CH-4 mass spectrometer connected to the gas chromatography column via a molecule separator of the jet type (8, 16), and to the use of prototypes and production models of the LKB 9000 instrument. 

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