Gas chromatography-mass spectrometr

Greaves et al. [74] used a selected ion-monitoring assay method for the determination of primaquine in plasma and urine using gas chromatography-mass spectrometric method and a deuterated internal standard. After freeze-drying and extraction with trichloroethylene, the sample plus internal standard was reacted with Tri Sil TBT (a 3 3 2 by volume mixture of trimethylsilylimidazole, A/O-bis-(trimethylsilylacetamide and trimethylchlorosilane) and an aliquot injected to the gas chromatograph-mass spectrometer. The gas chromatographic effluent was monitored at m/z 403, and m/z 406, the molecular ions of the bis-tetramethylsilane ethers of primaquine and 6-trideuteromethoxy primaquine. 

D. Fabbri, G. Chiavari, S. Prati, I. Vassura and M. Vangelista, Gas chromatography/mass spectrometric characterisation of pyrolysis/silylation products of glucose and cellulose, Rapid Commun. Mass Spectrom., 16, 2349 2355 (2002). 

The Chem Master Workstation is a gas chromatography and gas chromatography-mass spectrometry data-processing system that speeds the flow of data through the laboratory and provides essential quality-assurance and quality-control review. It is a PC-based integrated hardware/ software system that converts gas chromatographic and gas chromatography-mass spectrometric data into reliable analytical reports. 

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. [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]. 

Ishmatari, R. and Hanya, T. (1974) Gas chromatography-mass spectrometric detection of organic compounds in a river water. Proceedings International Meeting Ed. Technig. 6th, 1051. 

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. 

Alford Stevens et al. [49] carried out a multi-laboratory study of automated gas chromatography-mass spectrometric determinations of polychlorinated biphenyls in soil. The influence of various factors on the accuracy of analytical results were studied. Shaker extraction for 12.5h followed by Florisil chromatography were demonstrated to be the most reliable methods for extraction and clean-up. 

Representative multiple ion mass chromatograms of soil samples are presented in Fig. 5.4. These gas chromatography-mass spectrometric determinations of polychlorodibenzo-p-dioxin and polychlorodibenzofurans, and non-ortho polychlorobiphenyls in differing types of samples serve to exemplify the versatility of the procedure for such analyses. The gas chromatography-mass spectrometric data were usually uncluttered by extraneous components, and interpretation of the data was routinely straightforward. 

An isotope dilution gas chromatography-mass spectrometric method [16] has been applied to the determination of Diazinon at the 0.1-lpg kgy1 level in soils. Accuracy exceeds 86% while precision is better than 8%. 

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. 

Janini, GM., Muschik, G.M., Schroer, J.A., and Zielinski, W.L., Gas-liquid-chromatographic evaluation and gas-chromatography mass spectrometric application of new high-temperature hquid-crystal stationary phases for polycyclic aromatic hydrocarbon separations. Ana/. Chem., 4S, 1879, 1976. 

Loutelier-Bourhis C, Legros H, Bonnet JJ, Costentin J, Lange CM. 2004. Gas chromatography/mass spectrometric identification of dopaminergic metabolites in striata of rats treated with L-DOPA. Rapid Commun Mass Spectrom 18 571. 

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. 

Gas Chromatography-Mass Spectrometric Characterization of Polynuclear Aromatic Hydrocarbons in Particulate Diesel Emissions... 

Lopshire [188] explored the exchange reaction of chlorine by oxygen with polychlorobiphenyl anions as a method of compound-selective polychloro-biphenyl congener detection in a gas chromatography-mass spectrometric system. Multiple reaction monitoring allowed separate chromatograms to be detected for each different polychlorobiphenyl composition from tetra-through nonachloro. 

Hauser, B., P. Popp, and E. Kleine-Benne (2002). Membrane-assisted solvent extraction of triazines and other semi-volatile contaminants directly coupled to large-volume injection-gas chromatography-mass spectrometric detection. J. Chromatogr. A, 963 27-36. 

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. 

Matthias et al. [216] have described a comprehensive method for the determination of aquatic butyltin and butylmethyltin species at ultratrace levels using simultaneous sodium borohydride hydridisation, extraction with gas chromatography-flame photometric detection and gas chromatography-mass spectrometric detection. The detection limits for a lOOmL sample were 7ng L 1 of tin for tetrabutyltin and tributyltin, 3ng L 1 of tin for dibutyltin and 22ng L 1 tin for monobutyltin. For 800mL samples detection limits were l-2ng L 1 tin for tri- and tetrabutyltin and below lng L 1 tin for dibutyltin. The technique was applied to the detection of biodegradation products of tributyltin in non saline waters. 

Johnson, L. P., McLeod, J. K., Summons, R. E., and Hunt, N. (1980). Design of a stable isotope dilution gas chromatography/mass spectrometric assay for cAMP Comparison with standard protein-binding and radioimmunoassay methods, Anal. Biochem. 106,285-290. 

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

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

Saraji, M. Mousavinia, F. 2006. Single-drop microextraction followed by in-syringe derivatization and gas chromatography-mass spectrometric detection for determination of organic acids in fruits and fruit juices. J. Sep. Sci. 29 1223-1229. 

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. 

Wang, K.D., Chen, P.S., Huang, S.D. Simultaneous derivatization and extraction of chloro-phenols in water samples with up-and-down shaker-assisted dispersive liquid-liquid microextraction coupled with gas chromatography/mass spectrometric detection. Anal. Bioanal. Chem. 406, 2123-2131 (2014)... 

Lee ML, Novotny M, Bartle KD (1976) Gas chromatography/mass spectrometric and nuclear magnetic resonance determination of polynuclear aromatic hydrocarbons in airborne particulates. Anal Chem 48 1566-1572. 

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. 

---