Headspace capillary gas chromatography

Schuberth J. 1994. Joint use of retention index and mass spectrum in postmortem test for volatile organics by headspace capillary gas chromatography with ion-trap detection. J Chromatogr A 674 63-71. 

Streete PJ, Ruprah M, Ramsey JD, et al. 1992. Detection and identification of volatile substances by headspace capillary gas chromatography to aid the diagnosis of acute poisoning. Analyst (London) 117(7) 1111-1127. 

Schroers, H.-J. and Jermann, E., Determination of physiological levels of volatile organic compounds in blood using static headspace capillary gas chromatography with serial triple detection, Analyst, 123, 715-720, 1998. 

Electronic nose technology and analysis of volatiles has long been apphed in the food industry to control the quahty of food products and to determine shelf hves. For example, sensor arrays based on different Sn02 gas sensors can be used to distingiush milk products of different rancidity levels [41]. Standard microbial test prediction of shelf hfe of milk products has a low level of reliability due to relatively poor correlation between microbial counts and actual shelf hfe. Several alternative methods have therefore been developed. One method is based on dynamic headspace capillary gas chromatography analyses of volatiles in mUk followed by MDA analyses. [42]. Principals of this method were later used for development of a faster and simpler test, where the extraction was performed by the SPME technique, the extracts... 

The method titled BTEX.mth will be retrieved from Turboehrom, External standard calibration curves will be generated using HS-C-GC-FID (headspace capillary gas chromatography with flame ionization detection). An aqueous environmental sample that has been contaminated with gasoline will be available and analyzed for traces of BTEX. 

Watanabe-Suzuki, K Seno, H. Ishii, A Kumazawa, T. Suzuki, O. (1999). Ultrasensitive method for the determination of ethanol in whole blood by headspace capillary gas chromatography with cryogenic oven trapping. Journal of chromatography B. 727,89-94... 

S. Raghavan, S. Reeder, and A. Khayat, Rapid analysis of vegetable oil flavor quality by dynamic headspace capillary gas chromatography, J. Am. Oil Chem. Soc. 66 942 (1989). 

Classification of wines according to the grape variety succeeds better, in general, because there are many more typical bouquet components (several hundreds) than mineral and trace elements being typical for the origin of wine. The organic compounds can be analyzed easily and reliably by Headspace Solid-Phase Microextraction Capillary Gas Chromatography and afterwards used for classification (De la Calle et al. [1998]). An example... 

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). 

Moens, L., DeSmaele, T., Dams, R., VandenBroeck, R and Sandra, P. (1997) Sensitive, simultaneous determination of organomercury, -lead, and -tin compounds with headspace solid phase microextraction capillary gas chromatography combined with inductively coupled plasma mass spectrometry. Anal. Chem., 69, 1604—1611. 

Solid-phase microextraction capillary gas chromatography (SPME-GC) is also an interesting preconcentration method. After derivatization with tetraethylborate, tetrapropylborate, or tetraphenylborate, the ethylated compounds are extracted by SPME on a silica fiber coated with polydimeth-ylsiloxane (PDMS). SPME can be performed either in the aqueous phase or in the headspace. After SPME extraction, species are thermally desorbed, separated by GC, and analyzed.106... 

K. Takekawa, M. Oya, A. Kido and O. Suzuki, Analysis of cyanide in blood by headspace solid-phase microextraction (SPME) and capillary gas chromatography, Chromatographia, 47, 209-214 (1998). 

J. Vercauteren, A. De Meester, T. De Smaele, F. Vanhaecke, L. Moens., R. Dams, P. Sandra, Headspace solid-phase microextraction-capillary gas chromatography-ICP mass spectrometry for the determination of the organotin pesticide fentin in environmental samples, J. Anal. Atom. Spectrom., 15 (2000), 651D656. 

McNeal TP, Nyman PJ, Diachenko GW, et al. 1993. Survey of benzene in foods by using headspace concentration techniques and capillary gas chromatography. Journal of AOAC International 76 1213-1219. 

Cobranchi, D. R, Botelho, M. W. B., Buck, R. C., Kaiser, M. A. Vaporpressure determinations of 8-2 fluorotelomer alcohol and 1-H perfluorooctane by capillary gas chromatography. Relative retention time versus headspace methods. J. Chromatogr. A, 1108 248-251 (2006). 

The volatiles of fresh pineapple (Ananas comosus [L] Merr.) crown, pulp and intact fmit were studied by capillary gas chromatography and capillary gas chromatography-mass spectrometry. The fnjit was sampled using dynamic headspace sampling and vacuum steam distillation-extraction. Analyses showed that the crown contains Cg aldehydes and alcohols while the pulp and intact fruit are characterized by a diverse assortment of esters, h rocarbons, alcohols and carbonyl compounds. Odor unit values, calculated from odor threshold and concentration data, indicate that the following compounds are important contributors to fresh pineapple aroma 2,5-dimethyl-4-hydroxy-3(2H)-furanone, methyl 2-methybutanoate, ethyl 2-methylbutanoate, ethyl acetate, ethyl hexanoate, ethyl butanoate, ethyl 2-methylpropanoate, methyl hexanoate and methyl butanoate. 

Mulligan, K.J. 1995. Acqueous alkylation of anions for static headspace sampling with analysis by capillary gas chromatography mass spectrometry. Journal of Microcolumn Separations 7 567-573. 

Lee Y.K., Nurok D. and Zlatkis A. (1978) Combined headspace profile analysis by capillary gas chromatography. J. Chromatogr. 158, 377-86. 

Theory of chromatography column efficiency expanded Chromatography simulation software for method development Capillary gas chromatography (GC) columns updated and expanded Headspace, thermal desorption, and purge and trap GC analysis Fast gas and hquid chromatography... 

Djozan, D. and Assadi, Y., A new porous-layer activated-cbarcoal-coated fused silica fiber application for determination of BTEX compounds in water samples using headspace sofid-phase microextraction and capillary gas chromatography, Chromatographia, 45(SuppL), S183-S189, 1997. 

SPME capillary gas chromatography (SPME-GC) can be used for the extraction of organometal compounds after these have been derivatized to a sufficiently volatile form (see also organotin speciation). A silica fiber coated with polydimethylsiloxane (PDMS) is brought into the (headspace) of the sample. After exposure, the fiber is inserted into the GC injection port and the compounds are thermally desorbed for subsequent analysis. This method has higher sensitivity compared to the injection of solvent on a capillary column (usually 1 fil) but requires the use of standard addition as a calibration method. After GC separation, analysis can be performed by furnace atomization plasma emission spectrometry (FARES)." ... 

About 50 mg were extracted with a mixture of H2S04/MeC00H in Milli-Q water (2 mL). The extract was injected in the headspace separation was by capillary gas chromatography (1 m length column with 3 mm internal diameter Chromosorb WAW 80-100 mesh loaded with 10% AT-1000 stationary phase injector temperature of 120°C, column temperature of 180 °C Ar as carrier gas at 100 mLmin ). Final detection was by atomic fluorescence spectrometry. Calibration was by standard additions, using MeHgCl in Milli-Q water as calibrant. 

Trace environmental quantitative analysis (TEQA) utilizes various determinative teehniques (Chapter 4) in combination with various sample prep techniques (Chapter 3). In this appendix, one specific trace analysis using static headspace sampling automatically coupled to capillary gas chromatography with element specific detection is described. LSQUARES is a computer program developed by the author in BASIC and is used in the quantitative analysis discussed below. The actual program written in GWBASIC is also listed after illustrating its use in TEQA. 

Figure 2 Analysis of a whole blood specimen (200 pi) from a patient who died after abusing a cigarette lighter refill and a typewriter correcting fluid containing 1,1,1-trichloroethane. GC conditions as for Figure 1. Injection 300 pi headspace. Detector sensitivities (fsd) FID 80 pA, ECD 2 kHz. Whole blood 1,1,1-trichloroethane concentration 1.2 mg I T (Reproduced with permission from Streets PJ, Ruprah M, Ramsey JD, and Flanagan RJ (1992) Detection and identification of volatile substances by head-space capillary gas chromatography to aid the diagnosis of acute poisoning. Analyst 117 1111-1127. The Royal Society of Chemistry.)...

Figure 3.2 Automated headspace sampling systems. Descriptions of each system are provided in text. Reproduced from Schomburg, G., Temperature programmed sample transfer, in Sample Introduction in Capillary Gas Chromatography (ed. P. Sandra), pp. 55-76 published by Huethig...

Kolb, B., Pospisil, P. and Auer, M. (1981) Quantitative analysis of residual solvents in food packaging printed films by capillary gas chromatography with multiple headspace extraction. Journal of Chromatography, 204, 371-6. 

Garcia, D. de la, C. Reichenacher, M. Danzer, K. Hurlbeck, C. Bartzsch, C. Feller, K.H. Analysis of wine bouquet components using headspace solid phase micro extraction-capillary gas chromatography. J. High Resol. Chromatogr. 1998, 21 (7), 373. 

Combined Headspace and Extraction Techniques for Profile Analysis by Capillary Gas Chromatography J. Chromatogr. 158 377-386 (1978) ... 

A desirability function was established to optimise the working conditions of a headspace solid-phase microextraction step, combined with capillary gas chromatography and ICP. 

Fig. 3. Combined headspace sampiing, themnai desorption and purge and trap injection system with exampie headspace chromatogram, (a) injection system (b) Headspace chromatogram. Detection of solvents In blood sample by headspace analysis as part of an Industrial hygiene study. Sample held at 60°C. Column UCON LB 550, 25 m, at 40°C. Produced tom D.W. Grant, Capillary Gas Chromatography, 1996. John Wiiey Sons Ltd. Reproduced with permission.

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