Multidimensional GC

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GCxGC Symposium

The GC×GC-7 symposium ran concurrently with this year?s ISCC in Riva del Garda, Italy. Speaking with The Column, Philip Marriott of the Australian Centre for Research on Separation Science, RMIT, Melbourne, Australia, said it ?offered the most comprehensive and thorough GCxGC programme yet assembled.?

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The misuse of androgenic anabolic steroids in sports was banned in 1976 by the International Olympic Committee and global sports community. The illegal use of anabolic steroids has reached disturbing levels worldwide. This worldwide problem is fueled partially by an ever-increasing demand for better athletic performance. The World Anti-Doping Agency has formulated strict guidelines for minimum allowable concentrations of exogenous anabolic steroids and their metabolites. The standard test methods for doping control are analyzed in urine samples with trimethyl-silyl derivatization. Urine is a complex and difficult biological matrix. This research shows the advantages of using comprehensive two-dimensional gas chromatography–time-of-flight-mass spectrometry (GCÃ-GC–TOF-MS) and illustrates the capability of GCÃ-GC-TOF-MS to be an effective instrumental option for antidoping control screening.

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Polybrominated diphenyl ethers (PBDE) are persistent environmental contaminants that are being extensively studied by environmental researchers worldwide. Their potential for toxicological impacts on humans and wildlife has made them a focal point of regulatory agencies. Their widespread use as flame retardants in electronics, household furniture, and many other building materials has lead to a need for analysis of many different sample matrices, including very complex environmental samples.

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Differential flow modulation is an inexpensive way to perform GCÃ-GC separations which has been attracting growing attention recently. Differential flow modulation uses high carrier gas flow rates in the second dimension column so it is widely thought that this rules out direct coupling with mass spectrometry. However direct coupled GCÃ-GC-QPMS using differential flow modulation is reported here for the first time using an unmodified mass spectrometer comprising a dual inlet turbomolecular pump and fast scanning quadrupole mass analyser. The suitability of the approach for characterization of essential oils is demonstrated.

Researchers Philip Marriott from the RMIT University (Melbourne, Australia), Warawut Tiyapongpattana, and Prapin Wilairat from the Mahidol University (Bangkok, Thailand) have developed a 2D GC with FID method for determining the composition of biofuels that extends to the C4-C24 esters. They reasoned that a 2D separation, based first on boiling point then on polarity, would provide better resolution of the components.

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Gas chromatography and comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (GC–TOFMS and GCxGC–TOFMS) were utilized to develop trace-level calibration curves in brewed green tea spiked with organochlorine and organophosphorus pesticide standards. A sensitive and robust calibration curve was developed from 10 to 500 parts per trillion (ppt), which allowed quantitative results to be determined for organochlorine–organophosphorus pesticides in brewed green tea. Exceptional limits of detection were achieved by GC–TOFMS and GCxGC–TOFMS at or below 10 ppt (solution concentration) for all but one of the pesticides. Stir bar sorption extraction (SBSE) was utilized to isolate the pesticide components from brewed green tea samples prior to analysis by GC–TOFMS and GCxGC–TOFMS. Different types of green tea were analyzed qualitatively by SBSE and GC–TOFMS with subsequent quantification for organochlorine–organophosphorus..