Page 346 - Multidimensional Chromatography
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Multidimensional Chromatography in Environmental Analysis       337

                              MDGC has also been used in the air analysis  field. For instance, it has been
                           applied to the analysis of volatile organic compounds (VOCs) in air, thus enabling a
                           wider range of these compounds to be analysed (18).
                              Today, however, GC–GC coupling is seldom used to determine pesticides in envi-
                           ronmental samples (2), although comprehensive MDGC has been applied to deter-
                           mine pesticides in more complex samples, such as human serum (19). On the other
                           hand, new trends in the pesticide market, which is now moving towards the produc-
                           tion of optically active enantiomers and away from racemic mixtures, may make this
                           area suitable for GC–GC application. The coupling of non-chiral columns to chiral
                           columns appears to be a suitable solution to the separation problems that such a trend
                           might cause.
                              Multidimensional gas chromatography has also been used in the qualitative anal-
                           ysis of contaminated environmental extracts by using spectral detection techniques
                           such as infrared (IR) spectroscopy and mass spectrometry (MS) (20). These tech-
                           niques produce the most reliable identification only when they are dealing with pure
                           substances; this means that the chromatographic process should avoid  overlapping
                           of the peaks.
                              Most applications in environmental analysis involve heart-cut GC–GC, while
                           comprehensive multidimensional gas chromatography is the most widely used tech-
                           nique for analysing extremely complex mixtures such as those found in the
                           petroleum industry (21).



                           13.2.2  EXAMPLES OF MULTIDIMENSIONAL GAS
                           CHROMATOGRAPHY APPLIED TO ENVIRONMENTAL ANALYSIS

                           A typical example of MDGC in environmental analysis is the determination of
                           PCBs. These are ubiquitous contaminants of the environment in which they occur as
                           complex mixtures of many of the 209 theoretically possible congeners. The compo-
                           sitions of environmental mixtures vary according to sample type.
                              Attempts to optimize the capillary GC separation conditions of 209 PCBs on a
                           single column of either single or mixed phases have had only limited success.
                           MDGC has therefore been very important. In some cases, mass spectrometry and, in
                           particular high-resolution mass spectrometry, may be enough to determine different
                           isomers which co-elute in a single column, and sensitivity may be enhanced by
                           selected ion monitoring (SIM) or negative chemical ionization (NCI).
                              In MDGC, the usual configuration normally has a non-polar phase (such as SE 54
                           or CPSil 8) on the first column to make the initial, well-characterized separation. The
                           sample is chromatographed on this column to a point just before the elution of the
                           unresolved peaks. The column flow is then switched into a second column of a dif-
                           ferent, usually more polar, phase such as CPSil 19 or CPSil88, for the duration of the
                           elution of these resolved peaks only. The column is again isolated and the small
                           group of unresolved peaks is separated on the second column (15). Other columns
                           which have been used include BPX5 (22), OV1(23) or Ultra 2 (11) as the  first
                           column, and HT8 (23), OV-210 (12, 24) or FFAP (14) as the second column.
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