Chapter 11 - Introduction - Page 407

     One of the main challenges of separation scientists, in general, is to unravel the chemical profiles of complex, naturally occurring samples. Among the analytical techniques, gas chromatography (GC) is one of the most widely employed for such a purpose. GC was invented >60 years ago, and since then a considerable degree of progress has been made (James and Martin, 1952). The introduction of comprehensive two-dimensional GC (GC x GC) in 1991 by Liu and Phillips represents one of the most important steps toward the increase of separation power. In GC x GC experiments, the separation process is carried out on two columns of different selectivity. An interface, defined as the modulator, is located between the two capillaries, and generates a separation peak capacity, which is roughly equal to the product of the two peak capacities (peak capacity can be defined as “the number of peaks that can be potentially located in the one or two dimensional space, with a specific resolution value”) in each dimension. Comprehensive GC can be considered as an extension of conventional heartcut multidimensional GC, which involves the separation of specific fractions on two different columns with similar lengths. A comprehensive GC separation is obtained when all the components from the first dimension (1D), usually a conventional column (e.g., 25-30 m x 0.25 mm ID x 0.25 um), are reanalyzed on the second dimension (2D), commonly a short microbore capillary segment (e.g., 1-2 m x 0.10 mm ID x 0.10 um). 2D analyses are carried out in a rapid manner, with a duration equal to what is defined as the modulation period (typically in the 4-8 s range). In this chapter, GC x GC fundamentals will be discussed, along with the main applications in the lipid analysis field.

Click on the thumbnail graphics below to access the original full-size figure.

Handbook of Advanced Chromatography / Mass Spectrometry Techniques - Chapter11 Figure 1

Figure 11.1

GC x GC analysis of human plasma fatty acids. For peak identification refer to Tranchida et al. (2008b). GC, gas
chromatography.

Handbook of Advanced Chromatography / Mass Spectrometry Techniques - Chapter 11 Figure 2

Figure 11.2

Comparison of the second-dimension resolution between a traditional and a split-flow GC x GC system, in cod liver fatty acid methyl esters analysis; expansion of the C16 group. GC, gas chromatography.

Reproduced with permission from Purcaro, G., Tranchida, P.Q., Mondello, L., 2011. Comprehensive 2D GC methodologies for the analysis of lipids. In: Byrdwell, W.C., Holcapek, M. (Eds.), Extreme Chromatography: Faster, Hotter, Smaller. AOCS Press, Urbana, IL, pp. 381-430.

Handbook of Advanced Chromatography / Mass Spectrometry Techniques - Chapter 11 Figure 3

Figure 11.3

Two-dimensional chromatogram of menhaden fish oil sample obtained using GC-online hydrogenation x GCFID. FID, flame ionization detector; GC, gas chromatography.

Reproduced with permission from Delmonte, P., Fardin Kia, A.R., Rader, J.I., 2013. Separation of fatty acid methyl esters by GC-online hydrogenation x GC. Anal. Chem. 85, 1517-1524.

Handbook of Advanced Chromatography / Mass Spectrometry Techniques - Chapter 11 Figure 4

Figure 11.4

GC x GCetime-of-flight mass spectrometry total ion current (TIC)-chromatogram of a methylated and silylated lanolin sample (on the left). Inserted windows of extracted ions (m/z 74, 103, 147). FAL, fatty alcohol; FAME, fatty acid methyl ester; Hy-A, hydroxyl acids; ME, methyl derivative; TMS, trimethylsilyl derivative.

Reproduced with permission from Jover, E., Adahchour, M., Bayona, J.M., Vreuls, R.J.J., Brinkman, U.A.T., 2005. Characterization of lipids in complex samples using comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry. J. Chromatogr. A 1086, 2-11.

Handbook of Advanced Chromatography / Mass Spectrometry Techniques - Chapter 11 Figure 5

Figure 11.5

GC x GC chromatogram of minor components of an extra-virgin olive oil. FAAEs, fatty acid alkyl esters; GC, gas chromatography; MAG, monoacylglycerol.

Reproduced with permission from Purcaro, G., Barp, L., Beccaria, M., Conte, L., 2015. Fingerprinting of vegetable oil minor components by multidimensional comprehensive gas chromatography with dual detection. Anal. Bioanal. Chem. 407 (1), 309-319.

Handbook of Advanced Chromatography / Mass Spectrometry Techniques - Chapter 11 Figure 6

Figure 11.6

Scheme of the sequential process applied in the blueprint characterization of virgin olive oils by GC x GC. GC, gas chromatography.

Reproduced with permission from Purcaro, G., Cordero, C., Bicchi, C., Conte, L.S., 2014. Toward a definition of blueprint of virgin olive oil by comprehensive two-dimensional gas chromatography. J. Chromatogr. A 1334, 101-111.

Overview of the Contents:

The Handbook of Advanced Chromatography /Mass Spectrometry Techniques is a compendium of new and advanced analytical techniques that have been developed in recent years for analysis of all types of molecules in a variety of complex matrices, from foods to fuel to pharmaceuticals and more. Focusing on areas that are becoming widely used or growing rapidly, this is a comprehensive volume that describes both theoretical and practical aspects of advanced methods for analysis. Written by authors who have published the foundational works in the field, the chapters have an emphasis on lipids, but reach a broader audience by including advanced analytical techniques applied to a variety of fields.


Handbook of Advanced Chromatography / Mass Spectrometry Techniques

Key Features

Contains both practical and theoretical knowledge, providing core understanding for implementing modern chromatographic and mass spectrometric techniques Presents chapters on the most popular and fastest-growing new techniques being implemented in diverse areas of research.


Handbook of Advanced Chromatography / Mass Spectrometry Techniques

Table of Contents

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Handbook of Advanced Chromatography / Mass Spectrometry Techniques

Expected Readership

The Handbook is intended for upper level undergraduate students and graduate students, researchers, technicians, and scientists.It is also well suited for advanced analytical instrumentation students as well as for analysts seeking additional knowledge or a deeper understanding of familiar techniques.


Handbook of Advanced Chromatography / Mass Spectrometry Techniques

Book Details

No. of pages: 520
Copyright: © Academic Press and AOCS Press 2017
Published: September 11th 2017
eBook ISBN: 9780128117330
Paperback ISBN: 9780128117323