Comprehensive GCxGC System

Comprehensive GC-MS (GCxGC-MS) System is a powerful technique that provides two-dimensional chromatography data acquisition capability. Shimadzu’s Comprehensive GC-MS (GCxGC-MS) System is suited for a variety of applications, including analysis of complex matrices such asa natural products that are hard analyze by conventional GC or GC-MS, and grouping analysis based on two-dimensional chromatograph patterns.

Comprehensive GC-MS (GCxGC-MS) System is a powerful technique that provides two-dimensional chromatography data acquisition capability.

APPLICATIONS

Food, Flavor & Fragrance, Environment, Petrochemical etc,

FEATURES

Separation of Overlapping Peaks

Peaks with similar boiling points that could not be separated adequately with one-dimensional chromatography can now be separated based on differences in polarity. This allows analysis of components that previously were difficult to separate in samples with complex matrices.

Image Patterns Show Compound Structure

GCxGC provides image patterns that can be correlated to compound structure; this capability is especially useful for grouping analysis of mixtures containing many components.

Analysis of Diesel Oil
The image shows patterns that indicate the number of benzene rings and number of carbons.

Data Analysis Software, ChromSquare

A 2D map, chromatogram view, mass spectrum, and spot information can be displayed in the same window.
In addition to being able to directly import data from GCMSsolution,ChromSquare can also use GCMSsolution mass spectra search technology.

ChromSquare

ChromSquare is a product of Chromaleont srl in Italy

* GCxGC thermal modulator and GC Image are products of Zoex Corporation (United States).

What is GCxGC?

GC×GC chromatography employs a pair of GC columns (generally, nonpolar and polar columns) connected in series through a modulator*. Effluent from the first column is trapped in the modulator for a fixed period of time (modulation time) before being focused and injected into the second column . The chromatograms obtained through repeated trapping and injection is rendered in two dimensions using specialized software*. This result in a two-dimensional chromatogram with the boiling point and polarity on the respective axes.

* GC×GC Modulator and GC Image are products of Zoex Corporation, USA.

MDGC/GCMS-2010 Multi Dimensional Gas Chromatograph System

MDGC uses two columns with different separation characteristics for highly accurate separation of target components from a complex matrix.

Applications using GcxGC

Introduction to Applications

The GC×GC system is a powerful tool for the analysis of natural substances with complex matrices that are difficult to analyze by conventional GC or GCMS.
Some applications are introduced below.

Analysis of Mate Tea
Fatty Acids in Blood Plasma
Analysis of Coffee

Data on this page was provided by the group run by Professor Luigi Mondello, University of Messina, Italy.

An interview with Professor Mondello is featured in our section, A bridge with our customers.http://www.shimadzu.com/an/bridge/brigde7.html

Analysis of Mate Tea

Mate tea is widely consumed in the countries of South America as a tonic and stimulating beverage to overcome fatigue. We performed GC×GC analysis of the volatile components in a mate tea beverage (Ilex paraguariensis leaves and twigs) purchased in the Brazilian market.

GC×GC-qMS Chromatogram of Mate Tea

(First column: SLB-5ms (L=30 m, I.D.=0.25 mm, df=0.25 μm); Second column: Equity 1701(L=1.5 m, I.D.=0.1 mm, df=0.1 μm), modulation time 6 s)

The first column is a micropolar column and the second column is a mid-polarity column with dimensions suitable for fast analysis. An extremely large number of components were detected in the 2D chromatogram obtained. Hydrocarbon group components were detected in the lower part of the 2D diagram (low-polarity region). Caffeine was also detected as a prominent compound.

Comparison of GC×GC and Single GC Analyses

	Detected peaks	Identified peaks
GC×GC-MS	1000 or more	241
Single GC-MS	200	70

A library search using the mass spectrum identified 241 of the over 1000 peaks detected. It is apparent that GC×GC is an effective means of analyzing complex samples.

GC×GC-qMS Chromatogram of Mate Tea and Identification Results

No	Compound Name	No	Compound Name	No	Compound Name
20	4-hydroxy-2-butanone	30	5-methyl-3-methylene-5-hexen-2-one	40	alpha-pinene
21	methylpyrazine	31	2-heptanone	41	2-octanone
22	furfural	32	nonane	42	2-heptenal
23	isovaleric acid	33	4-heptenal	43	2,2-dimethyl-3-heptanone
24	(2E)-hexenal	34	2-butoxyethanol	44	5-ethyl-2(5H)-furanone
25	2-allylfuran	35	2,4-hexadienal	45	5-methyl furfural
26	(2Z)-hexenal	36	2(5H)-furanone	46	benzaldehyde
27	furfuryl alcohol	37	gamma-butyrolactone	47	hexanoic acid
28	hexanol 38 pyrazine	38	pyrazine, 2,5-dimethyl-	48	3-methyl-2(5H)-furanone
29	pentanoic acid	39	2,7-dimethyloxepine	49	1-octen-3-ol

This application data was provided by the group run by Professor Luigi Mondello, (University of Messina, Italy and Chromaleont S.r.l)

Fatty Acids in Blood Plasma

Fats in foods are attracting attention due to their deep relationship to a series of diseases including hypertension, heart disease, obesity, and hypercholesterolemia. They have been widely researched using chromatography in recent years. However, conventional methods suffer from several problems: 1) inability to identify the double-bond position in fatty acid isomers due to the similarity of the mass spectra, 2) poor GC resolution, and 3) inability to detect trace peaks due to poor sensitivity. In this example,a high-resolution, high-sensitivity GC×GC method was applied to the determination of fatty acid methyl esters in human blood plasma.

2D Chromatogram of Fatty Acid Methyl Esters in Blood Plasma

（First column：SLB-5ms（L=30m, i.d.=0.25mm, df=0.25μm), Second column：Supercowax-10（L=0.95m, i.d.=0.1mm, df=0.1μm),　modulation time：6sec)

Peak	FAME	Peak	FAME	Peak	FAME	Peak	FAME
1	C8:0	18	a-C19:0	35	C18:2ω6 (st)	52	C22:4ω6
2	C9:0	19	C19:0	36	C20:2	53	C22:4ω3
3	C10:0 (st)	20	C20:0 (st)	37	C20:2ω6 (st)	54	C24:4ω6
4	C11:0 (st)	21	C21:0 (st)	38	C22:2ω6 (st)	55	C20:5ω3 (st)
5	C12:0 (st)	22	C22:0 (st)	39	C24:2ω6	56	C20:5ω1
6	i-C14:0	23	C23:0 (st)	40	C18:3ω6 (st)	57	C21:5
7	C14:0 (st)	24	C24:0 (st)	41	C18:3ω3 (st)	58	C22:5ω6
8	i-C15:0 (st)	25	C14:1ω5 (st)	42	C18:3	59	C22:5ω3 (st)
9	a-C15:0 (st)	26	C16:1ω7 (st)	43	C19:3	60	C24:5ω3
10	C15:0 (st)	27	C17:1ω7 (st)	44	C19:3ω6	61	C24:5
11	i-C16:0 (st)	28	C18:1ω9 (st)	45	C20:3ω6 (st)	62	C20:6ω1
12	C16:0 (st)	29	C19:1	46	C20:3ω3 (st)	63	C22:6ω3 (st)
13	i-C17:0 (st)	30	C20:1ω9 (st)	47	C22:3ω6	64	C23:6
14	a-C17:0	31	C22:1ω9 (st)	48	C18:4ω3	65	C24:6ω3
15	C17:0 (st)	32	C24:1ω9 (st)	49	C20:4ω6 (st)
16	i-C18:0	33	C16:2ω6	50	C20:4ω3 (st)
17	C18:0 (st)	34	C17:2	51	C21:4

It is apparent that the FAME peaks corresponding to the carbon number (C), double bond number (DB), and double bond position (ω) are regularly distributed on the 2D chromatogram. This spatial distribution arrangement is extremely effective for the identification of compounds. Of the 65 peaks, 29 could be identified based on this arrangement. (The peaks labeled (st) in the diagram result from standard samples.) In addition, low levels of fatty acids with odd carbon numbers were also detected.

This application data was provided by the group run by Professor Luigi Mondello, (University of Messina, Italy and Chromaleont S.r.)

Analysis of Coffee

The aroma of roasted coffee is characterized by the presence of several thousand types of volatile compounds, mainly belonging to the pyran, pyrazine, and pyrrole group. The olfactory sensitivity, concentration, and chemical characteristics differ from type to type and the mutual interactions between them determine the characteristic aroma of the coffee. We used GCGC-MS to analyze the volatile components in coffee beans that are hard to analyze by conventional GC due to their extremely complex compositions.

2D Chromatogram of the Volatile Components in Arabica Coffee
（First column：Supercowax-10
（L=30m, i.d.=0.25mm, df=0.25μm), Second column：SPB-5ms（L=1.0m, i.d.=0.1mm, df=0.1μm),　modulation time：6sec)

A polar-nonpolar column pair was used for this analysis. Several thousand peaks on the two-dimensional plane,and we obtained a good plot of the extremely complex coffee aroma.

Pyrazine Groups Visualized on the 2D Chromatogram

It is apparent that 14 types from the pyrazine group form according to the side-chain carbon number and are aligned as horizontal bands.

This application data was provided by the group run by Professor Luigi Mondello, University of Messina, Italy

GCxGC Handbooks

GC×GC Handbooks have been prepared to introduce the fundamentals of GC×GC analysis and a summary of GC×GC applications. They are available in pdf format.

Author: Professor Luigi Mondello, University of Messina, Italy

Document No.	Title
C146-E178 (PDF, 2,358kB)	Application Compendium of Comprehensive 2D GC Vol.1-5 Introduces analysis applications that exploit the features of GC×GC,based on Professor Mondello's specialized field of foods and aromas. It provides a good understanding about the use of　GC×GC techniques, even for people working in other fields.
C146-E177 (PDF, 1,725kB)	Fundamental Principles of Comprehensive 2D GC Explains the principle of GC×GC analysis, GC×GC hardware, method　optimization, data processing, and advances in GC×GC analysis.

Download Brochure GCxGC Systems

Product Brochure:

Comprehensive GCxGC flyer C146-E139A.pdf