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As easy as GC×GC
Aaron Parker
European Sales Manager
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Separation
Who are SepSolve Analytical?
Experts in analytical chemistry
Sample preparation Identification Data analysis
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▪ We solve problems in separation
science….
▪ …by delivering innovative GC-MS
and GC×GC-MS solutions, including
both hardware and software
▪ A single-vendor solution
Who are SepSolve Analytical?
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Sample introduction
• Sample preparation robots
• Multi-mode inlets
• Full range of Markes’ TD
Data analysis
• TOF-DS for 1D GC-TOF
• ChromSpace for GC×GC
Separation
• Heartcutting (GC-GC)
• GC×GC
What can we offer?
Detection
• TOF mass spectrometry
• FID, SCD, ECD…
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Why use GC×GC?
Retention time (min)
Inte
nsity
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What is GC×GC? 2
nd
rete
nti
on
tim
e (
s)
1st retention time (min)
0
100
Inte
nsity
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• Increased separation capacity
• Enhanced sensitivity
• Structured chromatograms
Why use GC×GC?
Time
Inte
nsi
ty 1D GC
GC×GC
TIC
EIC m/z 106
EIC m/z 134
EIC m/z 148
EIC m/z 162
EIC m/z 176
EIC m/z 120
C1 alkyl benzenes
C2 alkyl benzenes
C3 alkyl benzenes
C4 alkyl benzenes
C5 alkyl benzenes
C6 alkyl benzenes
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1. The sample is subjected to two independent separations.
2. The separation from the first dimension is preserved
throughout the process.
J. C. Giddings Anal. Chem. 1984, 56, 1258A-1270A.
Rules of 2D chromatography
Orthogonality rule
Conservation rule
Speed rule
3. The second dimension separation must be significantly
faster than the first dimension.
Comprehensive ˄
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What is GC×GC?
▪ The modulator is the ‘beating heart’ of a GC×GC system
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The modulator
The “beating heart” of GC×GC
Two-stage
modulator
Secondary column
Carrier gas flow
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The modulator
The “beating heart” of GC×GC
Primary column
Two-stage
modulator
Secondary column
Carrier gas flow
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Primary column
Two-stage
modulator
The modulator
The “beating heart” of GC×GC
Secondary column
Carrier gas flow
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The role of GC×GC software
3 s
2tR
1tR
2tR
1tR
Stacked modulation slices
3D Surface chart
Colour plot
▪ GC×GC software must merge the sub-peaks for easy
visualisation of the data
Sig
na
l
Time
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Non
-pola
r
Polar
“Reverse”
(or inverse)
phase separation
Choice of column set
Non-polar
Pola
r
“Normal”
(or conventional)
phase separation
Structured ordering (or “roof-tiling” effect)
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GC×GC modulation
20+ years of innovation
1984
1991
Phillips & Ledford
introduce rotating
thermal modulator
(or ‘sweeper’)
1996
Marriott develops
the longitudinally
modulated
cryogenic system
(LMCS)
1997
2000
Beens et al.
develop liquid CO2
single-stage
modulator
Giddings publishes
theory of
multidimensional
separations
Implementation of
first GC×GC
separation (using a
thermal desorption
modulator) by
Phillips & Liu
Miniaturisation of
thermal modulation
by Kim et al. for 2D
micro-GC
2010
2012Griffith et al.
publish on ‘reverse
fill/flush’ flow
modulation
O=C=O
2003
Seeley develops
first differential
flow modulator
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▪ Commercial devices use:
– Flow modulatione.g. INSIGHT modulator (SepSolve Analytical)
– Thermal modulation e.g. Delay loop modulator (Zoex)
▪ Both have their own pros and cons – the choice will depend on the application
Types of modulator
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Modulator pros and cons
Flow Thermal
Compound rangeNo volatility restrictions
(modulate from C1)
Cannot modulate ≤C4
(liquid cryogen needed for <C8 )
Cost of ownership € €€€
Repeatability Peak area RSD routinely < 5% Variable, peak area RSD 5-10%
Flexibility Easily configured for heart-cutting, back-
flushing and parallel detection Limited
Sensitivity Can be restricted if splitting the flow to
multiple detectorsSuitable for ultra-trace analyses
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How do I choose a modulator?
Depends on a range of factors:
BudgetRequired detection
limits
Sample throughput
Sample complexity
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▪ Consumable-free operation– Low running costs
▪ Efficient modulation of volatiles– Extends application range
▪ Excellent repeatability– For routine analyses and large sample batches
Benefits of flow modulation
INSIGHT®
(SepSolve Analytical)
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INSIGHT® modulator
How does it work?
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High peak capacity…
…and no tailing
Peak widths
<100 ms at base
100 ms
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▪ Flow-modulated GC×GC using INSIGHT for analysis of a gas standard
▪ Excellent peak shape and peak widths (at base) of ~100-200 ms
Efficient modulation of volatiles
PM = 1 s
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Efficient modulation of volatiles
1. Freon 12
2. Freon 114
3. Isobutane
4. Chloromethane
5. n-Butane
2
1
35
4
▪ Flow modulation by
INSIGHT has no volatility
restrictions
▪ Excellent peak shape for the
5 most volatile compounds
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Heart-cutting capability
Configure two detectors:
• Majority undergoes 1D separation and
sent to detector “A”
• Heart-cut portion sent to second
column and detector “B”
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Retrofit to existing GC(-MS)
Mega-mix of environmental
contaminants
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▪ SepSolve deliver flexible systems
– Time-of-flight MS (more about this shortly!)
– FID
– And many other single-channel detectors
e.g. ECD, SCD….
▪ Compatible with various detectors
▪ Parallel detection allows complementary
datasets to be obtained simultaneously
Choice of detector?
An overview of MS detectors used in published GCxGC studies
(P. Tranchida et al, TrAC Trends in Analytical Chemistry, 2018, 105, 360-366)
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▪ Designed for chromatographers
▪ Compatible with third-party
datafile formats
▪ Network licensing options now
available
▪ Processing of 1D GC and
GC×GC data
ChromSpace®
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▪ Reverse fill/flush dynamics for: – Improved peak shape and peak capacity
▪ Efficient modulation of both volatiles and semi-volatiles (CH4 to n-C60)
▪ Excellent repeatability for large sample batches – Rigid retention times
– Area %RSD routinely <5%
▪ Simple configuration of: – Parallel detection (e.g. FID/TOF MS)
– Heart-cutting
– Back flushing
– Dual-channel configuration
Summary
INSIGHT® provides:
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▪ Cannabis terpenes
▪ Total petroleum hydrocarbons (TPH)
Case studies
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▪ Over 200 terpenes have been identified in cannabis
▪ Separation and quantitation of these diverse compounds
can be challenging
▪ Conventional GC–FID or GC–MS results in co-elution of
similar compounds or oxygenated derivatives
– Abundance of important terpenes is over-estimated
– Poor confidence in data quality
Challenges
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▪ Analysis of a standard containing 32 cannabis terpenes plus a surrogate and internal standard
Cannabis terpenes…
…by GC×GC-FID
12 3
4
5
Surr. ISTD
6
7 8 9
10
11
12
13
14
14
15 18
17
16
20
19
21
22
23
24 27
25
26
2829
30 31
32
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Enhanced separation of GC×GC
▪ Dihydrocarveol and α-terpineol would have
perfectly co-eluted in a 1D GC separation
– Causing one terpene to be overestimated and
the other overlooked.
▪ Enhanced separation of GC×GC provides
increased confidence in terpene profiling
▪ Without the need for expensive mass
spectrometers or complicated deconvolution
algorithms
α-Terpineol
Dihydrocarveol
A single peak on the 1D GC trace
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Streamlined software workflows
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Just for fun…
▪ Peak markers in ChromSpace can be set as any image
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Full quantitative workflows
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▪ Calibration curves
prepared using standards
of 5–500 ppm in
dichloromethane
▪ All 32 terpenes displayed
excellent linearity with
R2 > 0.997
Linearity of GC×GC-FID
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Simple reporting of results
▪ Fast area percent results
through the application of
stencils
▪ Filtered group-type reports
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Comparison of cannabis oils
Pineapple Express
Candy Kush
CBD Yummy
Strawberry Banana
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Comparison of cannabis oils
▪ ‘Strawberry Banana’ has increased levels of α-pinene, trans-caryophyllene and α-humulene,
and was the only sample to contain citronelllol
▪ ‘CBD Yummy’ was the only sample to contain α-terpinene
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Improved confidence in aroma profiles
‘Pineapple Express’ ‘Strawberry Banana’ ‘CBD Yummy’‘Candy Kush’
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▪ Cannabis terpenes
▪ Total petroleum hydrocarbons (TPH)
Case studies
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▪ Commonly split into the Volatile Petroleum Hydrocarbons
(VPH) and the Extractable Petroleum Hydrocarbons (EPH)
▪ EPH monitors hydrocarbons from an equivalent carbon
number of C10-C40 (sometimes C44)
▪ For environmental fate and risk-based analysis the aliphatic
and aromatic hydrocarbons must be separated
▪ Compounds are reported as groups (>C10-C12, >C12-C16…etc)
rather than individually
Total Petroleum Hydrocarbons (TPH)
Background
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Total Petroleum Hydrocarbons
The Traditional Method
Solvent
Extract
Aliphatic
portion
(Hexane)
Aromatic
portion
(DCM)
1st GC
analysis
2nd GC
analysis
SampleSPE
fractionation
Post-analysis
processing
Post-analysis
processing
Reporting
Reporting
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Total Petroleum Hydrocarbons
What can we change?
Solvent
Extract
SPE
fractionation
Aliphatic
portion
(Hexane)
Aromatic
portion
(DCM)
1st GC
analysis
2nd GC
analysis
Post-analysis
processing
Sample
Post-analysis
processing
Reporting
Reporting
! Expensive consumables and waste disposal
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Total Petroleum Hydrocarbons
What can we change?
Solvent
Extract
SPE
fractionation
Aliphatic
portion
(Hexane)
Aromatic
portion
(DCM)
1st GC
analysis
2nd GC
analysis
Post-analysis
processing
Sample
Reporting
ReportingPost-analysis
processing
! Labour-intensive process
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Total Petroleum Hydrocarbons
What can we change?
Solvent
Extract
SPE
fractionation
Aliphatic
portion
(Hexane)
Aromatic
portion
(DCM)
1st GC
analysis
2nd GC
analysis
Post-analysis
processing
Sample
Reporting
ReportingPost-analysis
processing
! Health and safety concerns
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▪ Chromatographic separation of aliphatic and aromatic hydrocarbons in a single
run, reducing processing time
A new approach to TPH…
…using GC×GC-FID
Single
transferTraditional
solvent extract
Sample
ReportingSingle analysis AND
automated real-time
data processing
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Consumables savings
Fast return on investment
€280 €1410
€1120
€13,440
€5640
€67,680
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▪ Regions of interest (Aliphatic >C10-C12….etc) are identified using a banding standard
▪ Internal standard and surrogate regions can also be added
Simple data processing…
…using stencils
Aliphatics
Aromatics
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▪ Stencils are then applied to real samples in real-time data processing
Simple data processing…
…using stencils
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Repeatability
▪ 15 injections of the TPH marker standard over a 5 day period
▪ All RSD <5%
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▪ Run two samples simultaneously, with real-time data processing in ChromSpace
▪ Compatible with Agilent and Thermo GCs
Enhanced productivity…
…through dual-channel GC×GC Sample 1
Sample 2
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Real-time data processing
for both channels
ChromSpace for dual-channel GC×GC
Template methods
already configured
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Take home messages
▪ GC×GC provides enhanced separation for complex
environmental samples, eliminating the need for
sample fractionation
▪ INSIGHT offers consumable-free, robust GC×GC for
the widest range of analytes (VOCs to SVOCs)
▪ GC×GC is moving from “niche” to “routine” thanks to
improvements in hardware and software
▪ Coupling with TOF MS adds an extra level of
information on sample composition
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Contact SepSolve
Email: [email protected]
Tel.: +44 (0)1733 669222
Web: www.sepsolve.com
Twitter: @SepSolve
LinkedIn: www.linkedin.com/company/sepsolve-analytical