Académique Documents
Professionnel Documents
Culture Documents
and Disadvantages of
GC-MS to LC-MS
Gas Chromatography GC/liquid & gas
Injection
(vaporised)
Oven
Detector, Flame
FID ionisation
detector
Column
- capillary
Cylinder
- packed
(PC)
Integrator
Computer
C
y
l Carrier gas
Printer
i He, N2 plotter
n
d
e
Intensity
time
GC Chromatogram
GC-MS/liquid & gas
GC-MS / liquid & gas
Injection
(vaporised)
Oven
Detector, Flame
FID ionisation
detector
Column
Cylinder - capillary
- packed
Intensity
time
Chromatogram
Carrier gas Detector
He, N2 FID Flame Ionisation Detector
ECD Electron Capture Detector
He 4 GC, GCMS NPD Nitrogen phosphorus Detector
H2 2 GC, GCMS TCD Thermal Conductivity Detector
FPD Filter Photometric Detector
N2 28 GC, GCMS MS Mass Detector
AR/CH4 ECD
FID - general/universal detector
ECD - Ni63 radioisotop - halogenated compounds/Cl, Br
NPD - pesticide compounds
FPD - sulphurous/phosphorus compoundspesticides/ petrochemicals
FID qualitative & quantitative
A Full Range of Detectors
TRACE GC
What is a Mass Spectrometer?
Ionization Mass Sorting Detector
+
M
Analyser Ion Detection
EI
Source 20eV Electric field Photo- Electron
70eV or multiplier multiplier
Magnetic field
Data Analysis
> Solid
Inlet > Liquid
> Gas
Source Spectrum
Introduction
M+
Intensity
Relative
m/z
Ion Source
Filament
e- EI/CI
To Mass
CI
CH4 Analyzer EI
Removable
Ionization
Volume
Lenses
GC-MS/liquid & gas
1. Mass ionization
Filament sample size
e e M+ Too much sample
e e create secondary ionization
Sample [M-1]+
Trap
2. Quadrupole 3. Detector
photomultiplier
M 1+
+
M 3+ M + M 3+ M 2 M 1+
2
4. Vacuum
10 6 torr
oil + air molecules
oil
GC-MS/liquid & gas
Injection
(vaporised)
O ven
Flam e
D etector,
FID ionisation
detector
C olum n
- capillary
Intensity
Cylinder
- packed
tim e
Chrom atogram
C arrier gas M+ M+ M+
He, N 2
Classical techniques
Quantitative evaluation
1. Select column to provide best separation
2. Sample collection
3. Evaporation
4. Weight
Liquid Chromatography
Introduction
of sample
Normal phase
Reverse phase
Solvent
pump Injector Column
Response A C
Solvent
mobile phase time (t)
Chromatogram
Very elaborate method
HPLC/liquid
Sample Normal phase
Gradient elution
variable polarity Reverse phase
Solvent Injector
Column
pump "Valve"
Detector
A C
Response
B
Two solvent system
mobile phase
Degassing time (t)
A C A C
Response
B Response B
Response
B
time (t)
HPLC Chromatogram
Universal
Ref ractive Index RI UV - single wavelength
UV-Visible Diode Array - multiple wavelengths
Selective
Electrochemical (Amperometric)
Conductivity (Ion chromatography)
Fluorescence detector
Light Scattering detector
High Sensitivity
Mass Spectrometry
HPLC versus GC Instrumentation
H P LC M o b ile Pum p In je c to r
p h a se
S ta tio n a ry a n d Liq u id <400 <400µl
m o b ile p h a se
bar
1
m l/m in
D a ta D e te c to r C o lu m n
e v a lu a tio n DAD oven
lig h t < 1 0 0 oC
d e te c to r
Id e n tic a l
S ta tio n a ry Flo w
C a rrie r In je c to r
p h a se c o n tro lle r
gas
GC
G as <5 bar <5 µl
1
m l/m in
D a ta D e te c to r C o lu m n
e v a lu a tio n MS oven
fla m e < 4 0 0 oC
d e te c to r
Ionisation
Forming Charged Particles (Ions):
* Electron impact (EI)
* Chemical Ionization (CI)
* Fast atom bombardment (FAB)
* Field desorption (FD)
* Electrospray ionization (ESI)
* Laser desorption (LD)
MS in LC/GC-MS
Detect and quantify the various species
eluting off the column according to their
m/z value with the help of electrical or
magnetic fields, or combination of both.
A difficult decision
Sample Recovery
GCMS LCMS
Petroleum
Gasoline
Hydrocarbon gas analysis
Fuel and fuel oil analysis
Oxygenated additives in gasoline
Environmental
Determination of pesticides
Detection of PCBs (polychlorinated biphenyls) Air
pollution consituent analysis
Fast Analysis of Dioxin and related compounds
GCMS Application
Forensics
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# " " $
LCMS Application
Study of Proteomics
identification, isolation and purification of
proteins in a cell or body fluid
involves protease digestion (usually Trypsin)
followed by LC-MS with peptide mass
fingerprinting or LC-MS/MS (tandem MS) to
derive sequence of individual peptides.
LCMS Application
The advantages:
The disadvantages: