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SVEOBUHVATNA DVODIMENZIONALNA GASNA
HROMATOGRAFIJA SA MASENIM
SPEKTROMETROM
(GCXGC-MS)
Marija Lješević,
Istraživač pripravnik, Institut za hemiju, tehnologiju i metalurgiju Univerziteta u Beogradu
U Beogradu, 23.11.2018.
GASNA HROMATOGRAFIJA
Tehnika za razdvajanje isparljivih jedinjenja
https://teaching.shu.ac.uk/hwb/chemistry/tutorials/chrom/gaschrm.htm
GC-MS
Ima veći kapacitet pikova u odnosu na ostale
hromatografske tehnike
Razdvaja 100-150 jedinjenja
U zavisnosti od načina jonizacije i vrste MS
detektora osetljivost od 1 pg-100 pg
GC-GC I GCXGC
Multidimenzional
na gasna
hromatografija
Heart-cut process
Sveobuhvatna
gasna
hromatografija
https://www.omicsonline.org/editor-pdf/Hadir_M_Maher_Shalaby.pdf
• Kapacitet pikova- maksimalni teorijski broj
kompnenti koje mogu da se razdvoje na nekoj koloni pri
određenim uslovima
• GCxGC: kapacitet pikova prve kolone x kapacitet pikova druge
kolone
Phillips i saradnici- analiza naftnih derivata
• Najvažniji deo GCxGC sistema
• Modulatori sa ventilima, termalni i kriogeni
•Imaju tri glavne funkcije: akumuliranje, refokusiranje i oslobadjanje
uzorka
MODULATOR
•Vreme modulacije-
Trajanje kompletnog ciklusa
modulacije, jednako je vremenu
koje prođe između dva
injektovanja u drugu kolonu.
•3-4 modulacije za 1 pik na
prvoj koloni (modulacija ne
bi trebalo da bude veća od
cetvrtine širine pika)
•Pikovi su veoma uski (50-
600 ms
Marriott, Shellie, Trends in Analycal
chemistry, 2002, 21, p 573.
GC
GC oven temperature Temp range: amb. + 4˚C to 450˚C (in 1 °C steps)
Heat-up rate (1) Max. 100 °C/min, in 0.01 °C steps (230 V specifications)
GC cooling rate Cooling from 450 °C to 50 °C in 3.5 minutes or less
Temperature control 8 or more temperature control zones
Column flow rate Can accommodate column flow rates up to 15 mL/min.
Gas control The carrier gas can be controlled in constant linear velocity mode.
Pressure 0.000 to 970kPa
Columns x 2 RTX-1, 30 x 0.25 x 0.25 and BPX-50 1 m, 0.15 mm, 0.15 μm
AutoinjectorAuto injector with 15 sample position. Sample volume
1.5ml/2ml. Variable injection
Mass Spectrometer
Mass range Satisfies m/z range of 1.5 to 1,090 Separator
Quadrupole with a pre-filter (equipped
with a low-noise electron multiplier with
overdrive lens)
Resolution (1) R ³ 2M (FWHM) minimumQuadrupole rod contamination
countermeasures
The analysis system is equipped with a
quadrupole mass filter with a pre-rod.
Resolution (2) 2,000 minimum (FWHM at m/z 614) Ionization voltage Configurable from 10 eV to 200 eV
Dynamic
range of the
electrical
system
The dynamic range is at least 1.6 x 10^7. Ion source temperatureIndependently heated up to 350 °C or
higher.
Sensitivity (EI
scan)1pg octafluoronaphtalene m/z 272, S/N > 1500 Scan speed
Maximum scan speed of at least 20,000
u/sec
Sensitivity (CI
scan)
100 fg octafluoronaphtalene m/z 272, S/N >
500 (For methane)Filament (1) A dual filament is used
Sensitivity
(NCI scan)
100 fg octafluoronaphtalene m/z 272, S/N >
500 (For methane)Modulator
Two stage loop modulator; cycle range
from 1000ms – 32000ms
Nitrogen generatorAt least 99.999% purity of given gases, flow rate 250,600 cc/min, deliver pressure 0-
80psi, inlet air requirements Minimum 35 l/min at 120-145psi
BIOCHEMICAL PROFILING OF MICROORGANISMS USING COMPREHENSIVE GCxGC-MS
Djurić et al., Int J Biol Macromol 2017;104:311-21.Izrael-Živković et al., Journal of Molecular Catalysis. B, Enzymatic 2017; in press
The fatty acid methyl ester profile of
Brachybacterium sp. CH-KOV3 a) GC–MS;
b) 2D GCxGC–MS.
23
Lama et al., ACS Sustainable Chemistry & Engineering 2017;5:2415-20
Analiza degradacije kraft lignina