instrument |
Shimadzu GC2010 (Kyoto, Japan) |
Thermo Trace GC Ultra
(Thermo Fisher, Bremen, Germany) |
injector |
Split/splitless (SSL) injector |
Programmable
temperature vaporizer (PTV) |
column parameters |
TG5MS (Thermo Fisher Scientific;
Waltham, MA, USA) |
length: 30 m length |
internal diameter: 0.25 mm |
stationary phase thickness: 0.25
μm |
liner |
deactivated packed wool glass SSL inlet liner (Shimadzu, Sydney,
Australia) |
straight deactivated PTV metal liner (Thermo
Fisher Scientific;
Waltham, MA, USA) |
injection
parameters |
injection
volume: 1 μL |
temperature: 300 °C |
split ratio: 1:25 |
carrier gas: helium |
flow programming |
mode: flow control |
carrier gas flow rate: 2 mL/min |
oven temperature programming |
60 °C (2 min), 10 °C/min
to 300 °C (9 min) |
total run time: 34 min |
detectors |
TQ8040 MS (triple quadrupole) |
flame ionization detector (FID), TSQ Quantum XLS MS (triple
quadrupole) |
FID parameters |
|
temperature: 300 °C |
airflow: 350 mL/min |
H2-flow: 35 mL/min |
makeup (N2) flow: 30 mL/min |
MSD
parameters |
transfer
line temperature: 250
°C |
electron
ionization (EI) source
temperature: 200 °C |
electron energy: 70 eV |
emission current: 60 μA |
filament power switch time:
0
min off, 6 min on |
monitoring ions: |
1. Full scan (m/z 40 to 500); scan
time: 0.3 s |
2. Multiple reaction monitoring
(MRM, parameters see Figure 1); |
collision
gas: Argon |
data acquisition and evaluation
software |
GCMSsolution version 4.52 (Shimadzu) |
Thermo Xcalibur 4.4.16.14 (Thermo Fisher) |