690
GCCHROMATOGRAMS |
PHARMACEUTICAL
Potential Genotoxic Impurities (PGIs)
AlkylHalideGenotoxic Impurities
Rxi®-624SilMS (HighConcentration Injection)
Peaks
RT (min.)
Conc.
(µg/mL)
1. 2-Chloropropane
2.10
1
2. Bromoethane
2.36
1
3. 1-Chloropropane
2.72
1
4. 2-Bromopropane
3.393
1
5. Butyl chloride
4.627
1
6. 1-Bromobutane
5.973
1
Column
Rxi
®
-624Sil MS, 20m, 0.18mm ID, 1.00µm (cat.# 13865)
Sample
Diluent:
DMSO
Conc.:
1µg/mL
Injection
Inj. Vol.:
1µL splitless (hold 0.5min.)
Liner:
3.5mm SingleGooseneck Liner withwool placed 3cm
from top (middle) (cat.# 22286)
Inj.Temp.:
220 °C
Purge Flow:
3mL/min.
Oven
OvenTemp:
40 °C (hold 3min.) to 200 °C at 20 °C/min.
Carrier Gas
He, constant flow
Linear Velocity:
40 cm/sec.
Detector
MS
Mode:
Scan
Transfer LineTemp.: 200 °C
AnalyzerType:
Quadrupole
SourceTemp.:
280 °C
Solvent DelayTime: 0.5min.
IonizationMode:
EI
Scan Range:
30-300 amu
Scan Rate:
5 scans/sec.
Instrument
Shimadzu 2010GC&QP2010+MS
Notes:
Ionsmonitored 42, 43, 57, 108m/z
Good retention forhard-to-retain
polaranalytesmakesmethod
developmenteasier!
GC_PH1166
NEW!
1. 1-chloropropane
2. bromoethane
3. 2-chloropropane
4. 1-bromopropane
5. 2-bromopropane
6. 1-bromobutane
7. dimethyl sulfate
8. methyl methanesulfonate
9. ethyl methanesulfonate
10. isopropyl methanesulfonate
11. diethyl sulfate
12. di-isopropyl sulfate
13. di-
n
-propyl sulfate
14. dibutyl sulfate
15. methylbenzene sulfonate
16. ethylbenzene sulfonate
17. methyl toluenesulfonate
18. ethyl toluenesulfonate
19.
n
-butyl benzenesulfonate
20.
n
-propyl toluenesulfonate
21. isopropyl toluenesulfonate
22.
n
-butyl toluenesulfonate
*ortho isomer of ethyl toluenesulfonate
Column:
Rtx
®
-200, 30m, 0.25mm ID, 1.0µm (cat.# 15053)
Sample:
100µg/mL each compound in 90:10 acetonitrile:water
Inj.:
1µL, split (10:1), 4mm single gooseneck inlet liner w/wool (cat.# 22405)
Inj. temp.:
220°C
Carrier gas:
helium, constant flow
Flow rate:
1.0mL/min.
Oven temp.:
40°C (hold 8.3min.) to 70°C@ 70°C/min. to 115°C@ 40°C/min. to
250°C@ 30°C/min. to 300°C@ 15°C/min. (hold 3min.)
Det:
MS
Transfer line temp.: 280°C
Scan range:
20-250m/z
Ionization:
EI
Mode:
scan
GC_PH01076
PotentialGenotoxic Impurities (PGIs)
Rtx®-200
Website :
E-mail :
TelNo : 03 9762 2034 . . . inAUSTRALIA
Mar 2011
