690
GC CHROMATOGRAMS |
PHARMACEUTICAL
Potent ial Genotoxic Impur i t ies (PGIs)
Alkyl Halide Genotoxic Impurities
Rxi®-624Sil MS (High Concentration 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, 20 m, 0.18 mm ID, 1.00 µm (cat.# 13865)
Sample
Diluent:
DMSO
Conc.:
1 µg/mL
Injection
Inj. Vol.:
1 µL splitless (hold 0.5 min.)
Liner:
3.5mm Single Gooseneck Liner with wool placed 3cm
from top (middle) (cat.# 22286)
Inj. Temp.:
220 °C
Purge Flow:
3 mL/min.
Oven
Oven Temp:
40 °C (hold 3 min.) to 200 °C at 20 °C/min.
Carrier Gas
He, constant flow
Linear Velocity:
40 cm/sec.
Detector
MS
Mode:
Scan
Transfer Line Temp.: 200 °C
Analyzer Type:
Quadrupole
Source Temp.:
280 °C
Solvent Delay Time: 0.5 min.
Ionization Mode:
EI
Scan Range:
30-300 amu
Scan Rate:
5 scans/sec.
Instrument
Shimadzu 2010 GC & QP2010+ MS
Notes:
Ions monitored 42, 43, 57, 108 m/z
Good retention for hard-to-retain
polar analytes makes method
development easier!
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 8.3 min.) 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 3 min.)
Det:
MS
Transfer line temp.: 280°C
Scan range:
20-250m/z
Ionization:
EI
Mode:
scan
GC_PH01076
Potential Genotoxic Impurities (PGIs)
Rtx®-200
Website :
E-mail :
TelNo : 03 9762 2034 . . . in AUSTRALIA
Mar 2011
