689
GC CHROMATOGRAMS |
PHARMACEUTICAL
Potent ial Genotoxic Impur i t ies (PGIs)
Mesylate, Besylate, and Tosylate Genotoxic Impurities
Rxi®-624Sil MS (extracted ion chromatograms)
GC_PH1165
Peaks
RT (min.) Ions Monitored
(m/z)
1. Methyl methanesulfonate (MMS)
4.253
79, 80, 95
2. Isopropyl methanesulfonate (iPMS)
5.043
59, 79, 123
3. Diethyl sulfate (DES)
6.010 111, 125, 139
4. di-isopropyl sulfate (DPS)
6.357
45, 87, 167
5. dibutyl sulfate (DBS)
9.260
29, 41, 56
6. Methyl benzenesulfonate (MBS)
9.463 77, 141, 172
7. Ethyl benzenesulfonate (EBS)
9.883 77, 141, 186
8. Methyl toluenesulfonate (MTS)
10.337 91, 155, 186
9. Ethyl toluenesulfonate (ETS)
10.713 91, 155, 200
10.
n
-propyl toluenesulfonate (nPTS)
10.827 91, 155, 172
11.
n
-butyl benzenesulfonate (nBBS)
11.07 77, 141, 159
12. isopropyl
p
-toluenesulfonate (iPTS)
11.240 91, 155, 172
13.
p
-toluenesulfonic acid
n
-butyl ester (nBTS)
11.823 91, 155, 173
* Ortho isomers of ETS.
Column
Rxi
®
-624Sil MS, 20 m, 0.18 mm ID, 1.00 µm (cat.# 13865)
Sample
Diluent:
90:10 acetonitrile:water
Conc.:
500 ng/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:
80 °C (hold 2 min.) to 300 °C at 20 °C/min. (hold 5 min.)
Carrier Gas
He, constant flow
Linear Velocity:
45 cm/sec.
Detector
MS
Mode:
SIM
Transfer Line
Temp.:
200 °C
Analyzer Type:
Quadrupole
Source Temp.:
280 °C
Solvent Delay
Time:
4 min.
Ionization
Mode:
EI
Instrument
Shimadzu 2010 GC & QP2010+ MS
Acknowledgement In collaboration with Merck and Company
Extracted ions for
MMS and iPMS show
compatibility with
polar injection solvents
using a splitless
injection technique for
higher sensitivity.
Low bleed at 300°C allows for “bake-out”
oven programs.
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Mar 2011
