689
GCCHROMATOGRAMS |
PHARMACEUTICAL
Potential Genotoxic Impurities (PGIs)
Mesylate,Besylate, andTosylateGenotoxic Impurities
Rxi®-624SilMS (extracted ionchromatograms)
GC_PH1165
Peaks
RT (min.) IonsMonitored
(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, 20m, 0.18mm ID, 1.00µm (cat.# 13865)
Sample
Diluent:
90:10 acetonitrile:water
Conc.:
500 ng/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:
80 °C (hold 2min.) to 300 °C at 20 °C/min. (hold 5min.)
Carrier Gas
He, constant flow
Linear Velocity:
45 cm/sec.
Detector
MS
Mode:
SIM
Transfer Line
Temp.:
200 °C
AnalyzerType:
Quadrupole
SourceTemp.:
280 °C
Solvent Delay
Time:
4min.
Ionization
Mode:
EI
Instrument
Shimadzu 2010GC&QP2010+MS
Acknowledgement In collaborationwithMerck and Company
Extracted ions for
MMSand iPMS show
compatibilitywith
polar injection solvents
usinga splitless
injection technique for
higher sensitivity.
Lowbleedat 300°Callows for“bake-out”
ovenprograms.
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Mar 2011
