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Mesylate, Besylate, and Tosylate Genotoxic Impurities on Rxi-624Sil MS (extracted ion chromatograms)

PeakstR (min)Ions Monitored (m/z)
1.Methyl methanesulfonate (MMS)5.04379, 80, 95
2.Isopropyl methanesulfonate (iPMS)6.01059, 79, 123
3.Diethyl sulfate (DES)6.357111, 125, 139
4.di-isopropyl sulfate (DPS)6.97045, 87, 167
5.dibutyl sulfate (DBS)9.26029, 41, 56
6.Methyl benzenesulfonate (MBS)9.46377, 141, 172
PeakstR (min)Ions Monitored (m/z)
7.Ethyl benzenesulfonate (EBS)9.88377, 141, 186
8.Methyl toluenesulfonate (MTS)10.33791, 155, 186
9.Ethyl toluenesulfonate (ETS)10.71391, 155, 200
10.n-propyl toluenesulfonate (nPTS)10.82791, 155, 172
11.n-butyl benzenesulfonate (nBBS)11.0777, 141, 159
12.isopropyl p-toluenesulfonate (iPTS)11.24091, 155, 172
13.p-toluenesulfonic acid n-butyl ester (nBTS)11.82391, 155, 173
* ortho isomer of ETS
ColumnRxi-624Sil MS, 20 m, 0.18 mm ID, 1.00 µm (cat.# 13865)
Diluent:90:10 acetonitrile:water
Conc.:500 ng/mL
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 Temp.:80 °C (hold 2 min) to 300 °C at 20 °C/min (hold 5 min)
Carrier GasHe, constant flow
Linear Velocity:45 cm/sec
Transfer Line Temp.:280 °C
Analyzer Type:Quadrupole
Source Temp.:280 °C
Solvent Delay Time:4 min
Ionization Mode:EI
InstrumentShimadzu 2010 GC & QP2010+ MS
AcknowledgementIn collaboration with Merck and Company