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
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
image
GC_PH1165
ColumnRxi-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 GasHe, constant flow
Linear Velocity:45 cm/sec
DetectorMS
Mode:SIM
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
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PGI

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GTI

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mesylate

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besylate

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tosylate

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