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

GC_PH1165

	Peaks	t_R (min)	Ions Monitored (m/z)
1.	Methyl methanesulfonate (MMS)	5.043	79, 80, 95
2.	Isopropyl methanesulfonate (iPMS)	6.010	59, 79, 123
3.	Diethyl sulfate (DES)	6.357	111, 125, 139
4.	di-isopropyl sulfate (DPS)	6.970	45, 87, 167
5.	dibutyl sulfate (DBS)	9.260	29, 41, 56
6.	Methyl benzenesulfonate (MBS)	9.463	77, 141, 172

	Peaks	t_R (min)	Ions Monitored (m/z)
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 isomer of ETS

Standard/Sample
Column	Rxi-624Sil MS, 20 m, 0.18 mm ID, 1.00 µm (cat.# 13865)
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.:	280 °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

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