694
GCCHROMATOGRAMS |
PHARMACEUTICAL
Organic Volatile Impurities/Residual Solvents
Class1ResidualSolvents forWater-SolubleArticlesonRxi®-624SilMS
GC_PH1144
Conc.
Peaks
RT (min.)
(µg/mL)
1. 1,1-Dichloroethene
3.586
0.07
2. 1,1,1-Trichloroethane
8.536
0.08
3. Carbon tetrachloride
9.042
0.03
4. Benzene
9.787
0.02
5. 1,2-Dichloroethane
10.112
0.04
*DMSO Interference
Column
Rxi
®
-624Sil MS, 30m, 0.32mm ID, 1.80µm (cat.# 13870)
Sample
Residual Solvents - Class 1 (cat.# 36279)
Diluent:
water
Injection
headspace-loop split (split ratio 5:1)
Liner:
1mm Split (cat.# 20972)
Headspace-Loop
Inj. PortTemp.:
140 °C
Instrument:
Tekmar HT3
Inj.Time:
1min.
Transfer LineTemp.: 110 °C
ValveOvenTemp.: 110 °C
SampleTemp.:
80 °C
Sample Equil.Time: 60min.
Vial Pressure:
10 psi
PressurizeTime:
0.5min.
Pressure
EquilibrationTime: 0.05min.
Loop Pressure:
5 psi
Loop FillTime:
0.1min.
Oven
OvenTemp:
40 °C (hold 20min.) to 240 °C at 10 °C/min. (hold 20min.)
Carrier Gas
He, constant flow
Linear Velocity:
35 cm/sec.
DeadTime:
1.45min.@ 40 °C
Detector
FID@ 250 °C
Data Rate:
5Hz
Instrument
Agilent/HP6890GC
Acknowledgement TeledyneTekmar
GC_PH1146
Class2 -MixAResidualSolvents forWater-SolubleArticlesonRxi®-624SilMS
Conc.
Peaks
RT (min.) (µg/mL)
1. Methanol
2.281
25.00
2. Acetonitrile
4.009
3.42
3. Dichloromethane
4.313
5.00
4.
trans
-1,2-Dichloroethene 4.798
7.83
5.
cis
-1,2-Dichloroethene
7.028
7.83
6. Tetrahydrofuran
7.706
5.75
7. Cyclohexane
8.708
32.33
8. Methylcyclohexane
14.099
9.83
9. 1,4-Dioxane
15.054
3.17
10. Toluene
22.018
7.42
11. Chlorobenzene
26.570
3.00
12. Ethylbenzene
26.837
3.07
13.
m
-Xylene
27.147 10.85
14.
p
-Xylene
27.147
2.53
15.
o
-Xylene
27.927
1.63
Column
Rxi
®
-624Sil MS, 30m, 0.32mm ID, 1.80µm (cat.# 13870)
Sample
Residual Solvents Class 2 - Mix A (cat.# 36271)
Diluent:
water
Injection
headspace-loop split (split ratio 5:1)
Liner:
1mm Split (cat.# 20972)
Headspace-Loop
Inj. PortTemp.:
140 °C
Instrument:
Tekmar HT3
Inj.Time:
1min.
Transfer LineTemp.: 110 °C
ValveOvenTemp.: 110 °C
SampleTemp.:
80 °C
Sample Equil.Time: 60min.
Vial Pressure:
10 psi
PressurizeTime:
0.5min.
Pressure
EquilibrationTime: 0.05min.
Loop Pressure:
5 psi
Loop FillTime:
0.1min.
Oven
OvenTemp:
40 °C (hold 20min.) to 240 °C at 10 °C/min. (hold 20min.)
Carrier Gas
He, constant flow
Linear Velocity:
35 cm/sec.
DeadTime:
1.45min.@ 40 °C
Detector
FID@ 250 °C
Data Rate:
5Hz
Instrument
Agilent/HP6890GC
Acknowledgement TeledyneTekmar
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E-mail :
TelNo : 03 9762 2034 . . . inAUSTRALIA
Mar 2011
