696
GCCHROMATOGRAMS |
PHARMACEUTICAL
Organic Volatile Impurities: Retention Time Index
G16
G16
G43
G27
G1
NA
Carrier gas: helium
ICH
Stabilwax
®
Rtx
®
-WAX
Rtx
®
-1301
Rxi
®
-5ms
Rtx
®
-1
Rtx
®
-200
Compound
Class
Retention Time
Retention Time
Retention Time
Retention Time
Retention Time Retention Time
1,1,1-trichloroethane
1
3.96
3.49
5.43
5.40
10.82
8.35
1,1,2-trichloroethene
2
15.72
14.28
10.99
9.77
16.75
14.94
1,1-dichloroethene
1
2.23
2.04
2.79
4.41
5.73
4.16
1,2-dichloroethane
1
8.80
7.68
6.15
5.46
10.38
9.74
cis
-1,2-dichloroethene
2
6.50
5.65
4.79
2.88
8.71
7.11
trans
-1,2-dichloroethene
2
3.63
3.20
3.55
3.54
7.17
5.16
1,2-dimethoxyethane
2
4.80
4.18
6.03
5.54
10.98
10.63
1,4-dioxane
2
8.55
7.49
7.86
7.26
13.54
14.34
1-butanol
3
11.13
10.08
7.18
5.76
11.49
10.13
1-pentanol
3
14.95
13.75
11.19
9.44
16.99
14.95
1-propanol
3
7.69
6.80
4.20
3.37
6.81
6.13
2-butanol
3
7.25
6.44
5.08
4.16
8.51
7.69
2-ethoxyethanol
2
13.99
12.70
8.69
7.36
13.91
13.99
2-methoxyethanol
2
12.42
11.11
6.02
5.14
9.83
10.74
2-methyl-1-propanol
3
9.32
8.40
6.00
4.79
*
*
2-propanol
3
4.81
4.25
3.00
2.55
4.91
4.69
3-methyl-1-butanol
3
13.42
12.25
9.86
8.26
15.28
13.55
acetic acid
3
22.47
20.34
6.52
4.61
8.84
8.96
acetone
3
3.02
2.64
2.89
2.50
4.64
7.68
acetonitrile
2
6.91
5.83
3.28
2.47
4.32
8.89
anisole
3
18.65
17.09
17.12
16.28
25.00
22.84
benzene
1
5.23
4.54
5.98
3.83
11.63
9.17
butyl acetate
3
8.86
7.88
12.12
11.38
19.43
19.63
carbon tetrachloride
1
3.96
3.49
5.61
5.90
11.89
7.42
chlorobenzene
2
13.91
12.54
13.55
13.14
21.56
18.48
chloroform
2
7.31
6.41
5.23
4.64
9.18
6.66
cumene
3
12.36
11.17
16.66
16.69
25.88
20.90
cyclohexane
2
2.16
2.01
5.37
5.89
*
*
dichloromethane
2
5.01
4.33
3.31
3.06
5.87
4.88
dimethylsulfoxide
3
26.47
24.43
16.62
13.01
18.81
30.95
ethanol
3
4.98
4.37
2.52
2.19
4.03
3.80
ethyl acetate
3
4.08
3.56
4.87
4.44
9.04
10.35
ethyl benzene
2
10.72
9.58
13.86
13.81
22.54
18.18
ethyl ether
3
1.72
1.63
2.58
2.67
5.34
3.87
ethyl formate
3
3.16
2.78
3.00
2.78
5.46
6.48
ethylene glycol
2
28.06
26.23
10.77
6.63
12.59
13.86
formamide
2
32.99
30.93
11.85
7.30
12.72
19.93
formic acid
3
24.64
22.09
5.19
2.60
5.59
5.06
heptane
3
1.98
1.86
6.34
6.98
14.18
7.84
hexane
2
1.65
1.58
3.77
4.11
9.06
4.86
isobutyl acetate
3
6.99
6.18
10.39
9.69
17.35
18.02
isopropyl acetate
3
4.26
3.74
6.19
5.71
11.47
12.38
methanol
2
4.23
3.64
1.96
1.80
3.14
2.93
methyl acetate
3
3.19
2.80
3.17
2.93
5.80
7.10
methylbutyl ketone
2
9.10
8.05
11.81
10.50
17.94
20.81
methylcyclohexane
2
2.50
2.30
7.31
7.95
15.49
9.21
methylethyl ketone
3
4.33
3.76
4.90
4.09
7.99
11.55
methylisobutyl ketone
3
6.84
5.97
9.64
8.49
15.35
18.41
m
-xylene
2
11.21
10.04
14.29
14.17
23.01
18.78
N,N-dimethylacetamide
2
20.75
19.01
12.95
13.96
21.42
30.00
N,N-dimethylformamide
2
18.04
16.26
13.09
10.23
16.52
26.19
nitromethane
2
11.82
10.31
4.84
3.53
6.30
12.01
N-methylpyrrolidone
2
29.84
27.86
25.09
21.85
29.99
38.08
o
-xylene
2
12.79
11.51
15.46
15.26
24.23
20.33
pentane
3
1.49
1.45
2.39
2.62
5.36
3.29
propyl acetate
3
5.98
5.29
8.03
7.44
*
*
p
-xylene
2
10.98
9.82
14.29
14.17
22.99
18.69
pyridine
2
12.64
11.24
9.60
8.57
15.40
16.45
sulfolane
2
47.62
43.31
34.02
28.90
36.76
48.67
tert
-butylmethyl ether
3
1.94
1.82
3.50
3.59
7.52
5.73
tetrahydrofuran
3
3.63
3.19
5.12
4.90
9.81
9.48
tetralin
2
25.12
23.48
27.49
27.44
37.27
31.72
toluene
2
7.86
6.91
9.80
9.66
17.36
14.00
1,1-diethoxypropane
—
5.42
4.84
11.39
11.38
19.82
15.08
2,2-dimethoxypropane
—
3.11
2.79
5.48
5.55
11.37
8.67
2-chloropropane
—
1.96
1.82
2.67
2.66
5.20
4.61
2-methylpentane
—
1.58
1.52
3.22
3.56
7.72
4.32
acetaldehyde
—
2.05
1.85
1.86
1.84
3.14
3.90
chloroethane
—
1.83
1.71
2.14
2.10
3.97
3.55
chloromethane
—
1.63
1.55
1.70
1.70
3.01
2.73
ethylene oxide
—
2.05
1.86
1.89
2.02
3.59
3.92
formaldehyde
—
2.25
1.57
1.68
1.58
2.66
2.59
isoamyl acetate
—
10.51
9.43
14.84
14.18
22.80
22.62
isooctane
—
1.85
1.75
5.84
6.59
13.66
8.07
isopropyl ether
—
1.86
1.76
4.03
4.23
9.03
5.83
methyl cyclopentane
—
1.91
1.79
4.50
4.93
10.41
5.81
methyl isopropyl ketone
—
4.93
4.29
6.58
5.69
11.04
14.47
methylal
—
2.26
2.06
2.84
2.82
5.65
5.09
trichloroethene
—
6.50
5.70
7.07
7.05
13.58
9.75
water
—
8.24
7.18
1.74
1.68
2.75
2.57
*Not determined
Retention time data collected using the following conditions:
G16Stabilwax®:
30m, 0.25mm ID, 0.5µm df, Phase ratio: 125, Oven program: 40ºC, hold 1min., to 190ºC@ 4ºC/min., hold 15min., Carrier flow: 1.2mL/min., Dead time: 1.38min.@ 45ºC
G16Rtx®-WAX:
30m, 0.25mm ID, 0.5µm df, Phase ratio: 125, Oven program: 40ºC, hold 1min., to 190ºC@ 4ºC/min., hold 15min., Carrier flow: 1.2mL/min., Dead time: 1.40min.@ 45ºC
G43Rtx®-1301:
30m, 0.25mm ID, 1.0µm df, Phase ratio: 63, Oven program: 40ºC, hold 1min., to 190ºC@ 4ºC/min., hold 15min., Carrier flow: 1.2mL/min., Dead time: 1.40min.@ 45ºC
G27Rxi®-5ms:
30m, 0.25mm ID, 1.0µm df, Phase ratio: 63, Oven program: 40ºC, hold 1min., to 190ºC@ 4ºC/min., hold 15min., Carrier flow: 1.1mL/min., Dead time: 1.49min.@ 45ºC
G1Rtx®-1:
60m, 0.53mm ID, 3.00µm df, Phase ratio: 43, Oven program: 30ºC, hold 4min., to 220ºC@ 4ºC/min., Carrier flow: 6.3mL/min., Dead time: 2.54min.@ 35ºC
Rtx®-200:
60m, 0.53mm ID, 3.00µm df, Phase ratio: 43, Oven program: 30ºC, hold 4min., to 220ºC@ 4ºC/min., Carrier flow: 7.8mL/min., Dead time: 2.22min.@ 35ºC
Reducemethoddevelopment time—usea retention time index for column selection.
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Mar 2011