Restek Corporation • (800) 356-1688 • (814) 353-1300 •
30m, 0.53mm ID, 5.0µmRtx
®
-G27with 5m phenylmethyl Integra-Guard
™
(cat.# 10279-126).
Headspace injection of 24 common residual solvents for pharmaceutical processing. Prepared to equal about 500ppm in
the bulk pharmaceutical. Samples shaken and heated at 90°C for 15minutes, 1mL headspace injection.
Oven temp.:
35°C (hold 10min.) to 100°C@ 5°C/min., to 240°C@ 25°C/min. (hold 5min.);
Inj./det. temp.:
220°C/240°C;
FID sensitivity:
1.05 x 10
-11
AFS;
Carrier gas:
helium, 35cm/sec. set@ 35°C;
Split ratio:
2:1.
2
3
4
1
2
min.
4
10
12
14
6
8
16
18
7,5,6 8
11,9
10
12
13
14
15
17,16,21
18
19
20
22
23
24
20
22
ethanol
1. ethylene oxide
2. methanol
3. diethyl ether
4. 1,1-dichloroethene
5. acetone
6. isopropanol
7. acetonitrile
8. methylene chloride
9.
n
-hexane
10.
n
-propanol
11. methyl ethyl ketone
12. ethyl acetate
13. tetrahydrofuran
14. chloroform
15. 1,1,1-trichloroethane
16. carbon tetrachloride
17. benzene*
18. 1,2-dichloroethane
19. heptane
20. trichloroethylene
21.
n
-butanol
22. 1,4-dioxane
23. pyridine
24. toluene
30m x .53mm ID x 3.0mmRtx
®
-G43 (cat.# 16085-126).
Headspace injection of 28Class 1 and 2 residual solvents for pharmaceutical
processing. Prepared at the regulatory limit concentration. Samples shaken and
heated at 80°C for 15minutes, 1mL headspace injection.
Oven temp.:
40°C (hold 20min.) to 240°C@ 10°C/min. (hold 20min.);
Inj./det. temp.:
200°C/250°C;
FID sensitivity:
1.1 x 10
-11
AFS;
Carrier gas:
hydrogen@ 35cm/sec.;
Split ratio:
2:1.
1. methanol
2. 1,1-dichloroethene
3. acetonitrile
4. methylene chloride
(dichloromethane)
5. hexane (C6)
6.
cis
-1,2-dichloroethene
7. nitromethane
8. chloroform
9. cyclohexane
10. 1,1,1-trichloroethane
11. carbon tetrachloride
12. benzene*
13. 1,2-dimethoxyethane
14. 1,2-dichloroethane
15. trichloroethylene
(1,1,2-trichlorethene)
16. methylcyclohexane
17. 1,4-dioxane
18. pyridine
19. toluene
20. 2-hexanone
21. chlorobenzene
22. DMF
23. ethylbenzene
24.
m
-xylene
25.
p
-xylene
26.
o
-xylene
27. N,N-dimethylacetamide
28. 1,2,3,4-
tetrahydronaphthalene
min. 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34
1 2
3
4
5
6 9,10
7
8 11
12 13,14
15
16
17
18
19
20 21
22,23
24,25
26
27
28
Same peak list as Figure 5.
min. 1 2 3 4 5 6 7 8 9 10 26 28 30
28
27
22
21
18, 26
7
24
25 23
20
14
17
19
3 8
6, 15
12
4
1
10, 11
16
2
5, 9
*Testing for benzene only requiredwhen
specified in the individual monograph.
*Testing for benzene only requiredwhen
specified in the individual monograph.
Figure 4
AnRtx
®
-G27 column resolvesmany solvents commonly used in pharmaceutical processing.
Figure 5
AnRtx
®
-G43 column shows excellent resolution of commonly-used pharmaceutical processing solvents.
EuropeanPharmacopoeiaClass 1 andClass 2 compounds at the regulation limit concentration.
*Testing for benzene only requiredwhen
specified in the individual monograph.
Figure 6
A Stabilwax
®
columnmakes an excellent confirmation column for commonly-used pharmaceutical processing solvents.
EuropeanPharmacopoeiaClass 1 andClass 2 compounds at the regulation limit concentration.
30m x .53mm ID x 0.5µmStabilwax
®
(cat.# 10640-126). Headspace injection of 28Class 1
and 2 residual solvents for pharmaceutical processing. Prepared at the regulatory limit
concentration. Samples shaken and heated at 80°C for 15minutes, 1mL headspace injection.
Oven temp.:
50°C (hold 20min.) to 165°C@ 6°C/min. (hold 20min.);
Inj./det. temp.:
200°C/250°C;
FID sensitivity:
1.1 x 10
-11
AFS;
Carrier gas:
hydrogen@ 35cm/sec.;
Split ratio:
2:1
