700
GCCHROMATOGRAMS |
PHARMACEUTICAL
Organic Volatile Impurities/Residual Solvents
Column:
Rtx
®
-1301, 30m, 0.53mm ID x 3.0µm (cat.# 16085)
Sample:
headspace injection of 28 Class 1 and 2 residual solvents for pharmaceutical processing,
prepared at the regulatory limit concentration, using samples shaken and heated at 80°C
for 15min., 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
2
4
6
8
10 12 14 16 18 20 22 24 26 28
30 32 34
1 2
3
4
5
6
7
8
9,10
11 12 13,14
15
16
17
18
19
20 21
22,23
24,25
26
27
28
GC_PH00553
ResidualSolvents
EuropeanPharmacopoeiaClass1andClass2
Rtx®-1301
(headspace)
Inj.:
static headspace injection (see static headspace conditions)
Inj. temp.:
180°C
Carrier gas:
helium, split 2:1
Linear velocity: 5mL/min., constant flow
Oven temp.:
40°C for 20min. to 240°C at 25°C/min. (hold for 10min.)
Det.:
FID@ 250°C
hydrogen flow: 40mL/min.
air flow:
450mL/min.
make-up flow: 45mL/min.
Static Headspace (Loop) Conditions:
Instrument:
TeledyneTekmar HT3
Valve oven temp.:
150°C
Transfer line temp.:
150°C
Standby flow rate:
10mL/min.
Platen/sample temp.:
80°C
Platen temp equil. time: 2.00min.
Sample equil. time:
15.00min.
Mixer time:
2.00min.
Mixing level:
5
Mixer stabilize time:
0.50min.
Pressurize:
15psi
Pressurize time:
2.00min.
Pressurize equil. time: 0.50min.
Loop fill pressure:
5psi
Loop fill time:
2.00min.
Loop fill equil. time:
0.50min.
Inject time:
1.00min.
Column:
Rtx
®
-G43, 30m, 0.53mm ID, 3.0µm (cat.# 16085-126)
Sample:
USP<467>CalibrationMixture#5 (cat.# 36007) inDMSO stock
standard. To each 22mL headspace vial 5ml water,~ 1.0g of sodium
sulfate and 100µL of stock standardwere added.
The preparation yielded the following concentrations,
RetentionTime (min.) Sample Concentration (µg/mL)
1. dichloromethane
5.110
12.0
2. chloroform
9.285
1.2
3. benzene
11.173
0.04
4. trichloroethylene
14.647
1.6
5. 1,4-dioxane
17.436
7.6
GC_PH00810
OrganicVolatile Impurities
USP<467>
Rtx®-G43
(staticheadspace)
Website :
E-mail :
TelNo : 03 9762 2034 . . . inAUSTRALIA
Mar 2011
