738
HPLCCHROMATOGRAMS |
PHARMACEUTICAL
Analgesics
Peak List:
Conc. (µg/mL)
U. unknown
unknown
1. morphine sulfate
204
2. acetaminophen
92
3. codeine phosphate
216
4. oxycodoneHCl
206
5. hydrocodone bitartrate 218
LC_0221
AnalgesicAcetaminophenandNarcoticAnalgesics
onUltraC18
Sample:
Inj.:
4.0µL
Sample:
rawmaterial mix
Solvent:
mobile phase
Column:
Ultra C18
Cat.#:
9174575
Dimensions:
250mm x 4.6mm
Particle size:
5µm
Pore size:
100Å
Conditions:
Mobilephase:
A: 10mmpotassium
phosphate, pH 2.8
B: acetonitrile:methanol,
(90:10, v/v)
(85A:15B, v/v)
Flow:
1.0mL/min.
Temp.:
35°C
Det.:
UV@ 235nm
Column:
Pinnacle
®
II C18
Cat.#:
9214575-700
Dimensions:
250mm x 4.6mm
Particle size:
5µm
Pore size:
110Å
Conditions:
Mobile phase: A: 0.73g 1-heptane
sulfonic acid and 10mL
glacial acetic acid, diluted
to 720mLwithwater, pH= 2.33
B: methanol (72A:28B, v/v)
Flow:
1.00mL/min.
Temp.:
26.5°C
Det.:
UV@ 284nm
LC_0209
NarcoticAnalgesicMorphineSulfateRawMaterial -
USP25:ResolutionSolutiononPinnacle® IIC18
Peak List:
Conc. (µg/mL)
1. unknown
unknown
2. phenol
0.15
3.morphine sulfate 0.24
Sample:
Inj.:
20µL
Solvent:
mobile phase
0
1
2
3
4 min.
Peak List:
Ret. Time (min.) Inj. %RSD (n= 5)
1. hydrocodone bitartrate
3.1
0.37%
Sample:
Inj.:
20µL
Conc.:
1µg/mL
Sample:
assay standard
Solvent:
mobile phase
LC_0211
NarcoticAnalgesicHydrocodoneBitartratebyUSP25
onPinnacle® IISilica
Column:
Pinnacle
®
II Silica
Cat.#:
9210575
Dimensions:
250mm x 4.6mm
Particle size:
5µm
Pore size:
110Å
Conditions:
Mobile phase:
A: 800mL acetonitrile; 4mLwater;
1mL diethylamine
B: methanol (55A:45B, v/v)
Flow:
1.5mL/min.
Temp.:
27°C
Det.:
UV@ 280nm
Impurities resolved
from primary peak.
Column:
Ultra C8
Cat.#:
9103564
Dimensions:
150mm x 4.0mm
Particle size:
5µm
Pore size:
100Å
Conditions:
Mobile phase:
A: 5mM hexane sulfonic acid
with 2mLTEA and 3mL of
phosphoric acid per liter.
pH adjusted to 2.5
B: methanol (90A:10B, v/v)
Flow:
1.5mL/min.
Temp.:
40°C
Det.:
UV@ 206nm
NarcoticAnalgesicOxycodoneHClRawMaterialby
USP25:ResolutionSolutiononUltraC8
LC_0213
Peak List:
Conc. (µg/mL)
Ret. Time (min.)
RRT Tailing Res.
1. codeine phosphate
13
19.3
0.7
1.1
—
2. oxycodoneHCl
9
26.8
1.0
0.99 3.3
Sample:
Inj.:
10µL
Sample:
resolution solution
Solvent:
mobile phase
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E-mail :
TelNo : 03 9762 2034 . . . inAUSTRALIA
Mar 2011
