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1
PeakList:
1. unknown
2. levothyroxine
Sample:
Inj.:
20µL
Conc.:
1.1µg/mL
Solvent: water:methanol
(70:30)
Add 3 drops of concentrated
ammonium hydroxide to each
10mL of the sample diluent.
Levothyroxine will not dissolve
unless the pH is basic.
Column:
UltraPFP
Catalog #:
9199565
Dimensions:
150 x 4.6mm
Particle size:
5µm
Pore size:
100Å
Conditions:
Mobile phase: 10mM ammonium
formate, pH2.5:
methanol
(60:40, v/v)
Flow rate:
1.2mL/min.
Temp.:
25°C
Det.:
UV@254nm
2
0 2 4 6 8 10 12 14 16 min.
LC_0093
Figure4
Multi-halogenated analytes as levothyroxine can also
take advantage of the Ultra PFP’s strong retention
Figure5
The strong retention of the PFPmakes it an excellent
phase for the analysis of purines and pyrimidines.
0
5
10
15
20
25 min.
1
2
3
4
5
6
7
8
11 9
10
12 14 13
LC_0136
Sample:
Inj.:
10µL
Conc.:
100µg/mL
Solvent: mobile phase
Column:
UltraPFP
Catalog #:
9176575
Dimensions:
250 x 4.6mm
Particle Size:
5µm
PoreSize:
100Å
Conditions:
Mobile Phase: 50:50 0.001% (v/v)
FormicAcid inWater:
Methanol
Flow: 1.0mL/min
Temp.: ambient
Det.:UV@260nm
PeakList:
1. cytosine
2. 5-methylcytosine
3. uracil
4. uric acid
5. hypoxanthine
6. xanthine
7. thymine
8. purine
9. 6-methylpurine
10. theobromine
Figure6
HPLC/MSESI analysis of beta-blockers on the
Ultra PFP column shows good intensity
Data courtesy of Shane Needham, Pfizer Inc
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15min.
1.93e8cps
1
2
3 4
Peak list:
1 = atenolol
2 = acetbutolol
3 = alprenolol
4 = propranolol
Table I
Retention Data of Basic Solutes with 90% Acetonitrile
Retention Time (min.)
β
-blockers
CN OH PFP C4*
Acebutolol
3.22
2.02
6.32
<0.5
Alprenolol
3.79
1.74
9.99
<0.5
Atenolol
3.04
2.15
4.63
<0.5
Labetolol
3.56
1.32
4.93
<0.5
Metoprolol
3.42
1.83
7.70
<0.5
Nadolol
3.37
2.15
5.58
<0.5
Oxprenolol
3.81
1.78
9.20
<0.5
Pindolol
3.64
1.81
6.60
<0.5
Propranolol
3.27
1.78
10.3
<0.5
Sotalol
3.12
1.69
5.09
<0.5
Timolol
3.37
1.74
7.53
<0.5
*<20% acetonitrile needed for adequate retention
Data courtesy of Shane Needham, Pfizer Inc
References
1. S.R.Needham,P.R.Brown, andK.Duff,
RapidCommun.MassSpectrom.
13, 2231-2236 (1999).
2. J. Svensson.,
J. Anal. Toxicol.
, 10 (1986) 122-124.
3. P. Sjoberg andK.Markides.,
J. Chromatogr. A.
, 855 (1999) 317-327.
4. S.R.Needham,
op. cit.
5. B.Matuszewski,M.Constanzer, andC.Chavez-Eng.
Anal.Chem
70 (1998) 882-889.
6. S.R.Needham,
op. cit.
References not available fromRestek.
11. ethyluracil
12. 1,7-dimethylxanthine
13. theophylline
14. propyluracil
