Rapid Equilibration (Even with Low Ionic Strength Acidic Mobile Phases)
When analyzing basic compounds on a typical ODS column with low ionic strength acidic mobile phase, peak shape and long equilibration times are common problems. Shim-pack Arata LC columns can be rapidly equilibrated in low ionic strength acidic mobile phases yielding excellent peak shape and stable retention times.
HN
H
N
1. Dextromethorphan
2. Amitriptyline
Analytical Conditions Instruments
: NexeraX2MP_M30A (STD Cell)
Column
: Shim-pack Arata C18 (3.0 × 75 mm, 2.2 μm) Typical ODS column (3.0 × 75 mm, sub 2 μm),
Mobile Phase
: 0.1% HCOOH in H2O / CH3CN = 70 / 30
Flow Rate Detection
: 0.4 mL/min
: 280 nm
Column Temp.
: 40 °C : 2 μL
Inj. Volume
Sample
: Amitriptyline, Dextromethorphan
Equilibration Time (min) Retention Time (min)
Compounds
10
30
60 120 180 240 360 480 600 720 CV(%)
0.8 0.8 0.8 0.8 0.8 0.8 0.8 0.8 0.8 0.8 0.2 1.20 1.19 1.19 1.18 1.18 1.18 1.18 1.18 1.18 1.18 0.6 1.4 1.4 1.4 1.4 1.4 1.4 1.4 1.4 1.4 1.4 0.3 1.06 1.07 1.06 1.06 1.06 1.06 1.06 1.06 1.06 1.06 0.3
1 Dextromethorphan
Symmetry Factor
Retention Time (min)
2
Amitriptyline
Symmetry Factor
* Both were new columns (shipping solvent : acetonitrile) and equilibrated with mobile phase without any conditioning. Basic drugs were analyzed after a certain period of time of equilibration and RT and symmetry factor of the drugs were compared.
Equilibration Time (min) Retention Time (min)
Compounds
10
30
60 120 180 240 360 480 600 720 CV(%)
1.9 1.8 1.7 1.6 1.5 1.5 1.5 1.4 1.4 1.4 10.4 3.28 3.14 3.01 2.70 2.63 2.56 2.51 2.49 2.56 2.49 10.2 5.3 4.7 4.3 4.0 3.9 3.8 3.7 3.6 3.5 3.6 13.5 4.23 4.23 4.35 4.22 4.13 4.17 4.09 4.02 3.99 3.90 3.1
1 Dextromethorphan
Symmetry Factor
Retention Time (min)
2
Amitriptyline
Symmetry Factor
Comparison of Column Equilibration in The Mobile Phase with 0.1% Formic Acid (Shim-pack Arata C18 vs. Typical ODS Column)
Shim-pack Arata C18
I.D. (mm)
Particle Size (μm)
2.0
3.0
4.6
Length (mm)
50
227-32801-01
227-32802-01
-
75
227-32801-02
227-32802-02
-
2.2
100
227-32801-03
227-32802-03
-
150
227-32801-04
227-32802-04
227-32805-04
250
-
-
227-32805-05
50
227-32803-01
227-32804-01
227-32805-01
75
227-32803-02
227-32804-02
227-32805-02
5.0
100
227-32803-03
227-32804-03
227-32805-03
150
227-32803-04
227-32804-04
227-32805-04
250
-
-
227-32805-05
Pg A-25
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