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Application No.L495
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n Automated Optimization of Chiral Separation ranking results from the optional software. The software
Parameters for Omeprazole automatically ranks all the chromatograms with
Fig. 3 shows the results from a total of 36 possible separation greater than a given criteria (in this case, 1.5).
combinations of 12 chiral columns and 3 types of This confirmed the utility of using the Nexera UC chiral
modifiers (methanol, ethanol, and acetonitrile/ethanol screening system to automatically optimize separation
mixture). parameters for chiral SFC, which otherwise requires a
For omeprazole, separation of peaks for two chiral forms complicated process of selecting analytical conditions.
were confirmed within 8 minutes of retention. Fig. 4
shows the separation evaluation and optimal parameter

Modifier: Methanol Ethanol
IA IB IC ID IA IB IC ID

IE IF AD AS IE IF AD AS

AY OD OJ OZ AY OD OJ OZ

Acetonitrile/ethanol = 75/25 (v/v)
Column Stationary phase
Amylose tris (3, 5-dimethylphenylcarbamate)
IA IB IC ID CHIRALPAK ® IA-3/SFC (IA) Cellulose tris (3, 5-dimethylphenylcarbamate)
CHIRALPAK ® IB-3/SFC (IB)
CHIRALPAK ® IC-3/SFC (IC) Cellulose tris (3, 5-dichlorophenylcarbamate)
CHIRALPAK ® ID-3/SFC (ID) Amylose tris (3-chlorophenylcarbamate)
CHIRALPAK ® IE-3/SFC (IE) Amylose tris (3, 5-dichlorophenylcarbamate)
IE IF AD AS CHIRALPAK ® IF-3/SFC (IF) Amylose tris (3-chloro-4-methylphenylcarbamate)
CHIRALPAK ® AD-3/SFC (AD) Amylose tris (3, 5-dimethylphenylcarbamate)
CHIRALPAK ® AS-3/SFC (AS) Amylose tris [(S)-Ћ-methylbenzylcarbamate]
CHIRALPAK ® AY-3/SFC (AY) Amylose tris (5-chloro-2-methylphenylcarbamate)
AY OD OJ OZ CHIRALCEL ® OD-3/SFC (OD) Cellulose tris (3,5-dimethylphenylcarbamate)
CHIRALCEL ® OJ-3/SFC (OJ) Cellulose tris (4-methylbenzoate)
CHIRALCEL ® OZ-3/SFC (OZ) Cellulose tris (3-chloro-4-methylphenylcarbamate)
Fig. 3 Comparison of Separation Using Different Combinations of 12 Chiral Columns and 3 Modifiers

Ranking Run No. Analytical Condition Resolution Separatoin factor Symmetry factor Retention factor Area% Peak
Peak1 Peak2 Peak1 Peak2 Peak1 Peak2 number
1 32 Omeprazole_OZ-3_MeOH_20_40 7.965 1.921 1.16 1.159 6.583 12.644 49.829 50.171 2
2 17 Omeprazole_IC-3_MeOH_20_40 5.587 1.602 1.387 1.274 8.078 12.937 49.971 50.029 2
3 16 Omeprazole_IC-3_EtOH_20_40 5.382 1.639 1.915 1.661 8.617 14.124 49.984 50.016 2
4 31 Omeprazole_OZ-3_EtOH_20_40 5.377 1.599 1.169 1.162 7.229 11.561 49.778 50.222 2
5 1 Omeprazole_AD-3_EtOH_20_40 3.996 1.509 1.257 1.404 8.779 13.25 50.054 49.946 2
6 8 Omeprazole_AY-3_MeOH_20_40 3.55 2.08 1.178 1.145 3.652 7.597 49.974 50.026 2
7 11 Omeprazole_IA-3_MeOH_20_40 3.428 1.523 1.464 1.312 7.435 11.327 49.973 50.027 2
8 4 Omeprazole_AS-3_EtOH_20_40 2.515 1.673 1.657 1.518 1.244 2.081 49.754 50.246 2
9 10 Omeprazole_IA-3_EtOH_20_40 1.586 1.157 1.322 1.279 7.115 8.234 49.347 50.653 2
Separation Parameters for Rank 1
Column: CHIRALCEL OZ-3/SFC
®
Modifier: Methanol
Separation Parameters for Rank 2
®
Column: CHIRALPAK IC/SFC
Modifier: Methanol
Separation Parameters for Rank 3
Column: CHIRALPAK IC/SFC
®
Modifier: Ethanol
Fig. 4 Evaluation of Separation Parameters and Chiral Separation Chromatogram Using Optimized Parameters

* CHIRALPAK and CHIRALCEL are registered trademarks of Daicel
®
®
Corporation.
First Edition: Oct. 2015

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