Separation of the Enantiomers of Ibuprofen on Epitomize Chiral Phase CSP-1C
The Epitomizeâ„¢ CSP-1C chiral stationary phase uses cellulose tris-(3,5-dimethylphenylcarbamate) as the chiral receptor and is offered in a variety of particle sizes including 1.7, 3, 5, 10, 20, 50, 100, and 300 microns.
The Epitomize™ CSP-1C chiral stationary phase uses cellulose tris-(3,5-dimethylphenylcarbamate) as the chiral receptor and is offered in a variety of particle sizes including 1.7, 3, 5, 10, 20, 50, 100, and 300 microns. In this application, the enantiomers of ibuprofen in its free acid form (α-methyl-4-(isobutyl)phenylacetic acid, see Figure 1) have been separated using an Epitomize CSP-1C column packed with a 5-micron diameter, spherical chiral stationary phase.
Figure 1: Ibuprofen.
Experimental
The CSP-1C, 5 micron column configuration was 4.6 mm ID × 250 mm long. The mobile phase was 1% 2-propanol in n-heptane containing 0.1% TFA and the flow rate was 1.0 mL/min. The pressure drop observed was 620 psi (43 bar). The injection volume was 20 μL.
Figure 2: Separation of racemic ibuprofen on Epitomize CSP-1C, 5 μm at a flow rate of 1.0 mL/min.
Results
The chromatogram in Figure 2 shows the baseline separation of racemic ibuprofen, and Figure 3 shows the standard for the pure (S)-(+)-enantiomer, which denotes the order of separation. The retention time of the (R)-(–)-enantiomer was 10.3 min, the retention time of the (S)-(+)-enantiomer was 11.9 min, and the separation value for the racemate was 1.22.
Figure 3: Chromatogram of (S)-(+)-ibuprofen on Epitomize CSP-1C, 5 μm at a flow rate of 1.0 mL/min.
Conclusion
The enantiomers of ibuprofen were separated using an Epitomize CSP-1C, 5 μm column. This separation may be directly scaled up to commercial volumes using the CSP-1C stationary phase in a simulated moving bed chromatograph. The availability of CSP-1C in larger particle sizes permits the use of low pressure (less than 300 psi) SMB. Low pressure SMB, or LP-SMB, is a lower-cost alternative to high-pressure SMB units. Currently LP-SMB units are available that offer production rates from hundreds of grams per day to over 50 kilograms per day.
Orochem Technologies, Inc.
331 Eisenhower Ln South, Lombard, IL 60148
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Website: www.orochem.com
SEC-MALS of Antibody Therapeutics—A Robust Method for In-Depth Sample Characterization
June 1st 2022Monoclonal antibodies (mAbs) are effective therapeutics for cancers, auto-immune diseases, viral infections, and other diseases. Recent developments in antibody therapeutics aim to add more specific binding regions (bi- and multi-specificity) to increase their effectiveness and/or to downsize the molecule to the specific binding regions (for example, scFv or Fab fragment) to achieve better penetration of the tissue. As the molecule gets more complex, the possible high and low molecular weight (H/LMW) impurities become more complex, too. In order to accurately analyze the various species, more advanced detection than ultraviolet (UV) is required to characterize a mAb sample.
