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Thesis
Chiral and Achiral HPLC Separation of Chiral Pharmaceutical Compounds
Master of Science (M.S.), Drexel University
Jun 2020
DOI:
https://doi.org/10.17918/00001070
Abstract
This project is focused on developing a liquid chromatographic method that separates four Non-Steroidal Anti-Inflammatory Drugs (Ketoprofen, Naproxen, Ibuprofen, and Flurbiprofen) and three of the four pairs of enantiomers in one run. NSAID samples were prepared with 1 mg/mL of Ketoprofen, Naproxen, Ibuprofen, and Flurbiprofen, and 0.5 mg/mL thiourea as a t0 marker in a sample solvent consisting of 1:1 acetonitrile and 0.2% formic acid. The achiral separation of the compounds was investigated using four different columns and two simulations were used to consider the use of two achiral columns connected in tandem to achieve baseline separation of all compounds. The four columns investigated were a 5-cm C18 column, a 5-cm C8 column, a 5-cm perfluoro phenyl column, and a 5-cm biphenyl column. The two simulations were performed using the data from the 5-cm perfluoro phenyl column connected to the 5-cm biphenyl column and the 5-cm perfluoro phenyl column connected to the 5-cm C8 column. The separation of the enantiomers of the NSAIDs was investigated using a chiral column in two different lengths (5-cm, 10-cm) packed with Amylose tris(3,5-dimethylphenylcarbamate) coated on silica gel. The longer column was investigated first. The last method of separation explored utilized the 5-cm version of the aforementioned chiral column connected to each of the achiral columns used during the achiral separations using a zero dead volume column connector. The effect of column order on the retention time and resolution of the NSAIDs was investigated for all the achiral/chiral column combinations. Calculations were performed to predict the retention times and plate numbers for all of the achiral/chiral column combinations and were compared to the values obtained experimentally. The results of the chiral-only and tandem column runs, which employed a reversed-phase mobile phase comprised of aqueous 0.2% formic acid : acetonitrile (67 : 33 v/v), were compared to determine the benefits and drawbacks of each approach, with an emphasis on the resolution and analysis time.
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Details
- Title
- Chiral and Achiral HPLC Separation of Chiral Pharmaceutical Compounds
- Creators
- Karyn Anne Camilo
- Contributors
- Joe Preston Foley (Advisor)
- Awarding Institution
- Drexel University
- Degree Awarded
- Master of Science (M.S.)
- Publisher
- Drexel University; Philadelphia, Pennsylvania
- Number of pages
- xiv, 82 pages
- Resource Type
- Thesis
- Language
- English
- Academic Unit
- College of Arts and Sciences; Chemistry; Drexel University
- Other Identifier
- 991014695236004721