HPLC Separation of Positional Isomers of Trifluorophenylacetic Acid and its Starting Material

Trifluorophenylacetic acid (TFPAA) was synthesized from 2,4,5-trifluorophenyl bromide and malonic acid starting materials as part of process development for a pharmaceutical intermediate. Impurity profile methods, sensitive to positional isomers, have been developed for 2,4,5-trifluorophenyl bromide...

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Bibliographic Details
Published in:Journal of liquid chromatography & related technologies 2005-11, Vol.28 (19), p.3131-3142
Main Authors: Pinto, Angela M., Antonucci, Vincent, Moeder, Charles, Natishan, Theresa K., Novak, Tom J.
Format: Article
Language:English
Subjects:
2,4,5-Trifluorophenyl bromide
2,4,5-Trifluorophenylacetic acid
Analysis
Analytical chemistry
Biological and medical sciences
Chemistry
Chromatographic methods and physical methods associated with chromatography
Exact sciences and technology
General pharmacology
HPLC
LC-MS
Medical sciences
Other chromatographic methods
Pharmacology. Drug treatments
Positional isomers
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Summary:Trifluorophenylacetic acid (TFPAA) was synthesized from 2,4,5-trifluorophenyl bromide and malonic acid starting materials as part of process development for a pharmaceutical intermediate. Impurity profile methods, sensitive to positional isomers, have been developed for 2,4,5-trifluorophenyl bromide and 2,4,5-TFPAA. The HPLC impurity profile method for 2,4,5-TFPAA was validated consistent with ICH guidelines. An HPLC weight percent assay method was also developed and validated for 2,4,5-TFPAA. Residual malonic acid in 2,4,5-TFPAA was determined with a weight percent method by GC. Non-positional isomer impurities in 2,4,5-TFPAA were identified by LC-MS.
ISSN:1082-6076
1520-572X
DOI:10.1080/10826070500295278