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Determination of 2-chloro-4,5-difluorobenzoic acid and related impurities by liquid chromatography

2-Chloro-4,5-difluorobenzoic acid (CDFBA) and related impurities are determined using liquid chromatography (LC). Separations are achieved using a reversed-phase isocratic system with an ion-pair reagent (tetrabutylammonium hydroxide). Unique isomeric impurities observed in commercially produced CDF...

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Bibliographic Details
Published in:Analytica chimica acta 1993-08, Vol.280 (1), p.85-92
Main Authors: Elrod, Lee, Spanton, Stephen G., Cirovic, Moike, Shaffer, Dean I., Golich, Timothy G., Linton, Cathie L., Vievia, Douglas R., Kalaritis, Pano, Schmand, Horst
Format: Article
Language:English
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Summary:2-Chloro-4,5-difluorobenzoic acid (CDFBA) and related impurities are determined using liquid chromatography (LC). Separations are achieved using a reversed-phase isocratic system with an ion-pair reagent (tetrabutylammonium hydroxide). Unique isomeric impurities observed in commercially produced CDFBA were isolated and identified by NMR and single crystal x-ray diffraction. The method has relative standard deviations of ± 0.55% to ±1.26% for the CDFBA determination and from ±4.3% to ±12% for impurities below 0.3% in CDFBA. Impurities are determinable to at least 0.03% by weight.
ISSN:0003-2670
1873-4324
DOI:10.1016/0003-2670(93)80245-G