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Low level determination of p-toluenesulfonate and benzenesulfonate esters in drug substance by high performance liquid chromatography/mass spectrometry.
- Source :
-
Journal of chromatography. A [J Chromatogr A] 2006 Jun 30; Vol. 1119 (1-2), pp. 231-7. Date of Electronic Publication: 2005 Dec 27. - Publication Year :
- 2006
-
Abstract
- GC/FID and HPLC/MS single ion monitoring methods have been evaluated for the determination of trace levels of methyl, ethyl and isopropyl esters of p-toluenesulfonic acid and methyl, ethyl, isopropyl and n-butyl esters of benzenesulfonic acid in drug substances. These sulfonate esters have been highlighted as potential genotoxins. HPLC/MS was found to be more promising and limits of quantification were between 2.5 and 5 ng/mL, which enabled detection limits in drug substance at 0.01-0.1 ppm for a 50 mg/mL solution. For one drug substance excellent recoveries of 94-95% were obtained at the 1.0 ppm level, however, with a second drug substance, a besylate salt, recoveries ranged from 86% to 100% and were dependant on the sample preparation. Limited stability of the sulfonate esters in various potential sample solutions indicated that samples may need to be prepared immediately before injection.
Details
- Language :
- English
- ISSN :
- 0021-9673
- Volume :
- 1119
- Issue :
- 1-2
- Database :
- MEDLINE
- Journal :
- Journal of chromatography. A
- Publication Type :
- Academic Journal
- Accession number :
- 16376906
- Full Text :
- https://doi.org/10.1016/j.chroma.2005.11.088