Determination of the Impurity Profile of R1/CH-13584 by an On-line Gas Chromatography/Mass Spectrometry Method

✍ Scribed by K. Kovács; T. Erös-Takácsy; I. Ritz; J. Hegedüs-Vajda

• Publisher: John Wiley and Sons
• Year: 1996
• Tongue: English
• Weight: 262 KB
• Volume: 10
• Category: Article
• ISSN: 0951-4198
• DOI: 10.1002/(sici)1097-0231(199609)10:12<1536::aid-rcm692>3.0.co;2-m

✦ Synopsis

The impurity profile of the final intermediate in the manufacture of a new, original antiasthmatic drug candidate (CH-13584) was determined by gas chromatographylmass spectrometry. On-line GUMS identification was carried out using electron impact ionization. Gas chromatographic separation was performed on a fused-silica column. Identification was based on mass spectral data: fragmentation patterns and elemental composition for the selected ions as well as the NIST library-search for the separated impurities. GC retention times were also considered. Reference compounds with the proposed structure were synthesized and confirmed by IR, G U M S and NMR data. An identical impurity profile for the certified and the GMP batches proved the reliability of the synthetic process. The possibility of a potential parallel reaction of the impurities in the final reaction step was considered.