The identification of impurities requires sophisticated analytical techniques and experienced know-how. We offer the complete structural elucidation of unknowns using up-to-date analytical instrumentation and a multi-step approach:
- Isolation and clean-up of unknown impurities using an analytical fraction collector.
- Recording of UV/VIS- and IR-spectra.
- Elucidation of the molecular mass and empirical formula by Quadrupole Time-Of-Flight system (Agilent Technologies LC-QTOF 6530) with a mass resolution < 2 milli-mass units. The mass spectral fragmentation pattern provides information about the molecular structure.
- Structure determination by micro- NMR (Bruker AMX 600 MHz) in combination with a 20 µl detection cell. This enables elucidation of the structure even with small sample amounts.
The procedure for identification of unknowns is a non-routine operation. Therefore, we develop problem-solving strategies for each particular case.
High resolution mass spectrum of unknown impurity
(m/z 313.2171 complies with C21H29O2 = protonated molecular ion of pregna-4,14-dien-3,20-dione)
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