Azactam (aztreonam injection) is a synthetic monocyclic beta-lactam antibiotic.  Two unknown impurities at above 1% level were observed in the 12-month shelf life expiry HPLC/UV chromatograms.   In order to identify the impurities and provide them as standards for HPLC /UV validation, they were isolated (1-3 mg, each) using preparative HPLC.  Their structures were determined using HRMS, one and two-dimensional NMR spectroscopy.  Quantitative NMR (QNMR) was used to determine their accurate concentrations such that the isolated impurity solutions can be used as standards for HPLC/UV method validation.  The strategy of using QNMR to provide accurate isolated sample concentration allows us to avoid the need to isolate or synthesize larger quantities of materials for HPLC/UV method validation, thus saving time and reducing cost. This presentation describes the detailed isolation, structural elucidation and QNMR analysis of the two impurities.

Isolation, structural characterization, and quantitative NMR determination of impurities in aztreonam injection

245th National Meeting (2013)

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