Quantitation of cefepime.2HCl dihydrate in cefepime.2HCl monohydrate by diffuse reflectance IR and powder X-ray diffraction techniques.
The identification, characterization and quantitation of crystal forms is becoming increasingly important within the pharmaceutical industry. Multi-disciplinary, physical analytical techniques are necessary for this task. In this work, diffuse reflectance mid-infrared (IR) and powder X-ray diffraction (XRD) analyses were used to identify two different hydrated forms of cefepime.2HCl, a cephalosporin. Characterization of the mono- and dihydrate forms led to separate IR and XRD quantitative assays for the determination of dihydrate content in cefepime.2HCl monohydrate bulk material. For the IR assay, a working range of 1.0-8% (w/w) was established with a minimum quantifiable level (MQL) of 1.0% (w/w) and a limit of detection (LD) of 0.3% (w/w) dihydrate in monohydrate material. The XRD assay displayed a working range of 2.5-15% (w/w) with an MQL of 2.5% (w/w) and an LD of 0.75% (w/w). Cross validation was performed between the two techniques, with a good correlation displayed for each assay as compared with the known concentrations and as compared with each other. In addition, a full evaluation of potential assay errors was made.
Bristol-Myers Squibb Pharmaceutical Research Institute, New Brunswick, NJ 08903, USA. david_e._bugay@ccmail.bms.com
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D000077723:Cefepime; D002511:Cephalosporins / Q000032:analysis* / Q000737:chemistry; D008855:Microscopy, Electron, Scanning; D010316:Particle Size; D011208:Powders; D017550:Spectroscopy, Fourier Transform Infrared / Q000379:methods*; D014961:X-Ray Diffraction / Q000379:methods*
D002511:Cephalosporins; D011208:Powders; D000077723:Cefepime