Quantitation of cefepime center dot 2HCl dihydrate in cefepime center dot 2HCl monohydrate by diffuse reflectance IR and powder X-ray diffraction techniques

被引:62
作者
Bugay, DE
Newman, AW
Findlay, WP
机构
[1] Bristol-Myers Squibb P., New Brunswick, NJ 08903, One Squibb Drive
关键词
quantitative analysis of hydrates; cefepime center dot 2HCl monohydrate; cefepime center dot 2HCl dihydrate; infrared spectroscopy; powder X-ray diffraction;
D O I
10.1016/0731-7085(96)01796-7
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
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.
引用
收藏
页码:49 / 61
页数:13
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