Souza Marinês J, Canedo Natália A P, Souza Filho Paulo S, Bergold Ana M
Universidade Federal do Rio Grande do Sul (UFRGS), Faculdade de Farmácia, Programa de Pós-Graduação em Ciências Farmacêuticas, Porto Alegre, RS, Brazil.
J AOAC Int. 2009 Nov-Dec;92(6):1673-80.
A UV spectrophotometric method was developed for determination of ceftiofur sodium in the drug substance and sterile powder for injection. The method validation, which yielded good results, included evaluation of the range, linearity, intra- and interday precision, accuracy, recovery, specificity, robustness, LOQ, and LOD. The UV spectrophotometric determinations were performed at 292 nm. Good linearity was obtained between 2.5 and 20.0 microg/mL. A prospective validation showed that the method is linear (r = 0.9999) and precise, with RSD values of 0.3% for product A and 0.4% for product B. The intra- and interday precision values were < 2% for all samples analyzed. Comparison of UV spectrophotometry and LC by analysis of variance and Student's t-test showed no significant difference between methodologies. Moreover, the accuracy and precision obtained with the UV method correlated well with the values obtained with the LC method, and this correlation suggests that UV spectrophotometric analysis can be an inexpensive, reliable, and less time-consuming alternative to chromatographic analysis. The results demonstrated the validity of the proposed method as a simple and useful alternative for the determination of ceftiofur in routine QC analyses.
建立了一种紫外分光光度法用于测定头孢噻呋钠原料药及注射用无菌粉末中的头孢噻呋钠。该方法验证取得了良好结果，包括对范围、线性、日内和日间精密度、准确度、回收率、专属性、稳健性、定量限和检测限的评估。紫外分光光度法测定在292nm波长处进行。在2.5至20.0μg/mL范围内获得了良好的线性关系。前瞻性验证表明该方法呈线性（r = 0.9999）且精密度良好，产品A的相对标准偏差（RSD）值为0.3%，产品B为0.4%。所有分析样品的日内和日间精密度值均<2%。通过方差分析和学生t检验对紫外分光光度法和液相色谱法进行比较，结果表明两种方法之间无显著差异。此外，紫外法获得的准确度和精密度与液相色谱法获得的值具有良好的相关性，这种相关性表明紫外分光光度分析可以作为一种比色谱分析更便宜、可靠且耗时更少的替代方法。结果证明了所提出的方法作为常规质量控制分析中测定头孢噻呋的一种简单且有用的替代方法的有效性。
