Development and validation of a near infrared method for the analytical control of a pharmaceutical preparation in three steps of the manufacturing process

被引:30
作者
Blanco, M [1 ]
Coello, J [1 ]
Iturriaga, H [1 ]
Maspoch, S [1 ]
Pou, N [1 ]
机构
[1] Univ Autonoma Barcelona, Fac Ciencies, Dept Quim, Unitat Quim Analit, Bellaterra 08193, Spain
来源
FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY | 2000年 / 368卷 / 05期
关键词
D O I
10.1007/s002160000506
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A near infrared diffuse reflectance spectroscopy (NIRS) procedure for the quantitative control analysis of the active compound (otilonium bromide) in a pharmaceutical preparation in three steps of the production process (blended product, cores and coated tablets) and a methodology for its validation are proposed. The analytical procedure is composed by two consecutive steps. First, the sample is identified by comparing its spectrum with a second derivative spectral library. If the sample is positively identified, the active compound is quantified by using a previously established partial least squares (PLS) calibration model. The procedure was validated by studying repeatability, intermediate precision, accuracy and linearity. To this end, an adaptation of ICH (International Conference on Harmonisation) validation methodology to an NIR multivariate calibration procedure is proposed. The relative standard error of prediction (RSEP) was less than or equal to 1% and the suitability of the procedure for control analysis was confirmed by the results obtained analysing new production samples produced over a three-month period.
引用
收藏
页码:534 / 539
页数:6
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