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Development and validation of an infrared spectroscopy‐based method for the analysis of moisture content in 5‐fluorouracil
Author(s) -
Singh Parul,
Jangir Deepak K.,
Mehrotra Ranjana,
Bakhshi A. K.
Publication year - 2009
Publication title -
drug testing and analysis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.065
H-Index - 54
eISSN - 1942-7611
pISSN - 1942-7603
DOI - 10.1002/dta.47
Subject(s) - moisture , water content , infrared spectroscopy , attenuated total reflection , calibration , fourier transform infrared spectroscopy , partial least squares regression , analytical chemistry (journal) , spectroscopy , chemistry , infrared , titration , materials science , chromatography , mathematics , optics , statistics , geology , physics , organic chemistry , geotechnical engineering , quantum mechanics
The determination of moisture content in pharmaceuticals is very important as moisture is mainly responsible for the degradation of drugs. Degraded drugs have reduced efficacy and could be hazardous. The objective of the present work is to replace the Karl Fischer (KF) titration method used for moisture analysis with a method that is rapid, involves no toxic materials and is more effective. Diffuse reflectance infrared (IR) spectroscopy, which is explored as a potential alternative to various approaches, is investigated for moisture analysis in 5‐fluorouracil, an anticancer drug. A total of 150 samples with varying moisture content were prepared in laboratory by exposing the drug at different relative humidities, for different time intervals. Infrared spectra of these samples were collected with a Fourier transform infrared (FTIR) spectrophotometer using a diffuse reflectance accessory. Reference moisture values were obtained using the Karl Fischer titration method. A number of calibration models were developed using the partial least squares (PLS) regression method. A good correlation was obtained between predicted IR values and reference values in the calibration and validation set. The derived calibration curve was used to predict moisture content in unknown samples. The results show that IR spectroscopy can be used successfully for the determination of moisture content in the pharmaceutical industry. Copyright © 2009 John Wiley & Sons, Ltd.