Moisture determination in hygroscopic drug substances by near infrared spectroscopy

The moisture level in a hygroscopic drug substance was successfully determined by near infrared spectroscopy using coulometric Karl Fischer titration as the reference method. The importance of sample handling and proper application of the reference technique are stressed for this difficult sample ty...

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Bibliographic Details
Published in:Journal of pharmaceutical and biomedical analysis 1998-06, Vol.17 (2), p.219-225
Main Authors: Zhou, Xiangji, Hines, Patricia, Borer, Matthew W
Format: Article
Language:English
Subjects:
Analysis
Biological and medical sciences
Calibration
Drug substance
General pharmacology
Karl Fischer
Medical sciences
Moisture
Near infrared
NIR
NIRS
Pharmaceutical Preparations - analysis
Pharmacology. Drug treatments
PLS
Regression Analysis
Spectrophotometry, Infrared - methods
Titrimetry
Water - analysis
Wettability
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Summary:The moisture level in a hygroscopic drug substance was successfully determined by near infrared spectroscopy using coulometric Karl Fischer titration as the reference method. The importance of sample handling and proper application of the reference technique are stressed for this difficult sample type. Samples were prepared with moisture levels from 0.5 to 11.4% (w/w) and reflectance spectra were collected over the spectral range 1100–2500 nm. Calibration models were built using partial least squares (PLS) regression analysis. Optimum models were found by choosing proper spectral ranges and number of PLS factors. The best calibration models were built using first derivative spectra, a spectral range of 1850–1936 nm and 5 PLS factors. The corresponding standard error of prediction was 0.11% (w/w) water.
ISSN:0731-7085
1873-264X
DOI:10.1016/S0731-7085(97)00182-9