Near-infrared (NIR) spectroscopy, in combination with chemometrics, enable
the analysis of raw materials without time-consuming sample preparation met
hods. The aim of our work was to estimate critical parameters in the analyt
ical specification of oxytetracycline, and consequently the development of
a method for quantification and qualification of these parameters by MR spe
ctroscopy. A Karl Fischer (K.F.) titration to determine the water content,
a colorimetric assay method, and Fourier transform-infrared (FT-IR) spectro
scopy to identify the oxytetracycline base, were used as reference methods,
respectively. Multivariate calibration was performed on MR spectral data u
sing principal component analysis (PCA), partial least-squares (PLS 1) and
principal component regression (PCR) chemometric methods. Multivariate cali
bration models for MR spectroscopy have been developed. Using PCA and the S
oft Independent Modelling of Class Analogy (SIMCA) approach, we established
the cluster model for the determination of sample identity. PLS 1 and PCR
regression methods were applied to develop the calibration models for the d
etermination of water content and the assay of the oxytetracycline base. Co
mparing the PLS and PCR regression methods we found out that the PLS is bet
ter established by MR, especially as the spectroscopic data (NIR spectral a
re highly collinear and there are many wavelengths due to non-selective wav
elengths. The calibration models for MR spectroscopy are convenient alterna
tives to the colorimetric method and to the K.F. method, as well as to FT-I
R spectroscopy, in the routine control of incoming material. (C) 2000 Elsev
ier Science B.V. All rights reserved.