Development and validation of a method for the polymorphic analysis of pharmaceutical preparations using near infrared spectroscopy

A new method for the characterization and determination of crystalline miokamycin in a pharmaceutical preparation using near infrared spectroscopy is proposed. The procedure involves the identification against a spectral library of samples with contents above the legal limit (viz. 5% of the crystalline form in amorphous miokamycin) using the Mahalanobis distance as the discriminating criterion, and the determination of the total and crystalline contents using partial least squares models that provide errors <1%. The proposed method was validated following the ICH guidelines. Its simplicity and expeditiousness make it highly suitable for quality control analyses of solid dosage forms. (C) 2003 Wiley-Liss, Inc. and the American Pharmaceutical Association J Pharm Sci 92:823-830, 2003.