A near-infrared spectroscopy method to determine aminoglycosides in pharmaceutical formulations

• Type: Article in International Scientific Journal
• Date: 2011

Authors

Mafalda Cruz Sarraguça (Author) FFUP; Sandra Oliveira Soares (Author) FFUP; João Almeida Lopes (Author) FFUP

Journal

Title: Vibrational Spectroscopy

Vol. 56 No. 2

Pages: 184-192

ISSN: 0924-2031

Publisher: Elsevier

Indexing

Scopus

Scientific classification

FOS: Medical and Health sciences > Health sciences

CORDIS: Health sciences > Pharmacological sciences

Other information

Resumo (PT): The analytical determination of aminoglycosides in pharmaceutical formulations is very difficult due to the lack of chromophores or fluorophores. Several analytical methods have been developed along the years mainly based on derivatization reactions. The European Pharmacopeia (EP) and the United States Pharmacopeia (USP) describe a microbiological assay to the quantification of aminoglycosides. Near infrared spectroscopy (NIRS) can be used alternatively to analyse aminoglycosides without the need of derivatization reactions or other type of sample processing. A new NIRS based method was developed for the analysis of the aminoglycoside antibiotic neomycin. The method was developed with samples based on a commercial formulation containing neomycin sulphate and three excipients: lactose, talc and magnesium stearate. Synthetic and doped samples were manufactured for this purpose. Three lots of a commercial solid formulation were also used to assess the validity of the method to quantify neomycin sulphate in the industrial pharmaceutical product. The method proposes measurements in reflectance mode using a Fourier-transform near infrared (FT-NIR) spectrometer. Partial least squares regression was the multivariate method adopted to calibrate the NIR spectra with the neomycin sulphate mass fraction. The concentration of neomycin sulphate present in the commercial samples was confirmed by HPLC with pre-column derivatization with phenylisocyanate. Results show that neomycin sulphate was determined successfully in the commercial samples using the method calibrated with the doped samples (mass fraction error of 6.6%). Moreover, the synthetic samples were found to be unqualified to develop the method, producing a biased calibration. <br> <br> Keywords: Aminoglycosides; Neomycin sulphate; Near-infrared spectroscopy; Partial least squares regression; Pharmaceutical industry <br> <a target="_blank" href="http://www.sciencedirect.com/science/article/pii/S0924203111000257 "> Texto integral </a> <br> <br>

Abstract (EN): The analytical determination of aminoglycosides in pharmaceutical formulations is very difficult due to the lack of chromophores or fluorophores. Several analytical methods have been developed along the years mainly based on derivatization reactions. The European Pharmacopeia (EP) and the United States Pharmacopeia (USP) describe a microbiological assay to the quantification of aminoglycosides. Near infrared spectroscopy (NIRS) can be used alternatively to analyse aminoglycosides without the need of derivatization reactions or other type of sample processing. A new NIRS based method was developed for the analysis of the aminoglycoside antibiotic neomycin. The method was developed with samples based on a commercial formulation containing neomycin sulphate and three excipients: lactose, talc and magnesium stearate. Synthetic and doped samples were manufactured for this purpose. Three lots of a commercial solid formulation were also used to assess the validity of the method to quantify neomycin sulphate in the industrial pharmaceutical product. The method proposes measurements in reflectance mode using a Fourier-transform near infrared (FT-NIR) spectrometer. Partial least squares regression was the multivariate method adopted to calibrate the NIR spectra with the neomycin sulphate mass fraction. The concentration of neomycin sulphate present in the commercial samples was confirmed by HPLC with pre-column derivatization with phenylisocyanate. Results show that neomycin sulphate was determined successfully in the commercial samples using the method calibrated with the doped samples (mass fraction error of 6.6%). Moreover, the synthetic samples were found to be unqualified to develop the method, producing a biased calibration. <br> <br> Keywords: Aminoglycosides; Neomycin sulphate; Near-infrared spectroscopy; Partial least squares regression; Pharmaceutical industry <br> <a target="_blank" href="http://www.sciencedirect.com/science/article/pii/S0924203111000257 "> Full text</a> <br> <br>

Language: English

Type (Professor's evaluation): Scientific