title: A procedure for calibration transfer between near-infrared instruments--a worked example using a transmittance single tablet assay for piroxicam in intact tablets.
abstract: A procedure was developed for different modes of calibration transfer in near-infrared (NIR) spectroscopy, which included a method for the selection of a subset of samples appropriate for transfer. As a worked example, these guidelines were applied to the transfer of a multivariate calibration model, representing a validated NIR single tablet assay for the active within an intact pharmaceutical product, between three equivalent dispersive NIR transmission instruments. Transfer was first evaluated between two instruments, representing the situation where both were available during calibration development. A spectral correction method alone, applied to the transfer instrument, was not sufficient to facilitate transfer, with further optimisation of the calibration model using a novel wavelength selection algorithm necessary to remove regions of the spectral range that resulted in skewed predictions on the second instrument. Through this approach, a single calibration model was found to be equally accurate and precise on the two instruments. A procedure, using the Kennard-Stone algorithm, is described for determining a reduced number of samples as a transfer set using only the spectral information from the original instrument. The purpose of the subset was to permit transfer to a new instrument where that instrument was not available until after calibration development or where it was undesirable to re-measure the full sample set (i.e. due to excessive reference chemistry). Utilising the transfer set, transfer to a third instrument was evaluated. The calibration model, optimised between the first two instruments, was not directly applicable for the third instrument, with further wavelength selection required to remove a small region of spectral data. On completion, using a full statistical evaluation, a single calibration model was found to be equally accurate and precise on all three instruments.
authors.affiliation: Centre for Pharmaceutical Analysis, The School of Pharmacy, University of London, 29/39 Brunswick Square, London, UKWC1N 1AX. mark.smith@ulsop.ac.uk
authors.forename: Mark R
authors.initials: MR
authors.lastname: Smith
authors.forename: Roger D
authors.initials: RD
authors.lastname: Jee
authors.forename: Anthony C
authors.initials: AC
authors.lastname: Moffat
authors.forename: David R
authors.initials: DR
authors.lastname: Rees
authors.forename: Neville W
authors.initials: NW
authors.lastname: Broad
mesh_terms: D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis*; D002138:Calibration; D010894:Piroxicam / Q000032:analysis*; D019265:Spectroscopy, Near-Infrared / Q000295:instrumentation*
chemical_list: D000894:Anti-Inflammatory Agents, Non-Steroidal; D010894:Piroxicam