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Digital Filtering and Model Updating Methods for Improving the Robustness of Near-Infrared Multivariate Calibrations

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Abstract:

Fourier transform near-infrared (NIR) transmission spectra are used for quantitative analysis of glucose for 17 sets of prediction data sampled as much as six months outside the timeframe of the corresponding calibration data. Aqueous samples containing physiological levels of glucose in a matrix of bovine serum albumin and triacetin are used to simulate clinical samples such as blood plasma. Background spectra of a single analyte-free matrix sample acquired during the instrumental warm-up period on the prediction day are used for calibration updating and for determining the optimal frequency response of a preprocessing infinite impulse response time-domain digital filter. By tuning the filter and the calibration model to the specific instrumental response associated with the prediction day, the calibration model is given enhanced ability to operate over time. This methodology is demonstrated in conjunction with partial least squares calibration models built with a spectral range of 4700–4300 cm−1. By using a subset of the background spectra to evaluate the prediction performance of the updated model, projections can be made regarding the success of subsequent glucose predictions. If a threshold standard error of prediction (SEP) of 1.5 mM is used to establish successful model performance with the glucose samples, the corresponding threshold for the SEP of the background spectra is found to be 1.3 mM. For calibration updating in conjunction with digital filtering, SEP values of all 17 prediction sets collected over 3–178 days displaced from the calibration data are below 1.5 mM. In addition, the diagnostic based on the background spectra correctly assesses the prediction performance in 16 of the 17 cases.

Keywords: CALIBRATION; DIGITAL FILTERING; NEAR-INFRARED SPECTROSCOPY; NIR SPECTROSCOPY

Document Type: Research Article

DOI: http://dx.doi.org/10.1366/000370209787392076

Affiliations: 1: Optical Science and Technology Center and Department of Chemistry, University of Iowa, Iowa City, Iowa 52242; Cognis Corp., 4900 Este Ave., Cincinnati, OH 45232 2: Optical Science and Technology Center and Department of Chemistry, University of Iowa, Iowa City, Iowa 52242

Publication date: February 1, 2009

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