Abstract

Mid-infrared spectroscopy has been developed as a reliable and rapid tool for routine analysis of fat, protein, lactose and other components in liquid milk. However, variations within and between FTIR instruments, even within the same milk testing laboratory, present a challenge to the accuracy of measurement of particularly minor components in the milk, such as individual fatty acids or proteins. In this study we have used Analysis of variance–Simultaneous Component Analysis (ASCA), to monitor the spectral variation between and within each of four different FOSS FTIR spectrometers over each week in an independent milk testing laboratory over 4 years, between August 2017 and March 2021 (223 weeks). On everyday of each week, spectra of the same pilot milk sample were recorded approximately every hour on each of the four instruments. Overall, variations between instruments had the largest effect on spectral variation over each week, making a significant contribution every week. Within each instrument, day-to-day variations over the week were also significant for all but two of the weeks measured, however it contributed less to the variance overall. At certain times other factors not explained by weekday variation or inter-instrument variation dominated the variance in the spectra. Examination of the scores and loadings of the weekly ASCA analysis allowed identification of changes in the spectral regions affected by drifts in each instrument over time. This was found to particularly affect some of the fatty acid predictions.

Highlights

  • The goal of quantitative mid-infrared (MIR) analysis is to reproduce the analytical results achieved with accepted standard reference methods

  • The total sum of squares (TSSQ) for each of the 177 weeks, obtained from the ANOVA calculation of the Analysis of variance–Simultaneous Component Analysis (ASCA) algorithm are plotted in Figure 1 over the time period December 2016 to March 2021

  • We have described the novel use of ASCA on the spectra of pilot test milk samples over time as a new approach for routine monitoring of instrument performance in a milk testing laboratory

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Summary

Introduction

The goal of quantitative mid-infrared (MIR) analysis is to reproduce the analytical results achieved with accepted standard reference methods. The quantitative analysis of milk components from MIR spectra is based on the direct proportionality between the intensities of the absorbance bands for each component and their concentrations and the path length through the sample. The accuracy of this measurement requires routine calibration of the spectrometers with pre-analysed milk (with chemical reference tests). In a report on performance of the older generation of milk analysers, it was found that the main problems affecting calibration and accuracy of predictions were inaccurate reference tests, air incorporation, homogenizer inefficiency, mechanical wear, sample cell and filter system, electronics and mechanical maintenance and operator errors (Young, 1978). Manufacturers of other MIR spectrometers used for routine milk analysis incorporate one or more methods to reduce variations within and between instruments

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