Although Hom Mali rice is considered the highest quality rice in Thailand, it is susceptible to adulteration and substitution. There is a need for rapid, low-cost and efficient analytical techniques for monitoring the authenticity and geographical origin of Thai Hom Mali rice. In this study, two infrared spectroscopy techniques, Fourier-transform infrared spectroscopy with attenuated total reflection (FTIR-ATR) and near-infrared (NIR) spectroscopy, were applied and compared for the differentiation of Thai Hom Mali rice from two geographical regions over two production years. The Orthogonal Projections to Latent Structures Discriminant Analysis (OPLS-DA) model, built using spectral data from the benchtop FTIR-ATR, achieved 96.97% and 100% correct classification of the test dataset for each of the production years, respectively. The OPLS-DA model, built using spectral data from the portable handheld NIR, achieved 84.85% and 86.96% correct classification of the test dataset for each of the production years, respectively. Direct NIR analysis of the polished rice grains (i.e., no sample preparation) was determined as reliable for analysis of ground rice samples. FTIR-ATR and NIR spectroscopic analysis both have significant potential as screening tools for the rapid detection of fraud issues related to the geographical origin of Thai Hom Mali rice.
17 January 2022 in Rapid Communications in Mass Spectrometry
Black pepper is the most widely used spice crop globally and has significant economic value, making it a target for economically motivated adulteration. A wide range of organic and inorganic bulking materials has been used as adulterants in black pepper. Development of rapid non-targeted screening methods for use at different stages of the black pepper supply chain is extremely important for the identification and prevention of evolving fraudulent practices. This study has assessed the potential of benchtop Fourier Transform infrared with attenuated total reflectance (FTIR-ATR), benchtop Fourier Transform near-infrared (FT-NIR), and two handheld NIR spectrometers, coupled with chemometrics, for the discrimination of black pepper (Piper nigrum), pepper from other species and genera (non-Piper nigrum) and a broad range (n = 27) of endogenous and exogenous adulterants. Spiked samples were prepared to imitate pepper adulteration with seven different adulterants at five levels of adulteration (5%, 25%, 50%, 75%, 95% w/w). Orthogonal partial least squares discriminant analysis (OPLS-DA) achieved 100% total prediction accuracy for both FTIR-ATR and FT-NIR in differentiating authentic Piper nigrum and adulterant samples. The handheld microNIR 1700ES resulted in a 91.30% correct classification rate, while the SCiO model achieved 86.96% prediction accuracy. Detection of black pepper adulteration with multiple adulterants was performed using data-driven soft independent modelling of class analogy (DD-SIMCA). The highest performance of the DD-SIMCA model was achieved by FTIR-ATR (100% sensitivity and 100% specificity) followed by FT-NIR (98% sensitivity and 99% specificity). The handheld microNIR 1700ES resulted in 95% sensitivity and 90% specificity. This study demonstrated that FTIR-ATR and FT-NIR, coupled with DD-SIMCA, can effectively detect black pepper adulteration with multiple endogenous and exogenous adulterants. The handheld NIR (microNIR1700ES) clearly demonstrated the potential for rapid and effective verification of Piper nigrum authenticity outside the laboratory.