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In this study (open access) researchers developed and piloted a single in-line sensor to classify yoghurt as either sheep, goat or milk origin and simultaneously check viscosity and pH Quality Attribute Specifications.  Their goal is a rapid in-line sensor that incorporates automated decision making, for routine use in the dairy industry.

Their reference dataset was sourced directly from two reputable Spanish companies and included both pasteurised and UHT yoghurts.

They found that the animal origin of milk could be predicted by building models based on the spectral data between 400 and 600 nm whilst viscosity and pH could be predicted by building models based on the spectral data between 800 and 1800 nm. To identify the animal origin of milk, they used Partial Least Squares-Discriminant Analysis (PLS-DA), achieving 100 % accuracy (95 % confidence interval). The model used to predict pH and viscosity was built with Partial Least Squares Regression (PLSR). The predictive power was generally very good (MSE=0.04–0.06; R²=0.94–0.96; MAE=0.16–0.17).

They conclude that their study demonstrates that the proposed spectroscopic method offers a more efficient approach for the simultaneous prediction of pH, viscosity, and milk origin in yogurt compared to existing methods, that require separate and slower analyses. Further work still needs to be carried out to optimize the model and achieve real-time monitoring that enables automated decision-making.

[picture – from the publication]

In this study (purchase required) the authors propose and develop a strategy for a field-based screening test for crude honey adulteration (adulteration with inverted sugars) using Near InfraRed Spectroscopy (NIR) hand-held scanners.  They developed a single class classification model that was sufficient to either give an “unadulterated” verdict or to refer the sample for confirmatory (IRMS) analysis.

The authors developed their SIMCA model using “genuine” adulterated honeys that had been previously seized in a Brazilian police operation that had cracked down on industrial-scale addition of invert sugar to honeys over a three year period, along with unadulterated honeys collected by police during the same operation.  The traditional SIMCA was improved by optimizing the class boundaries based on receiver operating characteristic (ROC) curves and the estimate of an uncertainty region, thus optimising the model for a screening application.

Photo by Roberta Sorge on Unsplash

Cocoa is high on many companies’ current risk radar for authenticity threats, due to recent supply pressures and price increases. Carob has legitimate uses as a cocoa replacement, and carob flour has been cited as a potential cocoa adulterant.

 A number of chemometric classification methods to differentiate cocoa from carob recently have been proposed, including one featured in our blogs in January based on DART-MS.  In a more recent publication (purchase required) the authors use the alternate method of near and mid-infrared spectroscopy before applying various chemometric approaches.

Spectral data were collected using four different infrared spectrometers: a benchtop FT-NIR system, two portable NIR instruments, and a benchtop FT-MIR-ATR. Reference samples included pure cocoa, pure carob, and their mixtures with carob concentrations ranging from 0 % to 60 %. Both classification and regression models were developed to detect and quantify the presence of carobs in cocoa powder. Classification models, including Random Forest (RF), Support Vector Machine (SVM), Multi-Layer Perceptron (MLP), k-Nearest Neighbors (kNN), Linear Discriminant Analysis (LDA), and Soft Voting Classifiers, demonstrated superior performance for discriminating between cocoa powder, carob powder, and cocoa-carob mixtures, particularly using the benchtop FT-NIR. Similarly, regression models - RF, SVM, MLP, kNN, Partial Least Squares Regression, and Voting Regressor- exhibited robust predictive capabilities, particularly, FT-MIR and portable NIR.

Overall, these findings highlight and prove the potential of NIR and MIR spectroscopy as rapid, robust, and non-destructive tools for screening and quality control in food authentication.

Photo by lindsay Cotter on Unsplash

A2 cows’ milk is from selective breeds that produce a higher ratio of the A2/A1 form of β-casein in the milk.  It is sold mostly in Australia, New Zealand, China, and the United States and commands a price premium over conventional milk.  Authenticity testing has been difficult, typically requiring genetic techniques.

In this study (purchase required) the researchers piloted portable NIR to differntiate A2 milk versusnon-A2 milk and their mixtures using a portable NIR spectrometer.  They built a 1-class classification model.  63 samples of whole A2 milk were selected (authentic set), and 40 samples (fraudulent set) composed of non-A2 milk and mixtures in 3 different proportions (10, 25, and 50% v/v) of non-A2 milk in A2 milk. The abstract gives no further details of the reference samples in terms of production systems or seasonality.  For spectra collection, a MicroNIR was used.

Full data were pre-processed using different methods, but they found the most effective approach was the combination of the first derivative with Savitzky-Golay smoothing and Standard Normal Variate (SNV). A Data-driven Soft Independent Modeling of Class Analogy (DD-SIMCA) was applied. Using the Kennard-Stone algorithm, the authentic samples were split into two sets (45 for calibration and 20 for external validation). The non-A2 and fraudulent samples were added to the external validation set, and the model’s performance was evaluated using the metrics of sensitivity, specificity, accuracy, and precision.

They report that the DD-SIMCA model, utilizing 2 PCs, showed 100% results in all metrics, indicating no errors in the recognition of authentic samples.

They conclude that the model is suitable for use with portable equipment. Additionally, this fast and non-invasive technique can be optimized for applications in industrial management, food control, and A2 product authentication.

In this paper (open access) the authors trained a Machine Learning model to differentiate between Top, Bottom and Spontaneous fermented bottled beers.  Data were collected using a non-invasive hand held NIR scanner pointed directly through the unopened bottle using a customised foam attachment.  The model was trained on 25 samples of major brands purchased online, rather than reference samples of verified traceability, but the training samples covered a wide range of beer types from stouts to light ales, and a wide range of bottle types and colours.

The authors report good classification based on fermentation method.  They consider that evidence of a wrong fermentation method could be one quick and easy check that could flag counterfeits.  They also correlated the NIR data with sensory panel assessments and SPME-GC-MS data and concluded that non-invasive NIR has the potential to classify beers based on their aroma profiles.

Image from the paper

In this paper (open access) two optical spectroscopic techniques,  Laser-Induced Breakdown Spectroscopy (LIBS) and UV-Vis-NIR absorption spectroscopy, are assessed for EVOO adulteration detection, using the same reference database of olive oil samples. In total, 184 samples were studied, including 40 EVOOs and 144 binary mixtures with pomace, soybean, corn, and sunflower oils, at various concentrations (ranging from 10 to 90% w/w). The reference class of “pure” EVOOs were limited to oils from a specific geographic region (either Crete, Lesvos, Kalamata or Achaia, with a different model built for each case).

The emission data from LIBS, related to the elemental composition of the samples, and the UV-Vis-NIR absorption spectra, related to the organic ingredients content, were analyzed, both separately and combined (i.e., fused), by Linear Discriminant Analysis (LDA), Support Vector Machines (SVMs), and Logistic Regression (LR). In all cases, very highly predictive accuracies were achieved, attaining, in some cases, 100%.

The authors conclude that both techniques have the potential for efficient and accurate olive oil verification test protocols, with the LIBS technique being better suited as it can operate much faster.