The detection of raw material defects, e.g., due to incorrect or excessively long storage, is an important issue in incoming goods inspections in the food industry. Fast and easy-to-use analytical methods for evaluating the usability of raw materials are particularly important. In this study, the applicability of Fourier transform near-infrared (FT-NIR) spectroscopy and spatially offset Raman spectroscopy (SORS) for the detection of raw material defects was evaluated. For this purpose, six hazelnut batches stored at different temperatures, humidity levels, and storage times were used as examples in this pilot study. Classification models of samples before and after the different physical treatments show that the resulting changes can be detected by FT-NIR spectroscopy and SORS at elevated temperature and humidity. When one of the storage parameters is increased, FT-NIR spectroscopy is also useful for detecting differences between sample groups. In contrast, SORS cannot distinguish between pre- and post-stored samples when only one of the storage parameters is increased, making SORS unsuitable for incoming inspection of nuts. FT-NIR spectroscopy analysis is also a fast application, because freeze-drying of the sample material prior to analysis is not required as the results before and after freeze-drying are comparable. Combining the FT-NIR spectroscopy and SORS data in a low-level data fusion improved the classification models for samples stored at low storage temperatures, suggesting that the two methods provide complementary information. In summary, analyzing nuts with FT-NIR spectroscopy and SORS, as shown for hazelnuts, has the potential to identify abnormal samples during incoming goods inspections.

Near-infrared (NIR) spectroscopy is a proven tool for the determination of food authenticity, mainly because of good classification results and the possibility of industrial use due to its easy and fast application. Since water shows broad absorption bands, the water content of a sample should be as low as possible. Freeze-drying is a commonly used preparatory step for this to reduce the water content in the sample. However, freeze-drying, also known as lyophilization, is very time-consuming impeding the widespread usage of NIR analysis as a rapid method for incoming goods inspections. We used a sample set of 72 almond samples from six economically relevant almond-producing countries to investigate the question of how important lyophilization is to obtain a well-performing classification model. For this approach, the samples were ground and lyophilized for 3 h, 24 h, and 48 h and compared to non-freeze-dried samples. Karl-Fischer titration of non-lyophilized samples showed that water contents ranged from 3.0 to 10.5% and remained constant at 0.36 ± 0.13% after a freeze-drying period of 24 h. The non-freeze-dried samples showed a classification accuracy of 93.9 ± 6.4%, which was in the same range as the samples which were freeze-dried for 3 h (94.2 ± 7.8%), 24 h (92.5 ± 8.7%), and 48 h (95.0 ± 9.0%). Feature selection was performed using the Boruta algorithm, which showed that signals from lipids and proteins are relevant for the origin determination. The presented study showed that samples with low water content, especially nuts, can be analyzed without the time-consuming preparation step of freeze-drying to obtain robust and fast results, which are especially required for incoming goods inspection.

The untargeted metabolomics analysis of biological samples with nuclear magnetic resonance (NMR) provides highly complex data containing various signals from different molecules. To use these data for classification, e.g., in the context of food authentication, machine learning methods are used. These methods are usually applied as a black box, which means that no information about the complex relationships between the variables and the outcome is obtained. In this study, we show that the random forest-based approach surrogate minimal depth (SMD) can be applied for a comprehensive analysis of class-specific differences by selecting relevant variables and analyzing their mutual impact on the classification model of different truffle species. SMD allows the assignment of variables from the same metabolites as well as the detection of interactions between different metabolites that can be attributed to known biological relationships.

Accelerated storage is routinely used with pharmaceuticals to predict stability and degradation patterns over time. The aim of this is to assess the shelf life and quality under harsher conditions, providing crucial insights into their long-term stability and potential storage issues. This study explores the potential of transferring this approach to food matrices for shelf-life estimation. Therefore, hazelnuts were stored under accelerated short-term and realistic long-term conditions. Subsequently, they were analyzed with high resolution mass spectrometry, focusing on the lipid profile. LC-MS analysis has shown that many unique processes take place under accelerated conditions that do not occur or occur much more slowly under realistic conditions. This mainly involved the degradation of membrane lipids such as phospholipids, ceramides, and digalactosyldiacylglycerides, while oxidation processes occurred at different rates in both conditions. It can be concluded that a food matrix is far too complex and heterogeneous compared to pharmaceuticals, so that many more processes take place during accelerated storage, which is why the results cannot be used to predict molecular changes in hazelnuts stored under realistic conditions.