Revealing the Effect of Heat Treatment on the Spectral Pattern of Unifloral Honeys Using Aquaphotomics.

In this study we aimed to investigate the effect of heat treatment on the spectral pattern of honey using near infrared spectroscopy (NIRS). For the research, sunflower, bastard indigo, and acacia honeys were collected from entrusted beekeepers. The honeys were not subject to any treatment before. Samples were treated at 40 °C, 60 °C, 80 °C, and 100 °C for 60, 120, 180, and 240 min. This resulted in 17 levels, including the untreated control samples. The 5-hydroxymethylfurfural (HMF) content of the honeys was determined using the Winkler method. NIRS spectra were recorded using a handheld instrument. Data analysis was performed using ANOVA for the HMF content and multivariate analysis for the NIRS data. For the latter, PCA, PCA-LDA, and PLSR models were built (using the 1300-1600 nm spectral range) and the wavelengths presenting the greatest change induced by the perturbations of temperature and time intervals were collected systematically, based on the difference spectra and the weights of the models. The most contributing wavelengths were used to visualize the spectral pattern changes on the aquagrams in the specific water matrix coordinates. Our results showed that the heat treatment highly contributed to the formation of free or less bonded water, however, the changes in the spectral pattern highly depended on the crystallization phase and the honey type.

NIRS and Aquaphotomics Trace Robusta-to-Arabica Ratio in Liquid Coffee Blends.

Coffee is both a vastly consumed beverage and a chemically complex matrix. For a long time, an arduous chemical analysis was necessary to resolve coffee authentication issues. Despite their demonstrated efficacy, such techniques tend to rely on reference methods or resort to elaborate extraction steps. Near infrared spectroscopy (NIRS) and the aquaphotomics approach, on the other hand, reportedly offer a rapid, reliable, and holistic compositional overview of varying analytes but with little focus on low concentration mixtures of Robusta-to-Arabica coffee. Our study aimed for a comparative assessment of ground coffee adulteration using NIRS and liquid coffee adulteration using the aquaphotomics approach. The aim was to demonstrate the potential of monitoring ground and liquid coffee quality as they are commercially the most available coffee forms. Chemometrics spectra analysis proved capable of distinguishing between the studied samples and efficiently estimating the added Robusta concentrations. An accuracy of 100% was obtained for the varietal discrimination of pure Arabica and Robusta, both in ground and liquid form. Robusta-to-Arabica ratio was predicted with R2CV values of 0.99 and 0.9 in ground and liquid form respectively. Aquagrams results accentuated the peculiarities of the two coffee varieties and their respective blends by designating different water conformations depending on the coffee variety and assigning a particular water absorption spectral pattern (WASP) depending on the blending ratio. Marked spectral features attributed to high hydrogen bonded water characterized Arabica-rich coffee, while those with the higher Robusta content showed an abundance of free water structures. Collectively, the obtained results ascertain the adequacy of NIRS and aquaphotomics as promising alternative tools for the authentication of liquid coffee that can correlate the water-related fingerprint to the Robusta-to-Arabica ratio.

Determining Sonication Effect on E. coli in Liquid Egg, Egg Yolk and Albumen and Inspecting Structural Property Changes by Near-Infrared Spectra.

In this study, liquid egg, albumen, and egg yolk were artificially inoculated with E. coli. Ultrasound equipment (20/40 kHz, 180/300 W; 30/45/60 min) with a circulation cooling system was used to lower the colony forming units (CFU) of E. coli samples. Frequency, absorbed power, energy dose, and duration of sonication showed a significant impact on E. coli with 0.5 log CFU/mL in albumen, 0.7 log CFU/mL in yolk and 0.5 log CFU/mL decrease at 40 kHz and 6.9 W absorbed power level. Significant linear correlation (p < 0.001) was observed between the energy dose of sonication and the decrease of E. coli. The results showed that sonication can be a useful tool as a supplementary method to reduce the number of microorganism in egg products. With near-infrared (NIR) spectra analysis we were able to detect the structural changes of the egg samples, due to ultrasonic treatment. Principal component analysis (PCA) showed that sonication can alter C-H, C-N, -OH and N-H bonds in egg. The aquagrams showed that sonication can alter the properties of H2O structure in egg products. The observed data showed that the absorbance of free water (1412 nm), water molecules with one (1440 nm), two (1462 nm), three (1472 nm) and four (1488 nm) hydrogen bonds, water solvation shell (1452 nm) and strongly bonded water (1512 nm) of the egg samples have been changed during ultrasonic treatment.

Near-Infrared Spectroscopy and Aquaphotomics for Monitoring Mung Bean (Vigna radiata) Sprout Growth and Validation of Ascorbic Acid Content.

Mung bean is a leguminous crop with specific trait in its diet, namely in the form of anti-nutrient components. The sprouting process is commonly done for better nutritional acceptance of mung bean as it presents better nutritional benefits. Sprouted mung bean serves as a cheap source of protein and ascorbic acid, which are dependent on the sprouting process, hence the importance of following the biological process. In larger production scale, there has not been a definite standard for mung bean sprouting, raising the need for quick and effective mung bean sprout quality checks. In this regard, near-infrared spectroscopy (NIRS) has been recognized as a highly sensitive technique for quality control that seems suitable for this study. The aim of this paper was to describe quality parameters (water content, pH, conductivity, and ascorbic acid by titration) during sprouting using conventional analytical methods and advanced NIRS techniques as correlative methods for modelling sprouted mung beans' quality and ascorbic acid content. Mung beans were sprouted in 6 h intervals up to 120 h and analyzed using conventional methods and a NIR instrument. The results of the standard analytical methods were analyzed with univariate statistics (analysis of variance (ANOVA)), and the NIRS spectral data was assessed with the chemometrics approach (principal component analysis (PCA), discriminant analysis (DA), and partial least squares regression (PLSR)). Water content showed a monotonous increase during the 120 h of sprouting. The change in pH and conductivity did not describe a clear pattern during the sprouting, confirming the complexity of the biological process. Spectral data-based discriminant analysis was able to distinctly classify the bean sprouts with 100% prediction accuracy. A NIRS-based model for ascorbic acid determination was made using standard ascorbic acid to quantify the components in the bean extract. A rapid detection technique within sub-percent level was developed for mung bean ascorbic acid content with R2 above 0.90. The NIR-based prediction offers reliable estimation of mung bean sprout quality.

Origin Identification of Hungarian Honey Using Melissopalynology, Physicochemical Analysis, and Near Infrared Spectroscopy.

The objective of the study was to check the authenticity of Hungarian honey using physicochemical analysis, near infrared spectroscopy, and melissopalynology. In the study, 87 samples from different botanical origins such as acacia, bastard indigo, rape, sunflower, linden, honeydew, milkweed, and sweet chestnut were collected. The samples were analyzed by physicochemical methods (pH, electrical conductivity, and moisture), melissopalynology (300 pollen grains counted), and near infrared spectroscopy (NIRS:740-1700 nm). During the evaluation of the data PCA-LDA models were built for the classification of different botanical and geographical origins, using the methods separately, and in combination (low-level data fusion). PC number optimization and external validation were applied for all the models. Botanical origin classification models were >90% and >55% accurate in the case of the pollen and NIR methods. Improved results were obtained with the combination of the physicochemical, melissopalynology, and NIRS techniques, which provided >99% and >81% accuracy for botanical and geographical origin classification models, respectively. The combination of these methods could be a promising tool for origin identification of honey.

Sensory and Physicochemical Evaluation of Acacia and Linden Honey Adulterated with Sugar Syrup.

Honey is produced by honeybees and is used as a food and medical product. Adulteration of honey has been a problem for several years now because of the relatively high price of honey on the market according to its valuable composition. The aim of our study is to determine the physicochemical properties of authentic Hungarian linden and acacia honeys (pure samples or manipulated ones blended with sugar syrup) as well as commercially available blends of European Union (EU) non-European Union (non-EU) honeys. Authentic linden and acacia were blended with sugar syrup at 10%, 20% and 50% concentration levels, and physicochemical properties were determined according to the methods of the International Honey Commission. Our objectives also included testing of the performance of electronic sensory techniques (electronic tongue (ET) and electronic nose (EN)) in the detection of adulteration, and the results are compared to the sensory profile analysis. The results provide good average recognition and prediction abilities for the classification of adulterated and authentic honeys (>90% for ET and higher than >80 for EN). Misclassifications were found only in the case of honey with 10% added sugar syrup. The methods were also able to reveal adulteration of independently predicted samples.

Classification of Bee Pollen and Prediction of Sensory and Colorimetric Attributes-A Sensometric Fusion Approach by e-Nose, e-Tongue and NIR.

The chemical composition of bee pollens differs greatly and depends primarily on the botanical origin of the product. Therefore, it is a crucially important task to discriminate pollens of different plant species. In our work, we aim to determine the applicability of microscopic pollen analysis, spectral colour measurement, sensory, NIR spectroscopy, e-nose and e-tongue methods for the classification of bee pollen of five different botanical origins. Chemometric methods (PCA, LDA) were used to classify bee pollen loads by analysing the statistical pattern of the samples and to determine the independent and combined effects of the above-mentioned methods. The results of the microscopic analysis identified 100% of sunflower, red clover, rapeseed and two polyfloral pollens mainly containing lakeshore bulrush and spiny plumeless thistle. The colour profiles of the samples were different for the five different samples. E-nose and NIR provided 100% classification accuracy, while e-tongue > 94% classification accuracy for the botanical origin identification using LDA. Partial least square regression (PLS) results built to regress on the sensory and spectral colour attributes using the fused data of NIR spectroscopy, e-nose and e-tongue showed higher than 0.8 R2 during the validation except for one attribute, which was much higher compared to the independent models built for instruments.

Historical Evolution and Food Control Achievements of Near Infrared Spectroscopy, Electronic Nose, and Electronic Tongue-Critical Overview.

Amid today's stringent regulations and rising consumer awareness, failing to meet quality standards often results in health and financial compromises. In the lookout for solutions, the food industry has seen a surge in high-performing systems all along the production chain. By virtue of their wide-range designs, speed, and real-time data processing, the electronic tongue (E-tongue), electronic nose (E-nose), and near infrared (NIR) spectroscopy have been at the forefront of quality control technologies. The instruments have been used to fingerprint food properties and to control food production from farm-to-fork. Coupled with advanced chemometric tools, these high-throughput yet cost-effective tools have shifted the focus away from lengthy and laborious conventional methods. This special issue paper focuses on the historical overview of the instruments and their role in food quality measurements based on defined food matrices from the Codex General Standards. The instruments have been used to detect, classify, and predict adulteration of dairy products, sweeteners, beverages, fruits and vegetables, meat, and fish products. Multiple physico-chemical and sensory parameters of these foods have also been predicted with the instruments in combination with chemometrics. Their inherent potential for speedy, affordable, and reliable measurements makes them a perfect choice for food control. The high sensitivity of the instruments can sometimes be generally challenging due to the influence of environmental conditions, but mathematical correction techniques exist to combat these challenges.

Detection and Quantification of Tomato Paste Adulteration Using Conventional and Rapid Analytical Methods.

Tomato, and its concentrate are important food ingredients with outstanding gastronomic and industrial importance due to their unique organoleptic, dietary, and compositional properties. Various forms of food adulteration are often suspected in the different tomato-based products causing major economic and sometimes even health problems for the farmers, food industry and consumers. Near infrared (NIR) spectroscopy and electronic tongue (e-tongue) have been lauded as advanced, high sensitivity techniques for quality control. The aim of the present research was to detect and predict relatively low concentration of adulterants, such as paprika seed and corn starch (0.5, 1, 2, 5, 10%), sucrose and salt (0.5, 1, 2, 5%), in tomato paste using conventional (soluble solid content, consistency) and advanced analytical techniques (NIR spectroscopy, e-tongue). The results obtained with the conventional methods were analyzed with univariate statistics (ANOVA), while the data obtained with advanced analytical methods were analyzed with multivariate methods (Principal component analysis (PCA), linear discriminant analysis (LDA), partial least squares regression (PLSR). The conventional methods were only able to detect adulteration at higher concentrations (5-10%). For NIRS and e-tongue, good accuracies were obtained, even in identifying minimal adulterant concentrations (0.5%). Comparatively, NIR spectroscopy proved to be easier to implement and more accurate during our evaluations, when the adulterant contents were estimated with R2 above 0.96 and root mean square error (RMSE) below 1%.

Detecting Low Concentrations of Nitrogen-Based Adulterants in Whey Protein Powder Using Benchtop and Handheld NIR Spectrometers and the Feasibility of Scanning through Plastic Bag.

Nitrogen-rich adulterants in protein powders present sensitivity challenges to conventional combustion methods of protein determination which can be overcome by near Infrared spectroscopy (NIRS). NIRS is a rapid analytical method with high sensitivity and non-invasive advantages. This study developed robust models using benchtop and handheld spectrometers to predict low concentrations of urea, glycine, taurine, and melamine in whey protein powder (WPP). Effectiveness of scanning samples through optical glass and polyethylene bags was also tested for the handheld NIRS. WPP was adulterated up to six concentration levels from 0.5% to 3% w/w. The two spectrometers were used to obtain three datasets of 819 diffuse reflectance spectra each that were pretreated before linear discriminant analysis (LDA) and regression (PLSR). Pretreatment was effective and revealed important absorption bands that could be correlated with the chemical properties of the mixtures. Benchtop NIR spectrometer showed the best results in LDA and PLSR but handheld NIR spectrometers showed comparatively good results. There were high prediction accuracies and low errors attesting to the robustness of the developed PLSR models using independent test set validation. Both the plastic bag and optical glass gave good results with accuracies depending on the adulterant of interest and can be used for field applications.

Standard Analytical Methods, Sensory Evaluation, NIRS and Electronic Tongue for Sensing Taste Attributes of Different Melon Varieties.

Grafting by vegetables is a practice with many benefits, but also with some unknown influences on the chemical composition of the fruits. Our goal was to assess the effects of grafting and storage on the extracted juice of four orange-fleshed Cantaloupe type (Celestial, Donatello, Centro, Jannet) melons and two green-fleshed Galia types (Aikido, London), using sensory profile analysis and analytical instruments: An electronic tongue (E-tongue) and near-infrared spectroscopy (NIRS). Both instruments are known for rapid qualitative and quantitative food analysis. Linear discriminant analysis (LDA) was used to classify melons according to their varieties and storage conditions. Partial least square regression (PLSR) was used to predict sensory and standard analytical parameters. Celestial variety had the highest intensity for sensory attributes in Cantaloupe variety. Both green and orange-fleshed melons were discriminated and predicted in LDA with high accuracies (100%) using the E-tongue and NIRS. Galia and Cantaloupe inter-varietal classification with the E-tongue was 89.9% and 82.33%, respectively. NIRS inter-varietal classification was 100% with Celestial variety being the most discriminated as with the sensory results. Both instruments, classified different storage conditions of melons (grafted and self-rooted) with high accuracies. PLSR showed high accuracy for some standard analytical parameters, where significant differences were found comparing different varieties in ANOVA.

Factors Influencing the Long-Term Stability of Electronic Tongue and Application of Improved Drift Correction Methods.

Temperature, memory effect, and cross-contamination are suspected to contribute to drift in electronic tongue (e-tongue) sensors, therefore drift corrections are required. This paper aimed to assess the disturbing effects on the sensor signals during measurement with an Alpha Astree e-tongue and to develop drift correction techniques. Apple juice samples were measured at different temperatures. pH change of apple juice samples was measured to assess cross-contamination. Different sequential orders of model solutions and apple juice samples were applied to evaluate the memory effect. Model solutions corresponding to basic tastes and commercial apple juice samples were measured for six consecutive weeks to model drift of the sensor signals. Result showed that temperature, cross-contamination, and memory effect influenced the sensor signals. Three drift correction methods: additive drift correction based on all samples, additive drift correction based on reference samples, and multi sensor linear correction, were developed and compared to the component correction in literature through linear discriminant analysis (LDA). LDA analysis showed all the four methods were effective in reducing sensor drift in long-term measurements but the additive correction relative to the whole sample set gave the best results. The results could be explored for long-term measurements with the e-tongue.

Electronic Nose for Monitoring Odor Changes of Lactobacillus Species during Milk Fermentation and Rapid Selection of Probiotic Candidates.

Probiotic bacteria have been associated with a unique production of aroma compounds in fermented foods but rapid methods for discriminating between foods containing probiotic, moderately probiotic, or non-probiotic bacteria remain aloof. An electronic nose (e-nose) is a high-sensitivity instrument capable of non-invasive volatile measurements of foods. In our study, we applied the e-nose to differentiate probiotic, moderately probiotic, and non-probiotic Lactobacillus bacteria strains at different fermentation time points (0th, 4th, and 11th) of milk fermentation. The pH of the changing milk medium was monitored with their corresponding increase in microbial cell counts. An e-nose with two gas chromatographic columns was used to develop classification models for the different bacteria groups and time points and to monitor the formation of the aromatic compounds during the fermentation process. Results of the e-nose showed good classification accuracy of the different bacteria groups at the 0th (74.44% for column 1 and 82.78% for column 2), the 4th (89.44% for column 1 and 92.22% for column 2), and the 11th (81.67% for column 1 and 81.67% for column 2) hour of fermentation. The loading vectors of the classification models showed the importance of some specific aroma compounds formed during the fermentation. Results show that aroma monitoring of the fermentation process with the e-nose is a promising and reliable analytical method for the rapid classification of bacteria strains according to their probiotic activity and for the monitoring of aroma changes during the fermentation process.

Authentication of Tokaj Wine (Hungaricum) with the Electronic Tongue and Near Infrared Spectroscopy.

Tokaj wines (Hungaricum) are botrytized wines acknowledged for the unique organoleptic properties bestowed by botrytized grape berries during production. Excluding these berries during wine production or manipulating the sugar content of low-grade wines to imitate high-grade wines are some recent suspicious activities that threaten the wine quality. Advanced methods such as spectroscopy and sensor-based devices have been lauded for rapid, reliable, and cost-effective analysis, but there has been no report of their application to monitor grape must concentrate adulteration in botrytized wines. The study aimed to develop models to rapidly discriminate lower grade Tokaj wines, "Forditas I" and "Forditas II," that were artificially adulterated with grape must concentrate to match the sugar content of high-grade Tokaj wines using an electronic tongue (e-tongue) and two near infrared spectrometers (NIRS). Data were evaluated with the following chemometrics: principal component analysis (PCA), discriminant analysis (LDA), partial least square regression (PLSR), and aquaphotomics (a novel approach). There was a noticeable pattern of separation in PCA for all three instruments and 100% classification of adulterated and nonadulterated wines in LDA using the e-tongue. Aquagrams from the aquaphotomics approach showed important water absorption bands capable of being markers of Tokaj wine quality. PLSR models showed coefficient of determination (R2 CV) of 0.98 (e-tongue), 0.97 (benchtop NIRS), 0.87 (handheld NIRS), and low root mean squared errors of cross-validation. All three instruments could discriminate, classify, and predict grape must concentrate adulteration in Tokaj with a high accuracy and low error. The methods can be applied for routine quality checks of botrytized wines. PRACTICAL APPLICATION: Tokaj wines (Hungaricum) are botrytized wines acknowledged for the unique organoleptic properties bestowed by botrytized grape berries during production. Excluding these berries during wine production or manipulating the sugar content of low-grade wines to imitate high-grade wines are some recent suspicious activities that threaten the wine quality. Using advanced instruments, the electronic tongue, benchtop near infrared spectroscopy, and a handheld near infrared spectroscopy, we could discriminate, classify, and predict grape must concentrate adulteration in Tokaj with a high accuracy and low error. The models in our study can be applied for routine quality checks of botrytized wines.