Fingerprinting black tea: When spectroscopy meets machine learning a novel workflow for geographical origin identification.

Food fraud, along with many challenges to the integrity and sustainability, threatens the prosperity of businesses and society as a whole. Tea is the second most commonly consumed non-alcoholic beverage globally. Challenges to tea authenticity require the development of highly efficient and rapid solutions to improve supply chain transparency. This study has produced an innovative workflow for black tea geographical indications (GI) discrimination based on non-targeted spectroscopic fingerprinting techniques. A total of 360 samples originating from nine GI regions worldwide were analysed by Fourier Transform Infrared (FTIR) and Near Infrared spectroscopy. Machine learning algorithms (k-nearest neighbours and support vector machine models) applied to the test data greatly improved the GI identification achieving 100% accuracy using FTIR. This workflow will provide a low-cost and user-friendly solution for on-site and real-time determination of black tea geographical origin along supply chains.

Using plants in forensics: State-of-the-art and prospects.

The increasing use of plant evidence in forensic investigations gave rise to a powerful new discipline - Forensic Botany - that analyses micro- or macroscopic plant materials, such as the totality or fragments of an organ (i.e., leaves, stems, seeds, fruits, roots) and tissue (i.e., pollen grains, spores, fibers, cork) or its chemical composition (i. e., secondary metabolites, isotopes, DNA, starch grains). Forensic botanists frequently use microscopy, chemical analysis, and botanical expertise to identify and interpret evidence crucial to solving civil and criminal issues, collaborating in enforcing laws or regulations, and ensuring public health safeguards. The present work comprehensively examines the current state and future potential of Forensic Botany. The first section conveys the critical steps of plant evidence collection, documentation, and preservation, emphasizing the importance of these initial steps in maintaining the integrity of the items. It explores the different molecular analyses, covering the identification of plant species and varieties or cultivars, and discusses the limitations and challenges of these techniques in forensics. The subsequent section covers the diversity of Forensic Botany approaches, examining how plant evidence exposes food and pharmaceutical frauds, uncovers insufficient or erroneous labeling, traces illegal drug trafficking routes, and combats the illegal collection or trade of protected species and derivatives. National and global security issues, including the implications of biological warfare, bioterrorism, and biocrime are addressed, and a review of the contributions of plant evidence in crime scene investigations is provided, synthesizing a comprehensive overview of the diverse facets of Forensic Botany.

Portable near-infrared (NIR) spectrometer and chemometrics for rapid identification of butter cheese adulteration.

Artisanal cheeses are highly valued around the world for their distinct sensory characteristics, thus being prone to adulteration by substituting authentic material for cheaper products, such as vegetable oil. In this work, we developed a method based on a portable NIR spectrometer as a non-destructive and low-cost alternative to identify adulteration in butter cheese. Dataset consisted of authentic and intentionally adulterated cheeses in the laboratory and commercial cheeses, which were identified as authentic and adulterated with vegetable oil after analysis of the fatty acid profile. PLS-DA classification models identified adulterated samples with an accuracy of 94.44%. PLS prediction models showed excellent performance (RPD > 3.0) to predict the adulterant level. These results demonstrate that NIR spectra can be used to identify the replacement of authentic fat by soybean oil in butter cheese and that the developed models can be used to identify adulteration in external samples with good performance.

Metabolomics in tea products; a compile of applications for enhancing agricultural traits and quality control analysis of Camellia sinensis.

Tea is one of the world's most popular beverages, with several health benefits. Polyphenols are the predominant constituents to account for its health benefits. Despite the well-known benefits of tea on health, the uniqueness of its aroma, taste, and features is an added value that contribute to the increased popularity of this beverage worldwide, and they are associated with the alterations in the metabolites during tea processing and cultivation. The manufacturing of tea consists of several stages with various processes as withering, fixing, rolling, fermentation and drying. The classification into tea types is according to such processing. The high-quality production of the various tea classes also depends on agricultural conditions, such as shading, plucking, climate, and soil composition. Metabolomics is well recognized as an effective tool for evaluating the quality of tea products. Applications in controlling the quality of tea products and adulterant detection are discussed in this review.

Application of DNA barcoding for ensuring food safety and quality.

With increasing international food trade, food quality and safety are high priority worldwide. The consumption of contaminated and adulterated food can cause serious health problems such as infectious diseases and allergies. Therefore, the authentication and traceability systems are needed to improve food safety. The mitochondrial DNA can be used for species authentication of food and food products. Effective DNA barcode markers have been developed to correctly identify species. The US FDA approved to the use of DNA barcoding for various food products. The DNA barcoding technology can be used as a regulatory tool for identification and authenticity. The application of DNA barcoding can reduce the microbiological and toxicological risks associated with the consumption of food and food products. DNA barcoding can be a gold-standard method in food authenticity and fraud detection. This review describes the DNA barcoding method for preventing food fraud and adulteration in meat, fish, and medicinal plants.

Qualitative identification of mature milk adulteration in bovine colostrum using noise-reduced dielectric spectra and linear model.

BACKGROUND: The rapid and accurate identification of colostrum, a strong non-homogeneous food, remains a challenge. In the present study, the dielectric spectra including the dielectric constant (ε') and loss factor (ε″) of 154 colostrum samples adulterated with 0-50% mature milk were measured from 20 to 4500 MHz. RESULTS: The results showed that the noise-reducing spectral preprocessing, including Savitzky-Golay (S-G), second derivative (SD), and S-G + SD, was significantly better than scattering-eliminating, including standard normal variate (SNV), multiplicative scatter correction (MSC), and SNV + MSC. The combination of S-G and SD was the best. Principal component analysis results demonstrated that dielectric spectroscopy is less susceptible to the inhomogeneity of colostrum and can be used to identify doped colostrum. The identification performance of linear models was better than that of non-linear models. The established linear discriminant analysis model based on full spectra had the best accuracy rates of 99.14% and 97.37% in the calibration and validation sets, respectively. Confirmatory tests on samples from different sources confirmed the satisfactory robustness of the proposed model. CONCLUSION: We found that the main unfavorable effect on the identification based on dielectric spectroscopy was noise interference, rather than scattering effect caused by inhomogeneity of colostrum. The satisfactory results undoubtedly cast light on rapid detection of strongly non-homogeneous foods based on dielectric spectroscopy. © 2022 Society of Chemical Industry.

Fraud detection in crude palm oil using SERS combined with chemometrics.

Edible crude palm oil (CPO) is a vital oil utilized in various industries, including food, pharmaceuticals, and domestic cooking. Unfortunately, reports of CPO adulteration with harmful Sudan dyes have surfaced over the years. Surface-enhanced Raman spectroscopy (SERS) and chemometrics were employed to detect Sudan dyes adulteration in CPO within 900 - 1800 cm- 1 Raman peak. The concentration of Sudan dyes detected in CPO samples ranged between 0.005 and 4 ppm. The principal component analysis (PCA) model detected Sudan II and Sudan IV in CPO with 99.88 and 99.90% accuracy. Linear discriminant analysis (LDA) and K-Nearest Neighbors (KNN) also recorded high detection rates of Sudan II and IV dyes in CPO. Sudan II and IV dyes could be detected at 0.0028 ppm and 0.0019 ppm by this sensor. The performance of the Au@Ag SERS sensor was comparable to that of HPLC. This study proved SERS and chemometrics can be used to authenticate edible CPO.

The reliability of biomedical science: A case history of a maturing experimental field.

There is much discussion in the media and some of the scientific literature of how many of the conclusions from scientific research should be doubted. These critiques often focus on studies - typically in non-experimental spheres of biomedical and social sciences - that search large datasets for novel correlations, with a risk that inappropriate statistical evaluations might yield dubious conclusions. By contrast, results from experimental biological research can often be interpreted largely without statistical analysis. Typically: novel observation(s) are reported, and an explanatory hypothesis is offered; multiple labs undertake experiments to test the hypothesis; interpretation of the results may refute the hypothesis, support it or provoke its modification; the test/revise sequence is reiterated many times; and the field moves forward. I illustrate this experimental/non-experimental dichotomy by examining the contrasting recent histories of: (a) our remarkable and growing understanding of how several inositol-containing phospholipids contribute to the lives of eukaryote cells; and (b) the difficulty of achieving any agreed mechanistic understanding of why consuming dietary supplements of inositol is clinically beneficial in some metabolic diseases.

Food regulation and policing: innovative technology to close the regulatory gap in Australia.

Internationally, food regulations are centred on human health and safety to prevent health crises. In Australia, regulatory control over the health and safety of humans is sound, however from a criminological perspective, control over fraudulent activities within food supply chains lack. Food fraud knows no geographical boundaries and has endless reach, therefore should be prioritised by policymakers, regulators and law enforcement. Australia's reputation for high-quality food is important domestically, but also for establishing and maintaining trust in international food trade relationships, therefore lack of enforcement over food could damage 'Brand Australia'. Given the food industry's vested interest in maintaining this reputation, it must also play a role to protect it. This research reviews regulatory landscape against food fraud in Australia and then, questions whether coupling informal controls to support existing formal regulatory controls may be the most appropriate and holistic way forward to protect the industry and consumers. It tests a regulatory pluralism framework to determine whether it can logically organize informal, innovative responses to contribute cohesively alongside formal controls at various points along the supply chain to prevent food fraud. Finally, it considers available informal, innovative technologies to: enhance testing regimes; prevent product and label tampering; and trace food supply chains adopted internationally show positive progress in responding to increasingly sophisticated and organized global food fraud. The research concludes adopting a regulatory pluralism framework, coupling existing regulatory controls and innovative technology could enhance and strengthen Australia's regulatory response to fraud within its food industry.

Fast and semiquantitative screening for sildenafil in herbal over-the-counter formulations with atmospheric pressure solid analysis probe (ASAP) to prevent medicinal adulteration.

Herbal medicines are commonly used in many countries all around the world. In Western countries they are now gaining more and more popularity, whereas in countries like China and India they have been entrenched for millenniums. Some of these perceived herbal medicines claim to help when suffering from erectile dysfunction. Nevertheless, many of these products are adulterated with PDE5 inhibitors like sildenafil or α-blockers. Patients who suffer from high blood pressure sometimes resort to herbal products, as they are not allowed to take sildenafil because of negative drug-drug interactions with nitrates (often utilized as treatment for coronary diseases). Products which are then adulterated with PDE5 inhibitors, can seriously harm patients. Therefore, this study reports the instant screening of alleged herbal products by employing atmospheric pressure solids analysis probe and high-resolution mass spectrometry to determine adulterants. Three out of 12 investigated products contained sildenafil in ranges from 0.5% to 18%. Multivariate analysis of ambient mass spectrometry measurements revealed encouraging outcomes for distinguishing non-sildenafil and sildenafil adulterated samples. Atmospheric pressure solids analysis probe is therefore a promising method for the rapid determination of sildenafil in herbal products with possible downstream semiquantitative analysis.

Authentication of extra virgin Argan oil by selected-ion flow-tube mass-spectrometry fingerprinting and chemometrics.

Recognized for its nutritional and therapeutic use, extra-virgin Argan Oil (EVAO) is frequently adulterated. Selected-Ion Flow-Tube Mass Spectrometry (SIFT-MS) spectra were applied to quantify adulterants (i.e., Argan oil of lower quality (LQAO), olive oil (OO), and sunflower oil (SO)) in EVAO. Four data sets, i.e., using H3O+, NO+, O2+ reagent ions, and the combined data were considered. Soft independent modelling of class analogy (SIMCA), and partial least squares discriminant analysis (PLS-DA) were assessed to distinguish adulterated- from pure EVAO. The effectiveness of SIFT-MS associated with PLS and support vector machine (SVM) regression to quantify trace adulterants in EVAO was evaluated. Variable Importance in Projection (VIP), and interval-PLS (iPLS) were also investigated to extract useful features. Different models were built to predict the EVAO authenticity and the degree of adulteration. High accuracy was achieved. SIFT-MS spectra handled with the appropriate chemometric tools were found suitable for the quality evaluation of EVAO.

Metabolic composition and authenticity evaluation of bergamot essential oil assessed by nuclear magnetic resonance spectroscopy.

In this work, a sample of pure and certified bergamot essential oil (BEO) was extensively studied for the first time directly by NMR spectroscopy with the aim of investigating its metabolic composition, quantifying the main components of this complex natural matrix and simultaneously assessing whether the NMR technique is able to highlight possible frauds to which this high-cost product may be subjected. Eleven low molecular weight compounds have been identified by using 1D 1H and 13C-{1H} NMR experiments, 2D homo- and heteronuclear correlation NMR spectra, and 2D 1H DOSY experiments; the most abundant of them, i.e., about 90% of the sample analyzed, has been quantified by employing benzoic acid as an internal standard by 1H NMR spectrum. Moreover, since the commercial fraud of this precious oil is often due to the addition of less expensive oils, we have simulated a possible adulteration through the preparation of BEO samples to which different percentages of orange essential oil (OEO) were added. The results, obtained by combining the 1H NMR spectra collected on the adulterated samples and on pure BEO, with chemometric analysis, principal component analysis (PCA), indicate that it is possible to distinguish the sample of pure BEO from the adulterated ones and also, among them, to differentiate between the degrees of adulteration.

Fraud Detection of Herbal Medicines Based on Modern Analytical Technologies Combine with Chemometrics Approach: A Review.

Fraud in herbal medicines (HMs), commonplace throughout human history, is significantly related to medicinal effects with sometimes lethal consequences. Major HMs fraud events seem to occur with a certain regularity, such as substitution by counterfeits, adulteration by addition of inferior production-own materials, adulteration by chemical compounds, and adulteration by addition of foreign matter. The assessment of HMs fraud is in urgent demand to guarantee consumer protection against the four fraudulent activities. In this review, three analysis platforms (targeted, non-targeted, and the combination of non-targeted and targeted analysis) were introduced and summarized. Furthermore, the integration of analysis technology and chemometrics method (e.g., class-modeling, discrimination, and regression method) have also been discussed. Each integration shows different applicability depending on their advantages, drawbacks, and some factors, such as the explicit objective analysis or the nature of four types of HMs fraud. In an attempt to better solve four typical HMs fraud, appropriate analytical strategies are advised and illustrated with several typical studies. The article provides a general workflow of analysis methods that have been used for detection of HMs fraud. All analysis technologies and chemometrics methods applied can conduce to excellent reference value for further exploration of analysis methods in HMs fraud.

New perspectives for evaluating relative risks of African swine fever virus contamination in global feed ingredient supply chains.

There are no published reports indicating that the African swine fever virus (ASFV) has been detected in feed ingredients or complete feed. This is primarily because there are only a few laboratories in the world that have the biosecurity and analytical capabilities of detecting ASFV in feed. Several in vitro studies have been conducted to evaluate ASFV concentration, viability and inactivation when ASFV was added to various feed ingredients and complete feed. These inoculation studies have shown that some feed matrices support virus survival longer than others and the reasons for this are unknown. Current analytical methodologies have significant limitations in sensitivity, repeatability, ability to detect viable virus particles and association with infectivity. As a result, interpretation of findings using various measures may lead to misleading conclusions. Because of analytical and technical challenges, as well as the lack of ASFV contamination data in feed supply chains, quantitative risk assessments have not been conducted. A few qualitative risk assessments have been conducted, but they have not considered differences in potential scenarios for ASFV contamination between various types of feed ingredient supply chains. Therefore, the purpose of this review is to provide a more holistic understanding of the relative potential risks of ASFV contamination in various global feed ingredient supply chains and provide recommendations for addressing the challenges identified.

Authentication of organically grown vegetables by the application of ambient mass spectrometry and inductively coupled plasma (ICP) mass spectrometry; The leek case study.

Health conscious and environmentally aware consumers are purchasing more organically produced foods. They prefer organic fruits and leafy vegetables as these are much less likely to have been exposed to contaminants such as pesticides. The detection of fraudulent activity in this area is difficult to undertake, because many chemical plant protection treatments degrade very quickly or can be washed off to remove evidence of their existence. It was found that when combining DART-MS with a compact, inexpensive and robust single quadrupole mass spectrometer, it was possible to differentiate organic from conventional leeks with 93.8% to 100% accuracy. ICP-MS results showed similar performance, with an ability to differentiate conventional from organic leeks with 92.5% to 98.1% accuracy. This study has paved the way for the certification of vegetables as being organically produced. The next step is to create data libraries to support the roll out of the methodologies described.

DNA-Based Herbal Teas' Authentication: An ITS2 and psbA-trnH Multi-Marker DNA Metabarcoding Approach.

Medicinal plants have been widely used in traditional medicine due to their therapeutic properties. Although they are mostly used as herbal infusion and tincture, employment as ingredients of food supplements is increasing. However, fraud and adulteration are widespread issues. In our study, we aimed at evaluating DNA metabarcoding as a tool to identify product composition. In order to accomplish this, we analyzed fifteen commercial products with DNA metabarcoding, using two barcode regions: psbA-trnH and ITS2. Results showed that on average, 70% (44-100) of the declared ingredients have been identified. The ITS2 marker appears to identify more species (n = 60) than psbA-trnH (n = 35), with an ingredients' identification rate of 52% versus 45%, respectively. Some species are identified only by one marker rather than the other. Additionally, in order to evaluate the quantitative ability of high-throughput sequencing (HTS) to compare the plant component to the corresponding assigned sequences, in the laboratory, we created six mock mixtures of plants starting both from biomass and gDNA. Our analysis also supports the application of DNA metabarcoding for a relative quantitative analysis. These results move towards the application of HTS analysis for studying the composition of herbal teas for medicinal plants' traceability and quality control.

Three centuries on the science of coffee authenticity control.

Food authenticity relies on genuineness and reliability according to the information displayed on the package. Since the 18th century, when coffee became popularized in the West, adulteration began. Several methods have been developed to detect different kinds of frauds and they have evolved as demands increased and new technologies were introduced. The evolution of the science of coffee authenticity control in the past three centuries is reviewed, focusing on the discrimination between coffee and other foods or between coffee and its by-products. The earliest chemical and physical methods are presented followed by methods developed in the 20th and 21st centuries using microscopy, chromatography and spectroscopy associated with advanced statistical tools, and DNA-based methods. In addition to non-food material, before the 20th century, chicory was the most studied food-adulterant. From the 20th century on, corn, coffee by-products, and barley were the most studied, followed by chicory, rice and other food items. Matrix effects seem to be among the most challenging problems in these approaches, associated with variations in roast degree, particle size (particularly in spectroscopy-based methods), and lack of control over reference samples regarding species and purity. Limits of detection vary considerably within each category, with most limits being too high for commercial use. DNA-based methods appear to be promising to assess coffee authenticity, given that the limits of detection and quantification are low, and specificity is higher than in other methods. Nevertheless, as roast intensity increases, the sensitivity of the method decreases. So far, most reported methods have not been validated and only a few have been tested on commercial brands, except for those involving microscopy which has been highly used for monitoring coffee authenticity although not always efficiently enough.

A Traditional Chinese Medicine Traceability System Based on Lightweight Blockchain.

BACKGROUND: Recently, the problem of traditional Chinese medicine (TCM) safety has attracted attention worldwide. To prevent the spread of counterfeit drugs, it is necessary to establish a drug traceability system. A traditional drug traceability system can record the whole circulation process of drugs, from planting, production, processing, and warehousing to use by hospitals and patients. Once counterfeit drugs are found, they can be traced back to the source. However, traditional drug traceability systems have some drawbacks, such as failure to prevent tampering and facilitation of sensitive disclosure. Blockchain (including Bitcoin and Ethernet Square) is an effective technology to address the problems of traditional drug traceability systems. However, some risks impact the reliability of blockchain, such as information explosion, sensitive information leakage, and poor scalability. OBJECTIVE: To avoid the risks associated with the application of blockchain, we propose a lightweight block chain framework. METHODS: In this framework, both horizontal and vertical segmentations are performed when designing the blocks, and effective strategies are provided for both segmentations. For horizontal segmentation operations, the header and body of the blockchain are separated and stored in the blockchain, and the body is stored in the InterPlanetary File System. For vertical segmentation operations, the blockchain is cut off according to time or size. For the addition of new blocks, miners only need to copy the latest part of the blockchain and append the tail and vertical segmentation of the block through the consensus mechanism. RESULTS: Our framework could greatly reduce the size of the blockchain and improve the verification efficiency. CONCLUSIONS: Experimental results have shown that the efficiency improves compared with ethernet when a new block is added to the blockchain and a search is conducted.

Non-destructive authentication of Gourmet ground roasted coffees using NIR spectroscopy and digital images.

The growing demand for excellent-quality coffees allied with their symbolic aestheticization that add value to the products favor the adulteration practices and consequently economic losses. So, this work proposes the suitability of NIR spectroscopy and Digital Images (from CACHAS) coupled with one-class classification methods for the non-destructive authentication of Gourmet ground roasted coffees. For this, Gourmet coffees (n = 44) were discriminated from Traditional (n = 36) and Superior (n = 10) by directly analyzing their powder without any sample preparation. Then, OC-PLS and dd-SIMCA were used to construct the models. dd-SIMCA using offset correction for NIR and RGB histogram for CACHAS achieved the best results, correctly recognizing all the 90 samples in both the training and test sets. Therefore, the proposed methodologies can be useful for both the consumers and regulatory agencies because it confirms the elevated standards of excellence of Brazilian specialty coffees, preventing fraudulent labeling, besides following the Principles of Green Analytical Chemistry.

Caffeine Health Claims on Sports Supplement Labeling. Analytical Assessment According to EFSA Scientific Opinion and International Evidence and Criteria.

Caffeine is a food supplement widely consumed by athletes, but it has not been established. So far, the veracity of their labeling in terms of the dosage and cause/effect relationship aimed at the consumer. The aim is to analyze the health claims and the dosage presented on the labeling of caffeine supplements and to evaluate if they follow the European Food Safety Authority (EFSA) and international criteria. A descriptive cross-sectional study of a sample of caffeine supplements was carried out. The search was done through the Amazon and Google Shopping web portals. In order to assess the adequacy of the health claims, the guidelines of reference established by European Food Safety Authority were compared to the Academy of Nutrition and Dietetics, International Olympic Committee, and Australian Institute of Sport guidelines; in addition, recent systematic reviews were addressed. A review of labels of 42 caffeine supplements showed that, in less than 3% of the products were the health claims supported by the recommendations and by the labeled quantity of caffeine. The claims that fully complied the recommendations were, "improves or increases endurance performance", "improves strength performance", or "improves short-term performance". In most cases, the recommended dosage was 200 mg/day for these products, which is the minimum for the caffeine effects to be declared. The rest of the health claims were not adequate or need to be modified. Most of the health claims identified indicated an unproven cause and effect, which constitutes consumer fraud, and so must be modified or eliminated.