Authentication Of Oils Research Articles

Detecting Olive Oil Fraud with Near-Infrared Spectroscopy and Chemometrics: A Modern Safety Control Approach

Background: Olive oil is one of the most essential components of the Mediterranean diet, obtained by mechanical extraction from the Olea europaea tree. Based on organoleptic properties (odor and taste) and the amount of free fatty acids, it is divided into three categories: Olive oil, virgin olive oil, and extra virgin olive oil. Due to the expensive production procedure of extra virgin olive oil, it is prone to adulteration with low-quality olive oils and other vegetable oils. Objectives: The current study focused on determining the authenticity of olive oil using near-infrared spectroscopy as a non-destructive method in conjunction with chemometrics. Methods: In this study, 100 samples of olive oils, comprising 34 domestic and 66 industrial olive oils, were purchased from the markets of Tehran and Roudbar. Common adulterants such as corn, canola, sunflower, and soybean oils were considered. Binary and ternary mixtures of olive oil with these vegetable oils were prepared and analyzed. Spectra were collected over the range of 12000 cm-1 to 4000 cm-1, and the data were preprocessed using SNV and Detrend before principal component analysis (PCA). Results: The results indicated that corn oil and canola oil were the dominant adulterants in the olive oil samples, likely due to their inexpensiveness and availability in Iran. Conclusions: Since multiple types of fraud were identified in the examined samples, it is recommended that future studies investigate other forms of fraud simultaneously. Additionally, the results demonstrated that principal component analysis could effectively categorize different samples with acceptable discrimination.

Machine learning-enabled high-throughput industry screening of edible oils

Long-term consumption of mixed fraudulent edible oils increases the risk of developing of chronic diseases which has been a threat to the public health globally. The complicated global supply-chain is making the industry malpractices had often gone undetected. In order to restore the confidence of consumers, traceability (and accountability) of every level in the supply chain is vital. In this work, we shown that machine learning (ML) assisted windowed spectroscopy (e.g., visible-band, infra-red band) produces high-throughput, non-destructive, and label-free authentication of edible oils (e.g., olive oils, sunflower oils), offers the feasibility for rapid analysis of large-scale industrial screening. We report achieving high-level of discriminant (AUC > 0.96) in the large-scale (n ≈ 11,500) of adulteration in olive oils. Notably, high clustering fidelity of ‘spectral fingerprints’ achieved created opportunity for (hypothesis-free) self-sustaining large database compilation which was never possible without machine learning. (137 words).

Real-Time Authentication of Camellia Oil by Rapid Evaporative Ionization Mass Spectrometry

Camellia oil is a high-value product with rich nutrients. Recently, the adulteration of camellia oil has become an increasingly concerning issue related to human health. In this study, electric soldering iron coupled with rapid evaporative ionization mass spectrometry (REIMS) was employed for the identification and analysis of camellia oil without any sample preparation. REIMS technology coupled with chemometrics was applied to develop an analysis model for the authentication of camellia oil adulterated with soybean oil, peanut oil, rapeseed oil, sunflower oil, and corn oil (5–40%, v/v). The results showed that different types of vegetable oils could be classified using principal component analysis-linear discriminant analysis (PCA-LDA) with a correct classification of 93.8% in leave-20%-out cross-validation and 100% correctly identified in real-time recognition. The established prediction models were found to be particularly sensitive when the camellia oil samples were adulterated with 5–40% of other oils, indicating that REIMS could be a powerful tool for the authentication and adulteration analysis of camellia oil, particularly for cases where the adulteration levels are relatively high. In conclusion, the results provide valuable insights into the potential of REIMS for the rapid, accurate, and real-time authentication and adulteration analysis of camellia oil.

TaqMan real-time quantitative PCR for the detection of beef tallow to assess the authenticity of edible oils

TaqMan real-time quantitative PCR for the detection of beef tallow to assess the authenticity of edible oils

Screening Method for the Visual Discrimination of Olive Oil from Other Vegetable Oils by a Multispecies DNA Sensor.

Olive oil is a prominent agricultural product which, in addition to its nutritional value and unique organoleptic characteristics, offers a variety of health benefits protecting against cardiovascular disease, cancer, and neurodegenerative diseases. The assessment of olive oil authenticity is an extremely important and challenging process aimed at protecting consumers and producers. The most frequent adulteration involves blending with less expensive and readily available vegetable/seed oils. The methods for adulteration detection, whether based on changes in metabolite profiles or based on DNA markers, require advanced and expensive instrumentation combined with powerful chemometric and statistical tools. To this end, we present a simple, multiplex, and inexpensive screening method based on the development of a multispecies DNA sensor for sample interrogation with the naked eye. It is the first report of a DNA sensor for olive oil adulteration detection with other plant oils. The sensor meets the 2-fold challenge of adulteration detection, i.e., determining whether the olive oil sample is adulterated and identifying the added vegetable oil. We have identified unique, nucleotide variations, which enable the discrimination of seven plant species (olive, corn, sesame, soy, sunflower, almond, and hazelnut). Following a single PCR step, a 20 min multiplex plant-discrimination reaction is performed, and the products are applied directly to the sensing device. The plant species are visualized as red spots using functionalized gold nanoparticles as reporters. The spot position reveals the identity of the plant species. As low as <5-10% of adulterant was detected with particularly good reproducibility and specificity.

Authentication of Fennel, Star Anise, and Anise Essential Oils by Gas Chromatography (GC/MS) and Stable Isotope Ratio (GC/IRMS) Analyses.

The aromatic compound (E)-anethol is widely used in the flavor, fragrance, and medicinal industries. This compound is commonly produced through steam distillation of fennel, star anise, and anise seed. Given the cost of production, these natural and authentic essential oils are commonly adulterated with lower-cost natural materials or synthetic alternatives. The current study investigates essential oil profiles (gas chromatography/mass spectrometry) and stable isotope ratios (gas chromatography/isotope ratio mass spectrometry) of the abundant compound (E)-anethol in both authentic reference standards (n = 15) and commercially available samples (n = 30). This multifaceted analytical approach establishes techniques for ensuring the authenticity of essential oil sources of (E)-anethol and was then used to evaluate the current essential oil market sources of (E)-anethol. These findings report that adulteration of (E)-anethol-containing natural products takes various forms, and a multifaceted analytical approach is recommended for authentication. Of the commercial samples analyzed for this report, 27% were adulterated.

Trends in authentication of edible oils using vibrational spectroscopic techniques.

The authentication of edible oils has become increasingly important for ensuring product quality, safety, and compliance with regulatory standards. Some prevalent authenticity issues found in edible oils include blending expensive oils with cheaper substitutes or lower-grade oils, incorrect labeling regarding the oil's source or type, and falsely stating the oil's origin. Vibrational spectroscopy techniques, such as infrared (IR) and Raman spectroscopy, have emerged as effective tools for rapidly and non-destructively analyzing edible oils. This review paper offers a comprehensive overview of recent advancements in using vibrational spectroscopy for authenticating edible oils. The fundamental principles underlying vibrational spectroscopy are introduced and chemometric approaches that enhance the accuracy and reliability of edible oil authentication are summarized. Recent research trends highlighted in the review include authenticating newly introduced oils, identifying oils based on their specific origins, adopting handheld/portable spectrometers and hyperspectral imaging, and integrating modern data handling techniques into the use of vibrational spectroscopic techniques for edible oil authentication. Overall, this review provides insights into the current state-of-the-art techniques and prospects for utilizing vibrational spectroscopy in the authentication of edible oils, thereby facilitating quality control and consumer protection in the food industry.

1H NMR AS A TOOL FOR VEGETABLE OIL QUALITY ASSESSMENT

Background. Vegetable oils play an important role in the food, pharmaceutical and cosmetic indus tries. They are not only a source of nutrients, but also a carrier of bioactive substances as an ingredient of creams or emulsions. Some oils, like extra virgin olive oil or argan oil, due to high consumer demand and high prices, may be subject to adulteration by using cheaper and easily accessible oils. Hence, the need to develop new research methods enabling the quick identification of such adulterations, but also enabling the assessment of oil quality, e.g. in variable storage conditions. Typically, gas chromatography (GC) is used to assess the profile of fatty acids. Oil parameters such as acid number, peroxide value and iodine number are also assessed to determine oil quality. Nevertheless, instead of performing all the above mentioned tests, these parameters can also be determined directly from 1H NMR spectra. Hence, there is great potential for using this method in quick screening of oil quality. The 1H NMR technique has been growing in importance in recent years in researching the quality and composition of food, including vege table oils. Multidimensional NMR techniques and analysis of other nuclei (13C NMR) are also used in the study of oils. The aim of this work is to present the applications of the most commonly used 1H NMR technique. Results and Conclusions. The article contains examples of the application of this method in testing the composition, quality and authenticity of olive oil, hemp oil and argan oil as oils used (both in the food, medical or cosmetic context) and becoming more and more popular among consumers.

Detection and quantification of olive oil adulteration using fluorescence spectroscopy and chemometric tools

The increasing incidence of fraud in the olive oil market, particularly through adulteration with cheaper oils, poses a major challenge for the industry. This study examines the effectiveness of fluorescence spectroscopy combined with chemometric tools as a method to detect and quantify olive oil adulteration. Chemical analyses were used to measure parameters such as specific absorption coefficients K232 and K270, peroxide value, and acidity, in accordance with International Olive Council (IOC) standards. These measurements were conducted on samples of olive oil blended with varying percentages of adulterating oils. 3D fluorescence spectra were analyzed to examine the changes induced by adulteration. The results show that free acidity and peroxide value decrease with increasing adulteration degree, while the parameters K232 and K270 increase with the degree of adulteration. Principal component analysis (PCA) was effectively used to differentiate samples based on the percentage of adulterant. A partial least squares (PLS) regression model was developed, achieving a correlation coefficient of 0.999 for predicting the percentage of adulterant in olive oil. This PLS model also proved effective in predicting oil quality parameters such as free acidity and K232 and K270 indices. The results of this study demonstrate the significant potential of fluorescence spectroscopy as a rapid and non-destructive method for olive oil authentication. PCA emerges as a powerful tool for characterizing pure oils without requiring sample preparation or destruction. Furthermore, PLS models provide accurate means to predict both the presence of adulterants and olive oil quality parameters. This approach offers a promising solution to combat fraud in the olive oil industry, ensuring product integrity and quality.

Fatty acid composition, biological activity and authentication of marine fish oil

Marine fish oils (MFO) are known as sources of polyunsaturated fatty acids such as eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA), having beneficial effects on human health. MFO is considered an important raw material in the pharmaceutical, food, and cosmetics industries. It is classified as high price oil; therefore, MFO are subjected to adulteration with low price oils. This review aimed to provide a scientific view of the fatty acid composition, biological activity, and authentication of marine fish oil. Different species of fish have different nutritional content such as triacylglycerols composition, especially DHA, EPA, and lipid-soluble vitamins. Marine fish oil is one of the functional oils that have beneficial effects on human health. Marine fish oil has a high price in the market which is lucrative to be adulterated with lower-priced ones to gain economic profit, therefore reliable analytical methods for detecting the possible adulterated such as combined fourier transform infrared and chemometrics.

A review of advanced techniques for detecting the authenticity and adulteration of camellia oil

AbstractCamellia oil, one of the four major woody oils globally, possesses exceptional nutritional value due to its high contents of unsaturated fatty acids and functional compounds like tocopherols, phenolics, and chlorophyll. Unfortunately, due to high demand and cost, fraudsters deliberately mix lower‐quality vegetable oils with camellia oil for profits. This has raised concerns among stakeholders, prompting the need for robust authentication methods. This review provides a concise overview of various analytical techniques employed to assess the authenticity, quality, and potential adulteration of camellia oil. Several techniques, such as chromatography, isotope‐ratio mass spectrometry (IRMS), ion mobility spectrometry (IMS), differential scanning calorimetry (DSC), plasma‐based and deoxyribonucleic acid (DNA)‐based techniques, as well as emerging methods like electronic noses and electronic tongues, are discussed. Notably, traditional chromatographic techniques (GC and HPLC) are reported to be time‐consuming, laborious, employ toxic chemicals, and require complicated sample pretreatments. DNA techniques also face challenges in detecting adulterants due to the complex refining processes of camellia oil, including high‐temperature decolorization and deodorization, which reduce DNA content and induce degradation. In contrast, spectroscopic techniques such as fluorescence spectroscopy, nuclear magnetic resonance, and infrared (near, mid, far) spectroscopy combined with chemometric analyses, have emerged as reliable, rapid, simple, sensitive, and accurate alternative analytical tools for the quality control of camellia oil.

Temperature dependence of acoustic parameters in pure and blended edible oils: Implications for characterization and authentication

This research investigates the temperature-dependent variation of diverse acoustic parameters in samples of edible oils. It further supplements previous studies on the effectiveness of non-destructive ultrasonic inspection in the authentication of edible oils. The oils under examination consist of pure samples of olive, sunflower, and corn oils, as well as variable mixtures ranging from 20 % to 80 % of the more expensive one (olive oil) with the other two, simulating a hypothetical adulteration scenario. The studied acoustic parameters are related to the velocity, attenuation, and frequency components present in 2.25 MHz ultrasonic waves propagating through the oil samples within a temperature range of 24 °C to 34 °C. The results confirm the suitability of non-destructive ultrasonic inspection in evaluating and detecting the adulteration of olive oil with economically inferior oils such as sunflower and corn. Additionally, this study provides added value by laying the groundwork for a non-destructive and innovative determination of the fatty acid profile of an edible oil based on the evolution of the aforementioned ultrasonic parameters with temperature. The findings hold potential for enhancing the authenticity assessment and quality control of edible oils in the food industry.

Rapid Authentication and Detection of Olive Oil Adulteration Using Laser-Induced Breakdown Spectroscopy.

The adulteration of olive oil is a crucial matter for food safety authorities, global organizations, and consumers. To guarantee olive oil authenticity, the European Union (EU) has promoted the labeling of olive oils with the indices of Protected Designation of Origin (PDO) and Protected Geographical Identification (PGI), while food security agencies are also interested in newly emerging technologies capable of operating reliably, fast, and in real-time, either in situ or remotely, for quality control. Among the proposed methods, photonic technologies appear to be suitable and promising for dealing with this issue. In this regard, a laser-based technique, namely, Laser-Induced Breakdown Spectroscopy (LIBS), assisted via machine learning tools, is proposed for the real-time detection of olive oil adulteration with lower-quality oils (i.e., pomace, soybean, sunflower, and corn oils). The results of the present work demonstrate the high efficiency and potential of the LIBS technique for the rapid detection of olive oil adulteration and the detection of adulterants.

Authentication of pure and adulterated edible oils using non-destructive ultrasound.

At present, the quality of edible oil is evaluated using traditional analysis techniques that are generally destructive. Therefore, efforts are being made to find alternative methods with non-destructive techniques such as Ultrasound. This work aims to confirm the feasibility of non-destructive ultrasonic inspection to characterise and detect fraudulent practices in olive oil due to adulteration with two other edible vegetable oils (sunflower and corn). For this purpose, pulsed ultrasonic signals with a frequency of 2.25MHz have been used. The samples of pure olive oil were adulterated with the other two in variable percentages between 20% and 80%. Moreover, the viscosity and density values were measured. Both these physicochemical and acoustic parameters were obtained at 24°C and 30°C and linearly correlated with each other. The results indicate the sensitivity of the method at all levels of adulteration studied. The responses obtained through the parameters related to the components of velocity, attenuation, and frequency of the ultrasonic waves are complementary to each other. This allows concluding that the classification of pure and adulterated oil samples is possible through non-destructive ultrasonic inspection.

Authentication of Lavandula angustifolia Mill. (Lamiaceae) essential oil using physical property, gas chromatography, enantiomeric selectivity, and stable isotope analyses

ABSTRACT Authentic Lavandula angustifolia (lavender) essential oil samples (n = 41) were procured from six producing countries. Essential oils were analyzed to determine physical properties and to determine profiles and related data by GC/MS, GC/FID, enantioselective GC, and GC/IRMS. The current study identified 43 volatile compounds that were detected in all authentic lavender samples (n = 41), and which can be considered authentic markers. Enantiomeric ranges for 15 volatile compounds and stable isotope ranges for four prominent compounds were determined in authentic lavender. Authentic samples and associated data were used to assess the quality of commercially available lavender essential oil samples (n = 12). 75% of the commercial samples studied were adulterated,and 17 volatile compounds were detected in these samples which can be considered markers for adulteration. This study establishes the utility and importance of using a multifaceted analytical approach to differentiate quality and determine authenticity of lavender essential oil.

Combined use of 87Sr/86Sr and carbon isotopes with multielemental analysis for the geographical authentication of Tunisian and European olive oils.

The geographical authentication in the agrifood industry has become a major issue to guarantee the quality of food products. Olive oil (OO) is particularly a complex matrix and establishing a reliable approach for linking OO samples to their origin is an analytical challenge. In this study, the isotopic composition of carbon, strontium and the concentrations of seventeen elements were determined in OOs from Tunisia, Southern France and the South Basque country. The preliminary results overlapped and showed that, taken individually, the isotopic and elemental approaches were not discriminant. A linear discriminant analysis applied to δ13C, 87Sr/86Sr and to the concentrations of 4 selected trace elements (Fe, Mn, V and Cr) allowed to classify, with high resolution, olive oils into 3 groups according to their provenance. The combination of the plant growing environment, the geological background, the mineral composition of the soil and the production process lead to a novel approach to deal with fraudulent practices in OO sector.

Quality Standards and Pharmacological Interventions of Natural Oils: Current Scenario and Future Perspectives.

Medicinal plants are rich sources of natural oils such as essential and fixed oils used traditionally for nutritive as well as medicinal purposes. Most of the traditional formulations or phytopharmaceutical formulations contain oil as the main ingredient due to their own therapeutic applications and thus mitigating several pathogeneses such as fungal/bacterial/viral infection, gout, psoriasis, analgesic, antioxidant, skin infection, etc. Due to the lack of quality standards and progressive adulteration in the natural oils, their therapeutic efficacy is continuously deteriorated. To develop quality standards and validate scientific aspects on essential oils, several chromatographic and spectroscopic techniques such as HPTLC, HPLC, NMR, LC-MS, and GC-MS have been termed as the choices of techniques for better exploration of metabolites, hence sustaining the authenticity of the essential oils. In this review, chemical profiling and quality control aspects of essential or fixed oils have been explored from previously reported literature in reputed journals. Methods of chemical profiling, possible identified metabolites in essential oils, and their therapeutic applications have been described. The outcome of the review reveals that GC-MS/MS, LC-MS/MS, and NMR-based chromatographic and spectroscopic techniques are the most liable, economic, precise, and accurate techniques for determining the spuriousness or adulteration of oils based on their qualitative and quantitative chemical profiling studies. This review occupies the extensive information about the quality standards of several oils obtained from natural sources for their regulatory aspects via providing the detailed methods used in chemoprofiling techniques. Hence, this review helps researchers in further therapeutic exploration as well as quality-based standardization for their regulatory purpose.

Data standardization strategy to correct the effect of seasonality in the authentication of virgin olive oil

This study proposes a standardization strategy for dealing with seasonal variability in the authentication of extra virgin oils from the PDOs Les Garrigues and Siurana. Samples from four harvests were measured by fluorescence spectroscopy. A PLS-DA two-class model was developed and validated from samples from one of the harvests. When samples from three other harvests were predicted with the model developed, it was observed that the sensitivity and specificity were lower than when the model was validated. For the standardization process, we adapted the PDS technique to obtain the transfer function. The results obtained from the transformed spectra show that standardization is a good strategy for extending the usefulness of the models if the samples to be predicted are subject to seasonal variability.

Rapid detection of argan oil adulteration by frying oils using laser induced fluorescence spectroscopy combined with chemometrics tools

There is a contentious need for robust and rapid methodologies for maintaining the authenticity of foods. The aim of this study was to detect and quantify argan oil adulteration using Laser Induced Fluorescence (LIF) spectroscopy coupled with chemometric methods. Principal Component Analysis (PCA) and Partial Least Squares Regression (PLSR) were used to assess argan oil authenticity; PCA was used to classify samples according to their quality and the PLS model to determine the amount of adulterants in pure argan oil. The correlation coefficient of the obtained model was about 0.99, with Root Mean Square Error of Prediction (RMSEP) and Standard Error of Prediction (SEP) of 2%. This study demonstrated the feasibility of LIF spectroscopy combined with chemometric tools to identify adulterants in pure argan oil from a percentage of adulteration, of 0.35 % without the need to destruct samples.

Moroccan extra virgin argan oil authentication by using ultraviolet–visible and front face fluorescence spectroscopies combined with different descriptive and predictive chemometric tools

Moroccan extra virgin argan oil authentication by using ultraviolet–visible and front face fluorescence spectroscopies combined with different descriptive and predictive chemometric tools