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Detection of the adulteration of extra virgin olive oil by near-infrared spectroscopy and chemometric techniques
摘要： Introduction and Objectives: Due to the value of extra virgin olive oil (EVOO), adulteration has become an important issue in the industry, which has created demand for quick and inexpensive fraud detection testing. In contrast to many current food fraud detection methods, near-infrared spectroscopy (NIRS) can be inexpensive and convenient by minimizing sample preparation and measurement times. In this study, we developed a method using NIRS and chemometrics to detect adulteration of EVOO with other edible oil types that does not require sample preparation and can be completed in less than 10 min. Methods, Results, and Discussions: First, a single EVOO was adulterated with corn oil from 2.7% to 25% w/w. Spectra for the unadulterated sample and its adulterated counterparts were measured. A principal component analysis (PCA) scores plot showed separation between the adulterated mixtures and the unadulterated sample, which demonstrated that the developed method could detect as low as 2.7% w/w adulteration if an unadulterated sample of the oil in question is provided. To study adulteration detection without an unadulterated sample for reference, the spectra of unadulterated samples and samples adulterated with corn, sunflower, soybean, and canola oils were measured. A PCA with soft independent modelling of class analogy was used for adulteration detection. Lower limits of adulteration detection for corn, sunflower, soybean, and canola oils were found to be approximately 20%, 20%, 15%, and 10%, respectively. Conclusions: These results demonstrate that the developed method can be used to rapidly screen for adulterated olive oils.
关键词： principal component analysis,olive oil adulteration,chemometrics,NIR,spectroscopy
更新于2025-09-23 15:23:52
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Prediction of coumarin and ethyl vanillin in pure vanilla extracts using MID-FTIR spectroscopy and chemometrics
摘要： Fourier transform mid-infrared (MID-FTIR) spectroscopy coupled with chemometric analysis was used to identify and quantify coumarin (CMR) and ethyl vanillin (EVA) adulterations in pure vanilla extracts. Forty samples adulterated with CMR (0.25-10 ppm) and forty with EVA (0.25-10%) were prepared from pure vanilla extracts and characterized by MID-FTIR spectroscopy to develop chemometric models. Additionally, six commercial vanilla samples were analyzed. A soft independent modeling of class analogy (SIMCA) model was developed to identify and classify the purity from EVA-adulterated or CMR-adulterated samples. Prediction models for CMR or EVA content were developed using the principal component regression (PCR), partial least squares with single y-variables (PLS1), and with multiple y-variables (PLS2) algorithms. Moreover, the predictions of the best quantification chemometric model were compared with the results of a high-performance liquid chromatography-diode array detector (HPLC-DAD) method to evaluate the accuracy of the prediction. The PLS1 algorithm had better performance using 3 and 8 factors for EVA and CMR, respectively. The SIMCA model showed 100% recognition and rejections rates. The results demonstrate that adulteration of pure vanilla with EVA and CMR could be successfully predicted by the developed technique.
关键词： coumarin,ethyl vanillin,chemometrics,MID-FTIR,vanilla extracts,adulteration
更新于2025-09-23 15:23:52
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The feasibility of applying NIR and FT-IR fingerprinting to detect adulteration in black pepper
摘要： Black pepper is the most widely used spice in the world. Spices are highly vulnerable to economically motivated adulteration as they are high value products and traded along complex supply chains. The main fraud opportunity is to add cheaper bulking materials. Near and Fourier-Transform Infrared Spectroscopy has been combined with chemometrics to screen for the substitution of black pepper with papaya seeds, chili and with non-functional black pepper material such as black pepper husk, pinheads and defatted spent materials. A good separation performance between black pepper and adulterated samples could be shown. After running a binary classification model with an external test set an area under the receiver operator characteristic curve of 0.98 for both, the NIR and FT-IR model was obtained. This study shows the huge potential for a fast and rapid screening method that can be used to prove the authenticity of black pepper and detect adulterants.
关键词： Black Pepper,Screening method,Adulteration,Fourier transform infrared,Near infrared,Authenticity
更新于2025-09-23 15:22:29
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Data fusion strategy in quantitative analysis of spectroscopy relevant to olive oil adulteration
摘要： Olive oil adulteration with various less expensive edible oils represents a great danger for consumers. Spectrometry has been used to detect olive oil adulteration with other oil, but we need more robust and accurate model. Therefore, this work investigated the combination of infrared (NIR) and mid infrared (MIR) spectroscopy for the quantification of rapeseed oil in olive oil blends. Furthermore, a partial least squares (PLS) model was established to predict the concentration of the adulterant. Models constructed using baseline correction by combination of standard normal variate (SNV), SG smoothing and vector normalization pretreatments, respectively. Three data fusion strategies (low, mid and high-level) have been applied to take advantage of the synergistic effect of the information obtained from NIR and MIR. We chose algorithm (SPA) to extract spectral features for mid-level data fusion. Binary linear regression used in high-level data fusion. We selected the best pretreatment for final evaluation according to the evaluation parameters (R2 of calibration and validation, RMSECV and RMSEP). NIR, MIR and data fusion models were evaluated by comparing the R2 of validation and RMSEP (root mean square error of prediction). The RMSEP of low-level (3.44) , high-level (2.86) data fusion were better than NIR（7.09）, MIR（4.04）, mid-level（6.09）and the validation coefficient of determination R2 of low-level data fusion (0.975) and high-level data fusion (0.988) are better than the NIR (0.896) and MIR (0.966). Results showed that：(1) NIR and MIR are fast and non-destructive testing tools to detect the extra-virgin olive oil adulteration with rapeseed oil. (2) Low-level data fusion can effectively improve model prediction accuracy. (3) SPA reduced the number of variables, but it did not improved the results. (4) High-level data fusion strategy can be used as a reliable tool for quantitative analysis.
关键词： Olive oil,data fusion,SPA,MIR,Adulteration,NIR
更新于2025-09-23 15:22:29
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A new formaldehyde optical sensor: detecting milk adulteration
摘要： A sensor consisting of an optic fibre with the exposed tip coated with a the polyoxometalate salt [(C4H9)4N]4H[PMo10V2O40], specially designed to be insoluble in water, which UV-Vis spectrum changed in contact with formaldehyde, is presented. The sensor limit of detection for formaldehyde was 0.2 mg L-1, and the limit of quantification was 0.6 mg L-1, which were close to the conventional spectrophotometric method values of 0.2 mg L-1 and 0.5 mg L-1, respectively, and lower than the tolerable limit for ingested food. The sensor was tested for formaldehyde quantification in milk, as its deliberate addition is a matter of concern. The results obtained analysing formaldehyde in milk samples by the optical sensor and by the conventional method were not statistically different (α=0.05).
关键词： acetylacetone method,milk,formaldehyde,polyoxometalate,food adulteration,optical fibre sensor
更新于2025-09-23 15:21:01
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[IEEE 2019 Workshop on Recent Advances in Photonics (WRAP) - Guwahati, India (2019.12.13-2019.12.14)] 2019 Workshop on Recent Advances in Photonics (WRAP) - A side-polished macro bend fiber sensor for the efficient Detection of petrol adulteration
摘要： A side-polished macro bend fiber sensor is fabricated and demonstrated here. The working principle is based on the macro bending loss and evanescent field absorption. A sensitivity of 90nW/% and 45nW/% are obtained for low and high level of adulteration respectively.
关键词： Side-polished,Sensors,Plastic optical fibers (POFs),Petrol adulteration
更新于2025-09-23 15:21:01
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Rapid analysis of food raw materials adulteration using laser direct infrared spectroscopy and imaging
摘要： The objective of this study was to assess the application of the Laser Direct Infrared (LDIR) imaging system as a rapid screening technology for detection, identification, and semi-quantitation of adulterants in food ingredients. Forty-five samples of skimmed milk powder, thirty-one samples of soy protein isolate, thirty-five samples of chicken meat powder, thirty-two samples of pea protein isolate and six samples of wheat flour were dry blended adulterated with nitrogen-rich compounds and bulking agents at concentrations of 1.0 to 15.0% (w/w). In addition, ten samples of skimmed milk powder were wet blended with food adulterants at 5.0% and 10.0% (w/w) to check the LDIR performance when different fraudulent processes are applied. The results from this study shows that LDIR can be used as a rapid untargeted screening method that are independent of adulterants to detect, identify and semi-quantify food adulterants in dry blended samples. In most samples, the technology accurately identified all nitrogen-rich compounds and bulking agents present in the dry blended samples. In addition, the technology shows sensitivity of 82% for samples adulterated at 1% and sensitivity from 92% to 100% for samples adulterated at ≥ 5% economic adulteration. On the other hand, the detection and identification of food adulterants in samples prepared by wet blending process was more challenging than dry blended samples because mid-infrared technology may not be sensitive enough to detect adulterants if they are dissolved or if hidden within the particles.
关键词： Food adulteration,mid-infrared,laser direct infrared imaging,vibrational spectroscopy,untargeted method,raw materials
更新于2025-09-23 15:19:57
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Bimetallic Core Shelled Nanoparticles (Au@AgNPs) for Rapid Detection of Thiram and Dicyandiamide Contaminants in Liquid Milk Using SERS
摘要： Existing methods for contaminants detection in liquid milk are complex, requires chemicals and time-consuming experimental procedure. In this study, SERS based on bimetallic core shelled nanoparticles was employed for simultaneous and fast detection of thiram and dicyandiamide (DCD) in the milk. Spectra ranging from 400 to 1700 cm-1 were selected to examine thiram (0.5, 1, 2, 5 and 10 ppm) and DCD (20, 40, 80,160 and 320 ppm), by employing 28 nm gold cores and silver-shell thickness of 8 nm. A strong peak at 1379 cm-1 was ascribed to thiram with LOD of 0.21 ppm and R2 of 0.9896, whereas a band at 929 cm-1 was associated with DCD, delivering LOD of 14.88 ppm and R2 of 0.9956. The proposed method could achieve results within 34 min and this ecofriendly method can be further employed for simultaneous and rapid screening of other accidental contaminants in milk.
关键词： SERS,dicyandiamide,milk adulteration,thiram
更新于2025-09-23 15:19:57
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Fast Quantification of Honey Adulteration with Laser-Induced Breakdown Spectroscopy and Chemometric Methods
摘要： Honey adulteration is a major issue in food production, which may reduce the effective components in honey and have a detrimental effect on human health. Herein, laser-induced breakdown spectroscopy (LIBS) combined with chemometric methods was used to fast quantify the adulterant content. Two common types of adulteration, including mixing acacia honey with high fructose corn syrup (HFCS) and rape honey, were quantified with univariate analysis and partial least squares regression (PLSR). In addition, the variable importance was tested with univariable analysis and feature selection methods (genetic algorithm (GA), variable importance in projection (VIP), selectivity ratio (SR)). The results indicated that emissions from Mg II 279.58, 280.30 nm, Mg I 285.25 nm, Ca II 393.37, 396.89 nm, Ca I 422.70 nm, Na I 589.03, 589.64 nm, and K I 766.57, 769.97 nm had compact relationship with adulterant content. Best models for detecting the adulteration ratio of HFCS 55, HFCS 90, and rape honey were achieved by SR-PLSR, VIP-PLSR, and VIP-PLSR, with root-mean-square error (RMSE) of 8.9%, 8.2%, and 4.8%, respectively. This study provided a fast and simple approach for detecting honey adulteration.
关键词： partial least square regression,laser-induced breakdown spectroscopy,adulteration,feature variable,honey
更新于2025-09-23 15:19:57
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Authentication of Grappa (Italian grape marc spirit) by Mid and Near Infrared spectroscopies coupled with chemometrics
摘要： The aim of the present study is to authenticate Grappa spirits and to develop a non-destructive methodology which would allow detecting possible adulteration (by less valuable spirits) on this product. Grappa is an Italian alcoholic drink obtained by distillation of grape marks which has recently received the Geographical Indication (GI) label. As a high added-value product, it is relevant to develop methodologies which allow its authentication and detecting possible frauds (e.g., adulterations); and, whether feasible, it would be suitable to achieve these goals through non-destructive approaches (in order to minimize the economic loss). Mid Infrared (MIR) and Near Infrared (NIR) spectroscopies have been used for the authentication and the characterization of the spirits under investigation. The present work is conceptually divided into two parts: the first one, centered on the authentication of grappa spirits, focused on distinguishing them from other Italian distillates, and a second one aimed at developing an analytical methodology suitable to discern between pure and adulterated grappas. Both classification problems have been investigated by PLS-DA and by three multi-block strategies, i.e., Multi-Block Partial Least Squares (MB-PLS), Sequential and Orthogonalized Partial Least Squares (SO-PLS) and Sequential and Orthogonalized Covariance Selection (SO-CovSel) in order to test whether a data-fusion approach would lead to an improvements of the classification rates. The best results (in terms of predictions) were provided by multi-block strategies; in particular, they provided 100 % of correct classification when applied to discriminate pure and adulterated samples, suggesting these methodologies are definitely suitable for the proposed purpose.
关键词： Adulteration,IR,SO-CovSel,SO-PLS,Data fusion,PLS-DA
更新于2025-09-23 15:19:57