Revealing adulterated olive oils by triacylglycerol screening methods: Beyond the official method.

Official control methods to detect olive oil (OO) adulteration fail to provide satisfactory consumer protection. Thus, faster and more sensitive screening tools are needed to increase their effectiveness. Here, the official method for adulterant detection in OO was compared with three untargeted screening methods based on triacylglycerol analysis using high-throughput (FIA-HESI-HRMS; HT-GC-MS; HPLC-RID) and pattern recognition techniques (PLS-DA). They were assayed on a set of genuine and adulterated samples with a high natural variability (n = 143). The sensitivity of the official method was 1 for high linoleic (HL) blends at ≥2 % but only 0.39 for high oleic (HO) blends at ≥5 %, while specificity was 0.96. The sensitivity of the screening methods in external validation was 0.90-0.99 for the detection of HL and 0.82-0.88 for HO blends. Among them, HT-GC-MS offered the highest sensitivity (0.94) and specificity (0.76), proving to be the most suitable screening tool for OO authentication.

Using fluorescence excitation-emission matrices to predict bitterness and pungency of virgin olive oil: A feasibility study.

Unlike other food products, virgin olive oil must undergo an organoleptic assessment that is currently based on a trained human panel, which presents drawbacks that might affect the efficiency and robustness. Therefore, disposing of instrumental methods that could serve as screening tools to support sensory panels is of paramount importance. The present work aimed to explore excitation-emission fluorescence spectroscopy (EEFS) to predict bitterness and pungency, since both attributes are related with fluorophore compounds, such as polar phenols. Bitterness and pungency intensities of 250 samples were provided by an official sensory panel and used to build and compare partial least squares regressions (PLSR) with the excitation-emission matrix. Both PARAFAC scores and two-way unfolded data led to successful PLSR. The most relevant PARAFAC scores agreed with virgin olive oil phenolic spectra, evidencing that EEFS would be the fit-for-purpose screening tool to support the sensory panel.

Geographical authentication of virgin olive oil by GC-MS sesquiterpene hydrocarbon fingerprint: Verifying EU and single country label-declaration.

According to the last report from the European Union (EU) Food Fraud Network, olive oil tops the list of the most notified products. Current EU regulation states geographical origin as mandatory for virgin olive oils, even though an official analytical method is still lacking. Verifying the compliance of label-declared EU oils should be addressed with the highest priority level. Hence, the present work tackles this issue by developing a classification model (PLS-DA) based on the sesquiterpene hydrocarbon fingerprint of 400 samples obtained by HS-SPME-GC-MS to discriminate between EU and non-EU olive oils, obtaining an 89.6% of correct classification for the external validation (three iterations), with a sensitivity of 0.81 and a specificity of 0.95. Subsequently, multi-class discrimination models for EU and non-EU countries were developed and externally validated (with three different validation sets) with successful results (average of 92.2% of correct classification for EU and 96.0% for non-EU countries).

Stepwise strategy based on 1H-NMR fingerprinting in combination with chemometrics to determine the content of vegetable oils in olive oil mixtures.

1H NMR fingerprinting of edible oils and a set of multivariate classification and regression models organised in a decision tree is proposed as a stepwise strategy to assure the authenticity and traceability of olive oils and their declared blends with other vegetable oils (VOs). Oils of the 'virgin olive oil' and 'olive oil' categories and their mixtures with the most common VOs, i.e. sunflower, high oleic sunflower, hazelnut, avocado, soybean, corn, refined palm olein and desterolized high oleic sunflower oils, were studied. Partial least squares (PLS) discriminant analysis provided stable and robust binary classification models to identify the olive oil type and the VO in the blend. PLS regression afforded models with excellent precisions and acceptable accuracies to determine the percentage of VO in the mixture. The satisfactory performance of this approach, tested with blind samples, confirm its potential to support regulations and control bodies.

Methods to determine the quality of acid oils and fatty acid distillates used in animal feeding.

Acid oils and fatty acid distillates are by-products from the refining of edible oils and fats. They are used as feed ingredients, but their highly variable composition sometimes affects the productive parameters of the animals. Thus, their quality control and standardization are necessary. The official methods recommended for crude and refined fats and oils must be modified to give reliable results when applied to acid oils and fatty acid distillates. This article summarizes the drawbacks that were encountered during the setup of the analytical methods and how were they overcome by adapting the methods to these type of fat samples. Some methods such as the determinations of fatty acid composition, tocopherol and tocotrienol content, unsaponifiable matter, acidity and peroxide value had to be minimally adapted. However, others such as the determinations of moisture and volatile matter, insoluble impurities, lipid classes and p-anisidine value showed important drawbacks that required a more significant adaptation.•All the analytical methods have been successfully applied to acid oils and fatty acid distillates.•A detailed description of the sample preparation for analysis and applied analytical methods is provided as a compendium of methods in the supplementary material.•These methods will be extremely useful to improve the quality control of these heterogeneous feed ingredients.

Lactobacillus fermentum CECT5716 supplementation in rats during pregnancy and lactation affects mammary milk composition.

Lactobacillus fermentum CECT5716 has shown immunomodulatory action and reduction of infections; therefore, it is suggested to be appropriate for use in early life. The present study aimed to assess the effects of the supplementation of L. fermentum CECT5716 in rats during gestation and lactation periods on the composition of some mammary milk components such as microbiota, fatty acid (FA) profile, and immunoglobulins. Wistar rats were supplemented by oral gavage with 1010 cfu/d of Lactobacillus fermentum CECT5716 (n = 6) or vehicle (n = 6) for 5 wk, comprising the 3 wk of gestation and the first 2 wk of lactation. At the end of the intervention, milk, mammary glands, and cecal contents were obtained for the tracking of the probiotic strain by nested PCR-quantitative PCR. Additionally, milk samples were used for the analysis of microbiota by 16S rRNA sequencing, FA by gas chromatography-flame ionization detector, and immunoglobulin by Luminex (Luminex Corporation, Austin, TX). Although L. fermentum CECT5716 administration did not modify the overall composition of milk microbiota, the strain was detected in 50% of the milk samples of rats supplemented with the probiotic. Moreover, probiotic administration induced beneficial changes in the FA composition of milk by increasing total PUFA, including linoleic and α-linolenic acids, and decreasing the proportion of palmitic acid. Finally, the milk of the rats treated with the probiotic showed a 2-fold increase of IgA levels. The supplementation with L. fermentum CECT5716 during pregnancy and lactation periods improved the milk composition of FA and immunoglobulins. These effects were not linked to the presence of the strain in milk, thus suggesting that the mechanism is connected to intestinal compartment. These findings provide novel insight into a potential new approach for infants to benefit from better nutrition, development of a healthy immune system and microbiota, and protection from gastrointestinal infections.

Oxidative stability of a heme iron-fortified bakery product: Effectiveness of ascorbyl palmitate and co-spray-drying of heme iron with calcium caseinate.

Fortification of food products with iron is a common strategy to prevent or overcome iron deficiency. However, any form of iron is a pro-oxidant and its addition will cause off-flavours and reduce a product's shelf life. A highly bioavailable heme iron ingredient was selected to fortify a chocolate cream used to fill sandwich-type cookies. Two different strategies were assessed for avoiding the heme iron catalytic effect on lipid oxidation: ascorbyl palmitate addition and co-spray-drying of heme iron with calcium caseinate. Oxidation development and sensory acceptability were monitored in the cookies over one-year of storage at room temperature in the dark. The addition of ascorbyl palmitate provided protection against oxidation and loss of tocopherols and tocotrienols during the preparation of cookies. In general, ascorbyl palmitate, either alone or in combination with the co-spray-dried heme iron, prevented primary oxidation and hexanal formation during storage. The combination of both strategies resulted in cookies that were acceptable from a sensory point of view after 1year of storage.

Discrimination of pulp oil and kernel oil from pequi (Caryocar brasiliense) by fatty acid methyl esters fingerprinting, using GC-FID and multivariate analysis.

Pequi is an oleaginous fruit whose edible oil is composed mainly by saturated and monounsaturated fatty acids. The biological and nutritional properties of pequi oil are dependent on its composition, which can change according to the oil source (pulp or kernel). There is little data in the scientific literature concerning the differences between the compositions of pequi kernel and pulp oils. Therefore, in this study, different pequi genotypes were evaluated to determine the fatty acid composition of pulp and kernel oils. PCA and PLS-DA were applied to develop a model to distinguish these oils. For all evaluated genotypes, the major fatty acids of both pulp and kernel oils were oleic and palmitic acids. Despite the apparent similarity between the analyzed samples, it was possible to discriminate pulp and kernel oils by means of their fatty acid composition using chemometrics, as well as the unique pequi genotype without endocarp spines (CPAC-PQ-SE-06).

Authentication of geographical origin of palm oil by chromatographic fingerprinting of triacylglycerols and partial least square-discriminant analysis.

Main goals of the present work were to develop authentication models based on liquid and gas chromatographic fingerprinting of triacylglycerols (TAGs) from palm oil of different geographical origins in order to compare them. For this purpose, a set of palm oil samples were collected from different continents: South eastern Asia, Africa and South America. For the analysis of the information in these fingerprint profiles, a pattern recognition technique such as partial least square discriminant analysis (PLS-DA) was applied to discriminate the geographical origin of these oils, at continent level. The liquid chromatography, coupled to a charged aerosol detector, (HPLC-CAD) TAGs separation was optimized in terms of mobile phase composition and by means of a solid silica core column. The gas chromatographic method with a mass spectrometer was applied under high temperature (HTGC-MS) in order to analyze the intact TAGs. Satisfactory chromatographic resolution within a short total analysis time was achieved with both chromatographic approaches and without any prior sample treatment. The rates of successful in prediction of the geographical origin of the 85 samples varied between 70% and 100%.

Moderately oxidized oils and dietary zinc and α-tocopheryl acetate supplementation: effects on the oxidative stability of rabbit plasma, liver, and meat.

The aim of this study was to assess the alterations in plasma, liver, and meat oxidative stability and α-tocopherol content when moderately oxidized sunflower oils were added to feeds and when feeds were supplemented with α-tocopheryl acetate (100 mg/kg) and Zn (200 mg/kg). The effects of cooking the meat and its subsequent refrigeration were also studied. When the content of primary oxidation compounds of the oil was high, rabbit plasma, liver, and meat α-tocopherol content was reduced and meat susceptibility to oxidation increased. The addition of oil with a high content of secondary oxidation compounds (oil heated at 140 °C, 31 h) to feed also led to an increase in meat susceptibility to oxidation, although it presented an α-tocopherol content similar to that of nonheated oil. Feed supplementation with α-tocopheryl acetate increased tissue α-tocopherol content and improved the oxidative stability of liver and meat. However, in the latter, it was less effective when oil heated at 55 °C was added.

Dietary strategies to improve nutritional value, oxidative stability, and sensory properties of poultry products.

Consumers demand both safer and more nutritious food products exempt of non-natural origin preservatives or other food additives. In this frame, products with lower fat content and/or a higher ratio in unsaturated fatty acids, especially n-3 fatty acids, are desired because these lipids can help prevent the development of cardiovascular and inflammatory pathologies. The intake of meat products is of interest because they are an excellent source of vitamins and minerals. In addition, the shelf-life of meat products can be extended by the presence of natural antioxidants coming from different sources such as plant extracts. Therefore, different strategies have been studied to improve the nutritional value, oxidative stability, and sensory characteristics of meat products and eggs through different mineral and natural dietary supplements. In comparison to other strategies, dietary supplements present the advantage that first the living animals may efficiently distribute the compounds throughout the tissues and second, the dietary supplementation is safer because the resulting enriched meat products and eggs ensure tolerable amounts in humans. Poultry meats and eggs are widely consumed and their fatty acid profile and tocopherol content can be easily modified through different dietary strategies thus being excellent models to improve their nutritional value and oxidative stability.

Influence of different dietary doses of n-3- or n-6-rich vegetable fats and alpha-tocopheryl acetate supplementation on raw and cooked rabbit meat composition and oxidative stability.

This study evaluates the effects of replacing beef tallow added to rabbit feeds (3% w/w) by different doses (0%, 1.5% and 3% w/w) of n-6- or n-3-rich vegetable fat sources (sunflower and linseed oil, respectively) and alpha-tocopheryl acetate supplementation (0 and 100 mg/kg) on the fatty acid composition, alpha-tocopherol content, and oxidation levels [assessed by analyzing thiobarbituric acid (TBA) and lipid hydroperoxide values] in rabbit meat. We also measured these parameters after cooking and refrigerated storage of cooked rabbit meat. Both dietary alpha-tocopheryl acetate supplementation and the dose and source of fat added to feeds influenced meat fatty acid composition, modifying the n-6/n-3 ratio, which was more nutritionally favorable when linseed oil was used. Furthermore, the addition of linseed oil and the supplementation with alpha-tocopheryl acetate enhanced long-chain PUFA biosynthesis. However, the addition of 3% linseed oil increased meat oxidation, and although it was reduced by dietary supplementation with alpha-tocopheryl acetate in raw meat, this reduction was not as effective after cooking. Therefore, dietary supplementation with 1.5% linseed oil plus 1.5% beef tallow and with alpha-tocopheryl acetate would be recommended to improve the nutritional quality of rabbit meat.

Lack of effect of oral supplementation with antioxidants on cholesterol oxidation product concentration of human plasma, as revealed by an improved gas chromatography method.

A gas chromatographic method was successfully applied to determine cholesterol oxidation products (COPs) in human plasma. The linearity, precision, recovery and sensitivity of the method were determined. Oral supplementation with a combination of vitamin E (800 IU), C (1 g) and beta-carotene (24 mg), given for 21 days to 21 patients, did not significantly decrease plasma COP content. No correlations (n = 26) were found between initial plasma COP content and the following parameters: age, body mass index, plasma content of alpha-tocopherol, cholesterol, high-density lipoprotein cholesterol and triglycerides, and fat, natural antioxidant and oxidized lipid intake. Differences in plasma COP content between type 2 diabetic (n = 6) and nondiabetic (n = 20) patients were not statistically significant. The results from this study lead us to hypothesize that the nonenzymatic oxidation of cholesterol in plasma is negligible compared to COPs originating from the diet. This article also includes a comprehensive review of the drawbacks of the analytical methods of COP determination in plasma and serum.