Search Results (53)

Micronutrient deficiencies, particularly of vitamins A, D₃, and folic acid, remain a significant global health challenge despite established dietary recommendations. This study proposes a novel fortification strategy using advanced emulsion technology to enrich extra-virgin olive oil (EVOO) with these essential micronutrients. Water-in-oil (W/O) and double oil-in-water-in-oil (O/W/O) emulsions were designed to enable the simultaneous encapsulation of lipophilic (A and D₃) and hydrophilic (folic acid) vitamins within a single functional food matrix. Vitamin concentrations were quantified using high-performance liquid chromatography (HPLC) coupled with a photodiode detector (PDA) to evaluate retention during processing. Bioaccessibility was assessed by subjecting vitamin-enriched emulsions to a standardized in vitro digestion model simulating gastrointestinal conditions. Results showed significantly higher incorporation efficiency in the O/W/O system compared to conventional W/O emulsions, regardless of the physicochemical properties of the vitamins. Both lipophilic (A and D₃) and hydrophilic (folic acid) compounds exhibited a satisfactory retention, highlighting the versatility of the double-emulsion approach. This study represents the first report of simple and multiple oil-continuous emulsions that simultaneously incorporate vitamins A, D₃, and folic acid, providing preliminary evidence of their stability and gastrointestinal release under simulated digestion conditions. Full article

The excessive use of phytosanitary products represents a growing concern, due to their persistence and potential environmental and toxicological impacts. Among these compounds, glyphosate, a glycine-derived chemical marketed as a broad-spectrum herbicide, is one of the most widely used pesticides worldwide. Breast milk is a complex biological matrix that can reflect environmental exposure, making it highly suitable for assessing glyphosate contamination. This study aimed to demonstrate a screening method to determine glyphosate concentrations in the breast milk of 100 postpartum women residing in Tupã, São Paulo, Brazil—90 in urban areas and 10 in rural areas—using high-performance liquid chromatography (HPLC) for rapid detection. By validation parameters, it was possible to verify, through the correlation coefficient (r), that the method is linear within the working range; the LD was 0.14 mg/L and the LQ was 0.43 mg/L. The recovery obtained by standard sample fortification was 92%. All analyzed samples presented detectable levels of glyphosate, indicating consistent exposure patterns and suggesting relevant environmental contamination routes in the region. These findings provide evidence of glyphosate presence in human milk and reinforce the importance of continuous monitoring strategies and preventive public health measures aimed at reducing exposure to agricultural contaminants. Full article

Port wine production involves the addition of grape spirit to halt fermentation and retain natural sweetness. This spirit, produced by distilling wine and its by-products, must comply with legal standards, including a mandatory sensory assessment. Because grape spirit influences Port wine’s volatile composition, this study investigated the odour-active compounds present in several grape spirits intended for fortification. Volatile compounds were extracted by liquid–liquid extraction, concentrated, and analysed using gas chromatography–olfactometry (GC-O) and gas chromatography–mass spectrometry (GC-MS). In GC-O, based on frequency detection, a panel of assessors sniffed the extracts to determine the presence of aroma compounds. The results revealed a wide range of odour-active compounds in grape spirits, belonging to several chemical families such as esters, alcohols, terpenic compounds and acids. These compounds exhibited both pleasant aromas, such as fruity, floral and caramel notes as well as undesirable ones like cheese and foot odour. Most of these compounds originate from the fermentation process and are also found in other unaged distilled beverages, including young Cognac, Calvados and fruit spirits. This research highlights the aromatic complexity of grape spirits and, for the first time, determined the aroma thresholds for 25 of 36 the compounds studied at an ethanol content of 20%. Full article

Astaxanthin, a potent antioxidant, has attracted growing interest for its applications in the food, pharmaceutical, and cosmetic industries. This study aims to optimize the green extraction of astaxanthin from shrimp (Parapenaeus longirostris) by-products using ultrasound-assisted extraction (UAE) with extra virgin olive oil (EVOO) as a sustainable solvent, and explore its application in trahana fortification, a traditional Greek fermented cereal-based product. Response Surface Methodology (RSM) was applied to optimize astaxanthin extraction conditions (extraction time, liquid-to-solid (L/S) ratio, and ultrasound amplitude). Fatty acid analysis was performed with gas chromatography (GC-FID), and sensory analysis was conducted using a 7-point hedonic scale for sensory attributes. The optimal UAE conditions for astaxanthin, determined by RSM, were 228 min extraction time, a 65:1 liquid-to-solid ratio, and 41% ultrasound amplitude, predicting 83.50 μg astaxanthin/g by-product. At the optimal conditions, the experimentally obtained yield of 76.75 ± 1.17 μg astaxanthin/g by-product fell within the 95% confidence interval of the predicted value. The enriched trahanas retained nutritionally relevant levels after cooking (46.35 ± 0.60 μg astaxanthin per 60 g serving). Accelerated storage testing at 65 °C for six days was used to assess the thermal stability of astaxanthin in enriched trahanas. Based on first-order degradation kinetics and Arrhenius-based extrapolation of literature-derived activation energy values, astaxanthin retention above 80% at 25 °C was estimated to be maintained for approximately 27–51 days. Thereafter, progressive degradation is expected, with the estimated half-life ranging from 85 to 159 days. GC-FID analysis revealed favorable incorporation of bioactive lipids, including omega-3 fatty acids (EPA and DHA). Sensory evaluation demonstrated enhanced consumer acceptability, with enriched samples scoring significantly higher in appearance, aroma, and overall acceptance compared to traditional trahanas. These findings highlight UAE as an efficient and environmentally friendly strategy for recovering astaxanthin from seafood by-products and for developing functional cereal-based foods that align with sustainability. This work demonstrates the effective use of extra virgin olive oil as a green extraction solvent that also serves as a nutritional carrier, enabling the enrichment of trahanas with astaxanthin. The approach ensures both nutritional stability and consumer acceptability, providing a practical pathway for the development of sustainable, functional cereal-based foods. Full article

As rapidly developing consumer products, cosmetics confront challenges regarding safety, especially hazardous ingredients, like sex hormones. Prolonged exposure to trace sex hormones in cosmetics can inflict immeasurable damage to human health. To accurately detect the trace amounts of sex hormones in cosmetics, a reliable method was developed and validated using ultra-high performance liquid chromatography–mass spectrometry (UHPLC-MS/MS) with magnetic solid-phase extraction (MSPE) and isotope-labeled internal standards (IL-ISs). The conditions of sample pretreatment, chromatography, and mass parameters were systemically investigated. In the MSPE procedure, the commercial Fe₃O₄@HLB magnetic material was employed for sample pretreatment, which was beneficial for operation, as well as sample purification and analyte enrichment. The utilization of IL-ISs compensated for potential matrix effects and losses during sample preparation, thereby improving precision and accuracy. Based on the proposed MSPE technology, UHPLC-MS/MS can address the qualitative and quantitative analysis needs for target analytes in complex cosmetic matrices. At three fortification levels, recoveries were in the range of 71.7–116.2%, with a relative standard deviation (RSD) ranging from 1.6% to 8.3%. Furthermore, based on the method proposed here, a total of 116 batches of cosmetics were analyzed, and trace progestins and estrogens were discovered in 10 samples. The MSPE method, coupled with UHPLC-MS/MS using IL-ISs, was convenient, efficient, and feasible for detecting trace amounts of sex hormones in cosmetics. The method scored 0.66 (out of 1) on the AGREE metric, confirming its green profile. Based on the detected concentrations, a preliminary safety evaluation was performed to assess the potential health risks of residual progesterone in hair loss prevention cosmetics by calculating the margin of safety (MoS). Full article

Bioprocessing grape pomace (GP) presents a sustainable solution aligned with circular economic principles and transforms it into valuable functional ingredients for baked products. This review (2020–2025) synthesizes enzymatic and microbial strategies that modify the fiber–phenolic matrix and improve dough performance. Enzyme-assisted extraction, alone or combined with ultrasound or pressurized liquids, increases extractable polyphenols and antioxidant capacity in GP fractions used as flour substitutions or pre-ferments. Fungal solid-state and lactic fermentations liberate bound phenolic compounds and generate acids and exopolysaccharides. Among these routes, enzyme-assisted extraction and lactic sourdough-type fermentations currently appear the most compatible with bakery-scale implementation, offering substantial phenolic enrichment while relying on relatively simple, food-grade equipment. In current bakery applications, GP is mainly used as crude grape pomace powder, which typically shows higher total phenolics and antioxidant capacity. Moreover, in several models it lowers starch hydrolysis and predicted glycemic index. The practical substitution rate is between 5 and 10% of flour, which balances nutritional gains with processing disadvantages. These can be mitigated by fractionation toward soluble dietary fiber or co-fortification with flours rich in protein and fiber. An additional benefit of these methods includes reduced mycotoxin bioaccessibility in vitro. A key evidence gap is the absence of standardized comparisons between raw and bioprocessed GP in identical formulations. Overall, GP emerges as a promising ingredient for bakery products, while the added technological and nutritional value of bioprocessing remains to be quantified. Full article

Objectives: This study aimed to develop and validate a sensitive and reliable liquid chromatography–tandem mass spectrometry (LC-MS/MS) method for the quantification of flualprazolam and isotonitazene in serum samples to address critical gaps in forensic and clinical toxicology. Materials and Methods: A single-center validation study was conducted using serum samples spiked with analyte standards. Analytical parameters, including linearity, precision, recovery, the limit of detection (LOD), and the limit of quantification (LOQ), were evaluated in accordance with international guidelines. The LC-MS/MS method employed a Shimadzu Triple Quadrupole™ MS 8045 system with solid-phase extraction (SPE) for sample preparation. Results: The method exhibited high linearity for flualprazolam (r² = 0.997) and isotonitazene (r² = 0.999) over a concentration range of 1–100 ng/mL. The LODs were determined as 0.608 ng/mL and 0.192 ng/mL, and the LOQs were 1.842 ng/mL and 0.584 ng/mL for flualprazolam and isotonitazene, respectively. Recovery tests yielded results within the acceptable range of 70–120%. Flualprazolam demonstrated recovery rates of 98.0% and 97.0% at theoretical concentrations of 10 ng/mL and 50 ng/mL, respectively. In contrast, the isotonitazene recovery rates were slightly lower, measuring 75.5% at 10 ng/mL and 71.9% at 50 ng/mL, suggesting minor matrix effects that could influence its quantification. Precision analysis, including both repeatability and reproducibility, highlighted the reliability of the method. The %RSD values for flualprazolam were consistently below 7.07%, with mean concentrations closely aligning with theoretical values across fortification levels. For isotonitazene, the %RSD values remained below 6.24%, although recoveries at higher concentrations indicated potential challenges in matrix interaction. Conclusions: This validated LC-MS/MS method offers high sensitivity, precision, and recovery for detecting flualprazolam and isotonitazene in serum, filling a critical need in toxicological investigations. Further validation in other biological matrices is recommended to broaden its applicability. Full article

Potassium iodate and potassium iodide are commonly fortified in iodized table salt, which must be continuously monitored to maintain quality. Our study reported an optimized detection method for total iodine in iodized table salt using 0.5 M sodium bisulfite as the reducing agent. The iodized table salt (0.5 g) was dissolved in 0.5 M sodium bisulfite solution prior to injection in ultra-high-performance liquid chromatography (UHPLC) coupled with a diode array detector using a weak anion-exchange column (2.1 mm × 150 mm, 5 μm). Iodide was eluted at 9.92 ± 0.06 min (λ = 223 nm) when an isocratic mobile phase of 1:1 (v/v) methanol/120 mM phosphate buffer mixed with tetrasodium pyrophosphate (pH 3.0) was running at 0.20 mL/min (15 min). Iodide was detected as total iodine from 10.0 to 50.0 mg/kg with a limit of detection (LOD) of 1.2 mg/kg and a limit of quantification (LOQ) of 3.7 mg/kg. The method was validated with relative standard deviations (RSDs) of 4.2%, 0.4%, 1.6%, and 0.8% for accuracy, repeatability, intermediate precision, and robustness, respectively. The determination of total iodine was successful on six (6) samples (n = 3), which recovered 87.2–106.9% of iodate and iodide spike. Thus, this study provides a validated protocol for the determination of total iodine in iodized table salt using 0.5 M sodium bisulfite. Full article

Background/Objectives: The dietary changes experienced by residents in long-term care facilities (LTCFs) following an earthquake are poorly understood. This study aimed to examine variations in nutritional status among residents of an Integrated Facility for Medical and Long-term Care (IFMLC), a particular type of Japanese LTCF, after the 2024 Noto Peninsula Earthquake. Methods: This descriptive study was conducted at the single IFMLC. A total of 115 residents living at the facility on 1 January 2024, at the time of the earthquake, were recruited for the study. The focus was the body weight and skeletal muscle mass changes observed before and after the earthquake. The observation period lasted for three months following the earthquake. Results: Water outage persisted for over a month, making dishwashing impossible and leading to an extended reliance on disposable dishes with limited capacity. This situation consequently reduced the variety and volume of meal options and overall energy intake meals. Residents’ body weight significantly decreased 3 months after the earthquake, and the prevalence of weight loss and skeletal muscle mass loss was particularly high in residents with normal swallowing function. To address nutritional deficiencies post-earthquake, the registered dietitian enhanced energy sufficiency through food fortification, oral nutritional supplements, and pre-prepared ready-to-hang liquid formulas. Conclusions: To prevent further weight and skeletal muscle mass reduction among IFMLC residents, providing ample water, and a disaster manual that can be used even with limited resources is essential. Furthermore, preparing for disasters by stockpiling foods and implementing strategies to enhance energy sufficiency is crucial. Full article

In recent decades, there has been growing interest in the fortification of food products with antioxidants and phenolics derived from plant by-products. The present study focused on the production of a plant-based beverage enriched with hazelnut cuticle extract to characterize its antioxidant content, phenolic profile, and organoleptic characteristics. Liquid chromatography-mass spectrometry (LC-MS) enabled the identification of key polyphenols in hazelnut cuticles, including catechin, epicatechin, and quercetin derivatives, guiding the selection of a biocompatible Natural Deep Eutectic Solvent (NADES) composed of choline chloride and lactic acid for efficient extraction. The obtained phytochemical profile of the extract revealed a high concentration of bioactive compounds, with a Total Phenolic Content of 160.88 ± 14.27 mg GAE/g and Antioxidant Power measured by DPPH of 5848.2 ± 11.3 μmol TE/g. The bioaccessibility of phenolics in the fortified hazelnut-based beverage was determined after in vitro digestion, reaching a value of 89.7%, indicating excellent release and stability during digestion. Organoleptic evaluation revealed high sensory acceptability, with aftertaste scoring 3.61 ± 0.4 respect the 3.94 ± 1.3 result of reference milk, on a 5-point scale. In conclusion, this study demonstrates the potential for sustainable valorization of hazelnut cuticles, through their incorporation as NADES extracts in plant-based milk, providing an innovative solution to reduce food waste while catering to consumer demand for nutritionally enriched and eco-friendly products. Full article

The in situ fortification of vitamin B12 (VB12) in foods through fermentation is an effective strategy to address the deficiency of this micronutrient, and precise monitoring of VB12 production is crucial for developing VB12-fortified functional foods. Liquid chromatography–tandem mass spectrometry (LC-MS/MS) is advantageous for analyzing trace substances in food due to its high sensitivity. In the present study, an LC-MS/MS method capable of rapidly and accurately quantifying three active forms of VB12, namely adenosylcobalamin (AdoCbl), methylcobalamin (MeCbl), hydroxocobalamin (OHCbl), in 8 min were developed. Meanwhile, the quantitative result of this method is not affected by pseudo-VB12 because the selected ion channels include fragments of active VB12. Maintaining light-shielding during extraction and purification is essential, as light exposure during the process can decrease the content of detected VB12 by about 30%. At last, the developed method was applied for the determination of VB12 in fermented rice bran and the cell mass of Propionibacterium freudenreichii. The results showed that AdoCbl was the predominant form of VB12 during fermentation, and the addition of cobalt did not influence the proportions of the three VB12 types. The present study reported a rapid and accurate method for the simultaneous determination of three active forms of VB12, which can effectively support the development of foods with VB12 fortification. Full article

This study aimed to enhance the nutritional value of jellies by fortification with polyphenol extracts derived from Pinus sylvestris L. shoots at various maturation stages. Pinus sylvestris L., a coniferous species, is widely used in traditional medicine and functional foods due to its antioxidant, anti-inflammatory, and antimicrobial properties. Its needles, bark, and shoots are commonly used to extract bioactive compounds such as phenolic acids and flavonoids. In the current study, extracts were derived from young shoots collected directly from natural forest environments and processed using a decoction method to preserve bioactive compounds. The novel jelly formulations were prepared using pine shoots harvested at three maturity stages: stage I (4 cm), stage II (8 cm), and stage III (12 cm). All determinations were conducted both on the pure decoction extracts and the jelly samples to ensure a comprehensive analysis. High-performance liquid chromatography coupled with electrospray ionization mass spectrometry (HPLC-ESI-MS) allowed the identification of eight phenolic acids and six flavonoids in the samples. Significant differences were observed between the pine shoot extracts and jellies at different development stages. Notably, stage II exhibited optimal polyphenol content (312.2 mg GAE/100 g), DPPH free radical scavenging activity (94.9%), dry matter content (79.5%), and acidity (0.79% citric acid/g). A similar pattern emerged in the jelly samples (jelly2 (pine decoction stage II) > jelly1 (pine decoction stage I) > jelly3 (pine decoction stage III)). All extracts demonstrated antioxidant potential in DPPH free radical quenching assays. FTIR analysis evaluated structural changes in phenolic compounds during jelly formulation, focusing on key absorption bands at 1600 cm⁻¹ (C=C stretching) and 3336 cm⁻¹ (-OH stretching) using a Shimadzu IR Prestige-21 spectrophotometer. Compared to extracts, jellies showed diminished band intensities, indicating thermal degradation of phenolic compounds during processing. This aligns with observed reductions in antioxidant capacity and phenolic content, suggesting partial destabilization of these bioactive compounds. However, their integration into the jelly matrix highlights the potential for functional applications. The textural attributes of jellies were also assessed, and differences were attributed to the changes in acidity and moisture content of the pine shoots during maturation. Pine shoot extracts at specific maturation stages are valuable sources of antioxidant and polyphenol compounds and were successfully employed in functional applications belonging to the food or nutraceutical industry. Full article

Background/Objectives: The widespread use of antibiotics, which wastewater treatment plants (WWTPs) cannot fully remove, in human and veterinary medicine leads to their release into wastewater, resulting in the contamination of aquatic environments. Bivalves can accumulate these antibiotics, posing a risk to shellfish consumers, including potential antimicrobial resistance. This study aimed to assess how three cooking methods—marinating, steaming, and grilling—affect the concentration of 33 different antibiotics in bivalves fortified at the level of maximum residue limit (MRL) and twice the MRL (2MRL). Results: The data show the percentage of antibiotic remaining after cooking: 100% indicates stability or no reduction; values above 100% show an increase in concentration, and values below 100% reflect a decrease in antibiotic concentration. In general, all culinary procedures removed part of the added antibiotics. However, the most effective method was marinating (47%), followed by steaming (60%) and finally grilling (92%). It was also found that, overall, the fortification level, MRL or 2MRL, did not impact antibiotic removal in each cooking method. Moreover, different antibiotics’ classes presented diverse removals when cooked, ranging between 0% for penicillins and 73% for sulphonamides. Furthermore, the results showed a great diversity of responses to cooking within some antibiotic classes. Methods: After cooking, the analysis was based on solid–liquid extraction followed by liquid chromatography–quadrupole time-of-flight mass spectrometry (UHPLC-ToF-MS). Conclusions: The ongoing monitoring of antibiotic levels is essential, and further research is needed to understand how cooking affects these substances and their metabolites. This will help assess the real risk to consumers and guide risk-mitigation measures. Full article

Along the food production chain of animal, fish, and vegetable products, a huge amount of by-products are generated every year. Major nutritional, financial, and environmental advantages can be achieved by transforming them into functional ingredients for food formulation and fortification. In this review, we investigated various conventional and emerging treatments recently employed to obtain functional ingredients rich in proteins, fibers, and bioactive compounds from vegetables, fish, meat, and dairy by-products. The optimal enrichment level in food as well as the nutritional, techno-functional, and sensory properties of the final food were also discussed. Novel technologies such as ultrasounds, microwaves, and high pressure have been successfully adopted to enhance the extraction of target compounds. The functional ingredients, added both in liquid or powder form, were able to improve the nutritional quality and antioxidant potential of food, although high levels of fortification may cause undesired changes in texture and flavor. This review provides important considerations for further industrial scale-up. Full article

Vitamin D₃ deficiency is a global phenomenon, which can be managed with supplementation and food fortification. However, vitamin D₃ bioaccessibility may depend on factors such as matrix composition and interactions throughout the gastrointestinal (GI) tract. This research focused on the effect of different matrices on vitamin D₃ content during digestion, as well as the effect of pH on its bioaccessibility. The INFOGEST protocol was employed to simulate digestion. Three different types of commercial supplements, two foods naturally rich in vitamin D₃, and three fortified foods were investigated. High-Performance Liquid Chromatography was used to determine the initial vitamin D₃ content in the supplements and foods, as well as after each digestion stage. The results indicate that the foods exhibited higher bioaccessibility indices compared to the supplements and a higher percentage retention at the end of the gastric phase. The pH study revealed a positive correlation between an increased gastric pH and the corresponding content of vitamin D₃. Interestingly, exposing the matrix to a low pH during the gastric phase resulted in an increased intestinal content of D₃. Vitamin D₃ is more bioaccessible from foods than supplements, and its bioaccessibility is susceptible to changes in gastric pH. Fasting conditions (i.e., gastric pH = 1) enhance the vitamin’s bioaccessibility. Full article