Search Results (107)

Rice (Oryza sativa L.) is a vital staple food and an important source of energy and macro- and micronutrients for billions of people. However, rice can accumulate undesirable levels of toxic trace elements, especially inorganic arsenic, which may pose a health risk. This study aimed to determine the concentrations of 29 essential and toxic elements and the fractions of four As species in 58 rice samples purchased in Croatian supermarkets. In addition, the influence of rice variety, cultivation methods, and origin on the composition of trace elements was analysed. The elements were quantified using inductively coupled plasma mass spectrometry (ICP-MS), and As species were quantified using high-performance liquid chromatography (HPLC) coupled with ICP-MS. Organic brown rice had higher concentrations of essential trace elements (Se, Zn, Cu, Fe, Mn, Co, Cr) than white rice, with organic brown rice containing more essential elements than conventionally grown rice. The average total arsenic concentration (tAs) across all samples was 142 ± 57 µg/kg, with brown, conventionally grown rice containing a higher amount. Arsenite was the predominant arsenic species. Regional differences in As and Se concentrations were observed. These results emphasize the complex relationship between trace elements in rice and their potential impacts on health. Full article

Three types of solid waste are produced during beer fermentation: spent grain, hot trub, and residual yeast. While the first is used as livestock feed, the seconds has not yet found any real reapplication in the field of circular economy. The aim of this work is to study and characterize these two brewing wastes, i.e., hot trub and residual yeast, to evaluate their potential reuse in the agricultural field. Samples from top-fermented and bottom-fermented beers were chemically investigated. Initially, the safety was assessed via multi-detection analysis of 57 mycotoxins, and all samples were deemed safe. Subsequently, the chemical and elemental composition was examined via ICP-MS and microanalysis, along with phenolic compounds and antioxidant activity via HPLC and spectrophotometric determinations, to achieve a thorough characterization of these waste samples. The C/N ratio of residual yeast from top-fermented beer and hot trub of the bottom-fermented one were near the optimal one (10:1). This research marks an initial step towards repurposing brewery waste materials as fertilizers. The subsequent steps will involve the formulation and field trials. Full article

Objectives: The aim of this study was to provide a comprehensive overview of the nutritional and toxicological aspects of different forms of blueberry products (fresh blueberries, dried blueberries, supplements and herbal teas). Methods: Twelve aglycone and glycoside polyphenolic compounds, such as stilbenoids (resveratrol, astringin), flavonols (quercetin, rutin, isoquercitrin, quercitrin, kaempferol), flavanols (catechin, epicatechin), flavanone (hesperitin), flavone (luteolin), and forty chemical elements were analyzed using high-performance liquid chromatography coupled to a mass spectrometer and inductively coupled plasma mass spectrometry. Total phenolic and flavonoid content and antioxidant activity were also evaluated. Results: Different distributions of polyphenolic compounds were observed in the blueberry samples, with quercetin and its derivatives, as well as catechin and epicatechin, present in all samples. High concentrations of Ca, K, Mg and P (10–5800 mg/kg) were detected, followed by Fe and Mn at levels below the allowable limits in foods (425 and 500 mg/kg, respectively). The daily intake of polyphenols was quantified, and the estimated daily intake (EDI) was calculated for sixteen elements (including As, Cd, Cu, Fe, Ni, Pb, V and Zn). Hazard quotients (HQs), hazard index (HI) and cancer risk (CR) were assessed for carcinogenic and non-carcinogenic risks associated with the EDI of these elements in food products for both adults and young consumers. For all samples, HI values were below 1, and CR values were within acceptable limits. Conclusions: The diversity in polyphenolic profiles and elemental content in blueberry-based products was highlighted by this exploratory study. These findings are valuable for understanding the health benefits and risks of blueberry products. Full article

We report on the preparation and characterization of a cost-effective, durable, and reusable macrocomposite, prepared in the form of pellets and designed for the photodegradation of water pollutants, using amoxicillin (AMX) as a model compound. Using the wet impregnation method, kaolin clay and TiO₂-P25 composites were doped with copper (Cu²⁺) and cobalt (Co²⁺). The produced materials were characterized by SEM-EDS, XRD, XRF, textural property analysis, and their potential lixiviation of components by ICP-MS. The photodegradation efficiency under solar irradiation was evaluated by varying the acidity of the medium, the concentration of AMX, and the amount of catalyst. The performance of the recycled photocatalysts was also studied. The photodegradation of AMX was monitored by UV–Vis and UV–Vis/HPLC spectrophotometry. The optimal formulations, Cu (0.1%)/TiO₂ and Co (0.1%)/TiO₂, achieved up to 95% degradation of 5 mg·L⁻¹ AMX in 3 h at pH 5.9, with a catalyst loading of 1 g·L⁻¹. The Cu-doped material showed a slightly faster reaction rate and higher total-organic-carbon removal (80.4%) compared to the Co-doped material (59%) under identical conditions. The same photodegradation intermediates were identified by LC-MS/MS for both doped macrocomposites, and a reaction mechanism is proposed. These macrocomposites showed efficient and consistent recyclability over more than five reuse cycles, showing their potential to be used for antibiotic pollution abatement in water-treatment facilities. Full article

The simultaneous determination of arsenic and mercury species in human urine is critical for clinical diagnostics and therapeutic monitoring because it reduces the costs, time, and consumption of samples. This study proposes a method of utilizing high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) for the concurrent analysis of arsenic and mercury species in urine samples. The separation was performed using a Hepu AR 5 μm C₁₈ (250 × 4.6 mm) column, employing a mobile phase composed of 0.1% L-cysteine, 5 mM NH₄H₂PO₄, and 4 mM tetrabutylammonium hydroxide (TBAH). The samples were diluted with water, and matrix interference was reduced through the application of a kinetic energy discrimination (KED) mode. Calibration curves for four arsenic species and three mercury species exhibited strong linearity within the range of 1–20 μg L⁻¹, with correlation coefficients (r) above 0.999. The limits of detection (LOD) ranged from 0.030 to 0.086 μg L⁻¹, while the limits of quantitation (LOQ) were observed to range from 0.10 to 0.29 μg L⁻¹. The spiking recoveries for all species varied from 87.0% to 110.3%, and the intra-day and inter-day relative standard deviations (RSD) were determined to be 1.1–6.0%, and 0.8–9.2%, respectively. These results indicate that the developed method achieves high precision, accuracy, and suitability for clinical applications, offering valuable insights for the diagnosis and treatment of heavy metal exposure. Full article

This study examines arsenic contamination in the Caplina Basin, Tacna, Peru, focusing on arsenic speciation and associated risks in surface waters. Arsenic concentrations were quantified using inductively coupled plasma mass spectrometry (ICP-MS) and high-performance liquid chromatography (HPLC). Total arsenic levels ranged from 0.0304 mg/L to 0.0730 mg/L across all monitoring points, exceeding the World Health Organization (WHO) limit of 10 µg/L (0.01 mg/L) for drinking water. Arsenite (As(III)), the most toxic and mobile species, reached levels up to 0.0154 mg/L, posing a significant concern at Point 7, characterized by acidic pH (3.82) and high conductivity (1456 µS/cm). Arsenate (As(V)), less toxic but predominant under alkaline conditions, peaked at 0.0260 mg/L at Point 6 (pH 8.42). Organic species such as dimethylarsenic acid (DMA) and monomethylarsenic acid (MMA) were also detected, indicating active methylation processes and anthropogenic influences. The risk assessment revealed carcinogenic risk values ranging from 2.56 × 10⁻⁵ to 6.28 × 10⁻⁵, below the USEPA threshold (1 × 10⁻⁴), but significant for prolonged exposure. Non-carcinogenic hazard quotient (HQ) values ranged from 0.09 to 0.21. These findings highlight severe public health implications and emphasize the urgent need for comprehensive strategies, including continuous monitoring, targeted treatment technologies, and community education, in order to guarantee water quality in vulnerable areas. Full article

This study aimed to investigate the nutritional value and potential for herbal tea production of two species Eryngium. The analysis includes the quantification of lipids, proteins, organic acids (HPLC-MS), sugars (HPLC-MS), phenolic compounds (HPLC-MS-MS), volatile compounds (GC-MS), fatty acids (GC-MS), amino acids (HPLC-MS-MS), some minerals (ICP-MS), total phenolic content, and antioxidant activities of Eryngium billardieri flowers (EBF) and thorns (EBT), as well as Eryngium planum flowers (EPF) and thorns (EPT). The results indicate that EPF and EPT exhibit elevated levels of protein (11.2%) and sugars (224.2 mg/gdw), respectively. Whereas, EBF demonstrates a higher concentration of amino acids (7.13 mg/100 gdw) and total phenolic content (19.25 mg GAE/gdw), which correlates with pronounced antioxidant properties. Oleic acid was notable in E. billardieri, while linoleic and α-linolenic acids were predominant in E. planum. Furthermore, essential minerals such as Fe, Mn, Zn, Mg, K, Ca, and P were also determined. Sensory evaluations by panelists confirmed that tea derived from the studied species possesses favorable taste and flavor profiles, attributed to its rich volatile compounds. These findings highlight the nutritional value of Eryngium species as a functional ingredient in the food industry. Additionally, their antioxidant properties suggest promising uses in pharmaceutical applications. Full article

To fight counterfeits, and to protect the consumer, the interest in certifying the origin of agricultural goods has been growing in recent years. In this context and to increase the accuracy of zoning models, multiple analytical techniques must be combined via a multivariate approach. During the sampling campaign, leaves and fruits (olives or drupes) were collected from multiple orchards and farms. By means of HPLC-DAD, metabolite levels were evaluated and combined with the trace and ultra-trace metal/metalloid levels evaluated by ICP-MS (QqQ). The combined dataset was then used to develop a model for geographical traceability. Furthermore, the mineral content of the soil, evaluated by means of ICP-MS, was correlated with both the mineral content in the leaves and drupes and the metabolomic profiles to further investigate the connection between the orchard’s location and characteristics of the final products. Full article

Understanding the correlation between soil chemical properties and tea quality is essential for the comprehensive management of ancient tea gardens. However, the specific links between these factors in ancient tea gardens remain underexplored. This study analyzes the soil chemical properties of four distinct research regions in Nanhua County to explore their effects on key chemical components in ancient tea garden teas, providing a scientific basis for improving the quality of ancient tea garden teas through soil management. Employing high performance liquid chromatography (HPLC) and inductively coupled plasma mass spectrometry (ICP-MS), the chemical components of tea and the chemical properties of the soil were meticulously quantified. Following these measurements, the integrated fertility index (IFI) and the potential ecological risk index (PERI) were evaluated and correlation analysis was conducted. The results revealed that ancient tea garden tea quality is closely linked to soil chemical properties. Soil’s total nitrogen (TN), total sulfur (TS), and available potassium (AK) negatively correlate with tea’s catechin gallate (CG) component and AK also with polyphenols. Most other soil properties show positive correlations with tea components. The research also evaluated soil heavy metals’ IFI and PERI. IFI varied significantly among regions. Hg’s high pollution index indicates ecological risks; Cd in Xiaochun (XC) region poses a moderate risk. PERI suggests moderate risk for XC and Banpo (BP), with other areas classified as low risk. Implementing reasonable fertilization and soil amelioration measures to enhance soil fertility and ensure adequate supply of key nutrients will improve the quality of ancient tea gardens. At the same time, soil management measures should effectively control heavy metal pollution to ensure the quality and safety of tea products. Insights from this study are crucial for optimizing soil management in ancient tea gardens, potentially improving tea quality and sustainability. Full article

The determination of chemical warfare agents (CWAs) and their toxic degradation products (DPs) has become increasingly important for public and military safety in recent years. We focused on assessing the possibility of the HPLC-ICP-MS analytical technique to verify the provisions of the Chemical Weapons Convention. This technique enables the identification and determination of minimal concentrations (ppt range) of elements in various matrices. This fact is important for the determination of CWAs and other highly harmful compounds, even small amounts of which can have serious consequences for living organisms. We have critically analysed the results of scientific research on the identification and quantitative determination of extremely toxic organophosphorus, organosulfur and organoarsenic CWAs, their derivatives and their degradation products using high-performance liquid chromatography (HPLC) coupled with inductively coupled plasma–mass spectrometry (ICP-MS). Full article

Edible Insects (EIs) are an alternative source of bioactive compounds such as proteins or fatty acids and micronutrients as vitamins or minerals, thus showing potential to replace traditional foodstuffs in an economical and environmentally friendly way. Nonetheless, EIs can accumulate hazardous chemicals such as mycotoxins and heavy metals. The aim of the present study is to determine mycotoxins and heavy metal content in raw insect samples and those resulting products obtained after supercritical fluid extraction (SFE). Insect samples included Acheta domesticus (cricket) meal, Tenebrio molitor (mealworm) meal, Alphitobius diaperinus (buffalo worm), and Locusta migratoria (locust). For this purpose, a QuEChERS method followed by LC-MS/MS analysis was optimized with good results for the analysis of mycotoxins, principally Aflatoxins (AFs), Ochratoxin A (OTA), and Enniatins (ENNs). In contrast, heavy metals (As, Cd, Hg, Pb) were determined by Inductively Coupled Plasma Mass Spectrometry (ICP-MS). The results obtained revealed that Locust was positive for AFG2 at a level of 115.5 μg/kg, and mealworm was only contaminated with OTA at 58.1 μg/kg. Emerging mycotoxins (ENNA, ENNA1, ENNB, and ENNB1) were detected at lower levels < 2.2 µg/Kg. Concerning heavy metals, limits exceeding regulation were detected for Cd in the insect species studied, with levels up to 219 μg/kg, and for Pb in crickets (100.3 μg/kg). Finally, the analysis of the post-extraction solids after SFE processing revealed that heavy metals remained in the resulting SFE cakes, while mycotoxins were detected at negligible levels (up to 1.3 µg/Kg). Full article

Ceratonia siliqua L. is a medicinal plant that has long been used in traditional Moroccan medicine to treat many diseases. This study aimed to assess the impact of the stages of the immature phase of carob pulp (M1, M2, M3, M4, and M5) on phytochemical composition, antioxidant activity, and antidiabetic activity of Ceratonia siliqua L. The identification of the phenolic profile by HPLC-UV/MS-MS and the study of the antidiabetic effect by in silico, in vitro, and in vivo studies were carried out for extracts with high contents of phenolic compounds from immature wild carob pulp from the communes of Timoulit (TM), Bin Elouidane (AW), and Ouaouizerth (TG) in the province of Azilal in the Béni Mellal-Khénifra region. The results revealed a gradual increase in total sugar content over the pulp’s ripening period, reaching a value of 2134 ± 56.23 mg GE/100 g fresh weight (FW) for TG. The three locations showed peak values for total polyphenol content (TPC), total flavonoid content (TFC), and total condensed tannin (TCT) at the M2 stage. AW had the highest concentrations of TPC (3819 ± 226.4 mg GAE/100 g FM), TFC (1034 ± 57.08 mg QE/100 g FM), and TCT (1472 ± 28.46 mg CE/100 g FM). The DPPH assay (7892 ± 296.1 mg TE/100 g FM) and the FRAP assay (278.2 ± 7.85 mg TE/100 g FM) both demonstrated that the TG zone is a highly potent antioxidant zone. In contrast, the AW site exhibited a markedly elevated value of 725.4 ± 103.6 mg TE/100 g FM in the ABTS assay. HPLC-UV-MS/MS analysis showed that the methanolic extracts of immature carob pulp (MEICP) from the three areas contained several different chemical compounds. The most prevalent were 3-O-p-coumaroyl-5-O-caffeoylquinic acid, quercetin 3-methyl ether, gallic acid, and galloylquinic acid. Immature carob pulp extract (ICPE) from AW showed the strongest in vitro inhibition of pancreatic α-amylase (IC₅₀ = 0.405 µg/mL) and TG extracts were most potent against intestinal α-glucosidase (IC₅₀ = 0.063 µg/mL). In vivo, AW, TG, and TM extracts significantly reduced postprandial glycemia in rats, with AW having the greatest effect. These results highlight the antidiabetic potential of ICPE. The 3-O-p-Coumaroyl-5-O-caffeoylquinic acid showed better affinity for α-amylase compared to acarbose and interacted significantly with several amino acid residues of the enzyme. Similarly, this molecule and 3,4-Dicaffeoylquinic acid demonstrated a strong affinity for α-glucosidase, suggesting their potential as natural inhibitors of enzymes involved in carbohydrate metabolism. Most of the compounds are not substrates of P-glycoprotein and exhibited high intestinal absorption. Furthermore, the majority of these compounds did not act as inhibitors or substrates of CYP450 enzymes, reinforcing their suitability for development as oral medications. These results underscore the potential of immature carob pulp as a promising antidiabetic agent. Full article

The current study aims to develop isolation protocols for several contaminants of emerging concern (i.e., microplastics (MPs), polycyclic aromatic hydrocarbons (PAHs), and heavy metals (HMs)) from different commercial brands and raw milk samples and also to quantify and characterize the risks of these contaminants pose to human health. The quantification, shape, color, and chemical composition of MPs were achieved using optical microscopy, micro-Fourier transform infrared spectroscopy, and scanning electron microscopy coupled with energy-dispersive spectroscopy. Based on the MP dimensions highlighted by the aforementioned techniques, it can be stated that their length ranges between tens of micrometers and a few centimeters; plus, the thickness in some cases reaches more than 15 µm, and the structure of the MPs can be mostly described as a fibriform with a glossy/matte aspect. The polymeric structures identified were polyamides, poly(methyl methacrylate), polyurethane, polyester, and polyethylene. Chemical investigations (PAHs and HMs concentrations) were performed by high-performance liquid chromatography with fluorescence detection and inductively coupled plasma mass spectrometry, respectively. The pollution load index (1.091–7.676) and daily intake of MPs for adults (0.021–1.061 n·kg⁻¹·d⁻¹) and children (0.089–4.420 n·kg⁻¹·d⁻¹) were calculated. It can be concluded that the presence of MPs in milk supports the hypothesis that microplastics can act as carriers for other contaminants (HMs and PAHs), thus increasing the threat to health. Full article

The Tibetan medicinal fruit E’seguo originates from two species, Malus toringoides (Rehd.) Hughes and Malus transitoria (Batal.) Schneid, both unique to the Hengduan Mountains. These species are predominantly found in high-altitude regions of Ganzi Prefecture, Sichuan Province, particularly in the Xianshui River and Yalong River basins. Malus toringoides (Rehd.) Hughes is far more abundant in both resource quantity and distribution compared to Malus transitoria (Batal.) Schneid. However, the nutritional and medicinal differences between the two remain unclear, which significantly impacts the development and utilization of E’seguo resources. This study aimed to measure the mineral content, nutritional components, and medicinal properties of E’seguo from 12 different regions of Ganzi Prefecture to explore the quality differences between these two species and across different regions. ICP-MS (Inductively Coupled Plasma Mass Spectrometry) was used to determine the mineral content, ultraviolet-visible spectrophotometry and potentiometric titration to analyze nutritional indicators, and HPLC (High-Performance Liquid Chromatography) to measure the medicinal components L-malic acid and 2-O-β-_D-glucopyranosyl-_L-ascorbic acid (AA-2βG). Results indicate that Malus transitoria (Batal.) Schneid contains higher levels of K, Ca, Zn, Mg, and Cu compared to Malus toringoides (Rehd.) Hughes, which has higher Fe and Mn content. Malus toringoides (Rehd.) Hughes from the Kangding and Litang regions showed the highest mineral content, with mineral elements primarily influencing polysaccharide levels, according to Mantel analysis. Nutritional and medicinal analyses revealed that Malus toringoides (Rehd.) Hughes outperformed Malus transitoria (Batal.) Schneid in all metrics except for the sugar-acid ratio. Given the mineral content and taste, Malus transitoria (Batal.) Schneid is better suited for consumption, while Malus toringoides (Rehd.) Hughes has superior medicinal properties, making it more appropriate for medicinal use. In the Malus transitoria (Batal.) Schneid regions, both Luhuo and Daofu are in the Xianshui River basin, with Daofu County producing the higher quality fruit. Among the nine Malus toringoides (Rehd.) Hughes regions, the M10 (Tuoba Township, Ganzi County) near the Yalong River had the highest overall score, followed by M7 (Yade Township, Luhuo County) and M6 (Keke, Xiala Tuo Town, Luhuo County), both of which are near the Xianshui River. In summary, Malus transitoria (Batal.) Schneid generally has higher mineral content, but Malus toringoides (Rehd.) Hughes has larger fruit and higher medicinal value, making the latter more suitable as a medicinal resource. At the same time, the medicinal quality of Xianshui River fruit was higher in the two watersheds of Malus toringoides (Rehd.) Hughes. Full article

Mercury (Hg) is a toxic element which impacts on biological systems and ecosystems. Because the toxicity of Hg species is highly dependent on their concentration levels and chemical forms, the sensitive identification of the chemical forms of Hg—i.e., Hg speciation—is of major significance in providing meaningful information about the sources of Hg exposure. In this study, a microfluidic-based device made of high-clarity poly(methyl methacrylate) (PMMA) was fabricated. Then, titanium dioxide nanoparticles (nano-TiO₂s) were attached to the treated channel’s interior with the aid of poly(diallyldimethylammonium chloride) (PDADMAC). After coupling the nano-TiO₂-coated microfluidic-based photocatalyst-assisted reduction device (the nano-TiO₂-coated microfluidic-based PCARD) with high-performance liquid chromatography (HPLC) and inductively coupled plasma mass spectrometry (ICP-MS), a selective and sensitive, hyphenated system for Hg speciation was established. Validation procedures demonstrated that the method could be satisfactorily applied to the determination of mercury ions (Hg²⁺) and methylmercury ions (CH₃Hg⁺) in both human urine and water samples. Remarkably, the zeta potential measured clearly indicated that the PDADMAC-capped nano-TiO₂s with a predominance of positive charges indeed provided a steady force for firm attachment to the negatively charged device channel. The cause of the durability of the nano-TiO₂-coated microfluidic-based PCARD was clarified thus. Full article