Search Results (16)

This paper aimed to study soil organic carbon (SOC) sequestration under no-tillage (NT) and full inversion tillage (FIT) soil management systems as influenced by crop residue placement. A five-year piece of research was carried out in western Sicily, Italy, on an Opuntia ficus-indica orchard (C-CAM soil) located in a semi-arid Mediterranean climate. Barley was sown annually in the orchard inter-rows at 180 kg ha⁻¹. FIT and NT were compared in interaction with two barley residue managements: (i) removed (rem) and (ii) retained in the field (ret), laid in a split-plot design, with soil management as the main plot and residue management as the sub-plot. The main plot was arranged on two inter-rows, 108 m long and 5 m wide each, replicated three times. SOC (%) and carbon natural abundance (δ¹³C‰) were determined by using an EA-IRMS. The highest biomass turnover was achieved by FITret (0.85%) vs. NTret (0.46%). The distribution of SOC showed higher values for NT in the top 10 cm soil layer (6.3 g kg⁻¹ in NTret vs. 5.0 g kg⁻¹ in FITret) but lower carbon content in deeper layers. At a depth of 30 cm, FITret maintained 4.4 g kg⁻¹ of SOC, while NTret reached only 3.7 g kg⁻¹, confirming that tillage facilitates the transport and stabilization of carbon in deeper layers. Our results also suggested that when crop residues are left on the soil surface instead of being incorporated into the soil, this may limit the effectiveness of carbon sequestration. Under the experimental tested conditions, which include low susceptibility to erosion processes, the FIT system proved to be an optimal strategy to enhance SOC sequestration and improve the sustainability of agricultural systems in a semi-arid Mediterranean environment. Full article

This study showcases an attached-biomass system based on twin-layer technology for cultivating Galdieria phlegrea using municipal wastewater, equipped with a smart sensor system for the remote monitoring of operational parameters. From an industrial scale-up perspective, the system offers high scalability, with low impact and operating costs. Mathematical approximation modelling identified the optimal growth conditions across five experiments. The theoretical yield was estimated to reach 1 kg_DW/m² of biomass within two months. Integrated use of isotopic mass spectrometry and spectrophotometric methods allowed us to study the metabolic strategies implemented by the algal community during the best growth condition at different resolutions, showing an increase in the nitrogen concentration over time and a favourable affinity of the organism for nitrogen species that are commonly present in the urban effluent. SEM studies showed a clean algal biofilm (free of foreign organisms), which could guarantee usage in the high economic potential market of biorefineries. Full article

The present study was undertaken for the first time in India to generate a database of isotopic signatures of authentic Indian honey to verify the regulatory criteria laid down by the Food Safety and Standards Authority of India (FSSAI). In this study, ninety-eight (98) authentic honey samples from nineteen (19) different botanical sources were collected from five (05) geographical regions of India and analyzed to generate a database of stable carbon isotope ratios (¹³C/¹²C) by Elemental Analyzer/Liquid Chromatography–Isotopic Ratio Mass Spectrometry (EA/LC-IRMS). The samples were analyzed for the parameters δ¹³C_Honey(δ¹³C_H), δ¹³C_Protein(δ¹³C_P), δ¹³C individual sugars, ∆δ¹³C_{Protein-Honey}(δ¹³C_P-H), C4 sugar, ∆δ¹³C_{Fructose-Glucose}(δ¹³C_Fru-Glu), ∆δ¹³C_max, and foreign oligosaccharides (FOs), as per the official methods of analysis of the Association of Official Analytical Chemists (AOAC 998.12) and the FSSAI. The results were evaluated against the published literature and Indian regulatory criteria for authentic honey. The δ¹³C value for honey (δ¹³C_H) ranged from −22.07 to −29.02‰. It was found that 94% of Indian honey samples met the criteria for Δδ¹³C_P-H (≥−1.0‰), Δδ¹³C_Fru-Glu (±1.0‰), and C4 sugar content (7% maximum), with negative C4 sugar values treated as 0% as prescribed by the AOAC method. Further, 86% of samples met the FO criteria (maximum 0.7% peak area). Thus, the data of this study provide scientific backing for these four (04) parameters as per the FSSAI regulation. However, the non-compliance of a high number (47%) of authentic honey samples for Δδ¹³C_max (±2.1‰) compels further systematic investigation with a special focus on bee feeding practices. Further, in the present study, it was found that honey samples with a Δδ¹³C_P-H greater than +1‰ and a C4 sugar content more negative than −7% also did not comply with the Δδ¹³C_max criteria. Hence, Δδ¹³C_P-H values (>+1‰ equivalent to C4 sugar < −7%) could be an indicator of C3 adulteration to some extent. Full article

Beef, as a nutrient-rich food, is widely favored by consumers. The production region significantly influences the nutritional value and quality of beef. However, current methods for tracing the origin of beef are still under development, necessitating effective approaches to ensure food safety and meet consumer demand for high-quality beef. This study aims to establish a classification model for beef origin prediction by analyzing elemental content and stable isotopes in beef samples from two countries. The concentrations of elements in beef were analyzed using ICP-MS and ICP-OES, while the stable carbon isotope ratio was determined using EA-IRMS. Machine learning algorithms were employed to construct classification prediction models. A total of 83 beef samples were analyzed for the concentrations of 52 elements and the stable carbon isotope ratio. The classification accuracy of the PLS-DA model built on these results was 98.8%, while the prediction accuracy was 94.12% for the convolutional neural network (CNN) and 82.35% for the Random Forest algorithm. The PLS-DA model demonstrated higher classification accuracy compared to CNN and Random Forest, with an explanatory power (R²) of 0.924 and predictive ability (Q²) of 0.787. Combining the analysis of 52 elements and the stable carbon isotope ratio with machine learning algorithms enables effective tracing and origin prediction of beef from different regions. Key factors influencing beef origin were identified as Fe, Cs, As, δ¹³C, Co, V, Sc, Rb, and Ru. Full article

Compound-specific isotope analysis (CSIA) can provide unique insights into the cycling of elements including carbon and nitrogen. One approach for CSIA is the use of high-performance liquid chromatography (HPLC) to separate compounds of interest, followed by analysis of these compounds using an elemental analyser coupled to an isotope ratio mass spectrometer. A key component of this technique is the fraction collector, which automatically collects compounds as they are separated by HPLC. Here, we present a fraction collector that is a simple adaptation of a 3D printer, and, thus, can be easily adopted by any laboratory already equipped for HPLC. In addition to the much lower cost compared to commercial alternatives, this adaptation has the advantage for CSIA that the 3D printer is able to heat the collected fractions, which is not true for many commercial fraction collectors. Heating allows faster evaporation of the solvent, so that the dried compounds can be measured by EA–IRMS immediately. The procedure can be repeated consecutively so that diluted solutions can have the compounds concentrated for analysis. Any computer-controlled HPLC can be integrated to the fraction collector used here by means of AutoIt. Full article

The present study aims to explore the degradation process of compostable, starch-based (i.e., Mater-Bi^®) shopping bags in the marine environment using isotope ratio mass spectrometry and Fourier-transform infrared spectroscopy (FTIR). The mixing model applied to the isotopic data suggested that the compostable shopping bags had a mixed composition with a higher percentage of polyesters (61% to 72%). Changes in the isotopic composition over a 73-day period of marine water immersion showed a decrease in the corn starch constituent (of 14% to 13%), with a similar rate in both types of bags in accordance with the evidence derived from the infrared spectra. The time required for complete degradation of the starch fraction was estimated by an isotopic approach from 124 to 180 days, following zero-order kinetics. The coupled application of these two analytical methodologies promises to (i) show complementary evidence regarding the time-course degradability of different polymers via FTIR changes, and (ii) infer potential degradation mechanisms via carbon isotope analyzes. We encourage the use of this information to support advancements in the development of more sustainable-by-design plastic materials. Full article

The need to guarantee the geographical origin of food samples has become imperative in recent years due to the increasing amount of food fraud. Stable isotope ratio analysis permits the characterization and origin control of foodstuffs, thanks to its capability to discriminate between products having different geographical origins and derived from different production systems. The Framework 6 EU-project “TRACE” generated hydrogen (²H/¹H), carbon (¹³C/¹²C), nitrogen (¹⁵N/¹⁴N), and sulphur (³⁴S/³²S) isotope ratio data from 227 authentic beef samples. These samples were collected from a total of 13 sites in eight countries. The stable isotope analysis was completed by combining IRMS with a thermal conversion elemental analyzer (TC/EA) for the analysis of δ(²H) and an elemental analyzer (EA) for the determination of δ(¹³C), δ(¹⁵N), and δ(³⁴S). The results show the potential of this technique to detect clustering of samples due to specific environmental conditions in the areas where the beef cattle were reared. Stable isotope measurements highlighted statistical differences between coastal and inland regions, production sites at different latitudes, regions with different geology, and different farming systems related to the diet the animals were consuming (primarily C3- or C4-based or a mixed one). Full article

One of the goals of archaeological studies is to determine how material goods and ideas moved among human populations, and bitumen is a worthy proxy because it has been used since prehistory. As a result, when bitumen is excavated from archaeological sites, determining its provenance is important because it sheds light on the trade and communication of populations at a given time. During the study of archaeological bitumen from coastal sites in central and southern Puglia (Italy), we observed that stable isotope ratios of saturated and aromatic fractions were incompatible with those obtained from asphaltenes, supporting the absorption of a foreign substance. Experiments showed that lipids are absorbed by bitumen and, in the case of oils, are distributed mainly in the saturated and aromatic fractions as their isotopic ratios change. The same experiments showed that the isotopic ratios of the asphaltenes do not change. Lipid absorption on the archaeological bitumen may have occurred before the bitumen was applied to the pottery, during the use of the pottery or while underground, before being excavated. These hypotheses are discussed, and it is concluded that the isotopic ratio of asphaltenes is a reliable proxy for provenance, whereas those of the saturated and aromatic fractions should be considered with caution due to possible lipid absorption. Nevertheless, they provide new information on pottery use that can be used in archaeological chemistry. Full article

The demand for organic food products has increased in recent years due to them being perceived healthier, safer, and eco-friendlier by consumers, boosting the development of this industry. The higher retailing price of organic products increases the risk of fraudulent practices, making it necessary to establish control mechanisms to authenticate these products. However, the authentication of organic foodstuffs is a great analytical challenge that still requires further research. In the case of organic agriculture, regulations mainly determine the nutrient inputs that can be used by farmers, and generally prohibit the use of pesticides and/or synthetic fertilisers, aiming at maintaining soil fertility using green manures, composts, animal manures, etc. These inputs affect the final food product, and numerous analytical attempts, based on the measurement of multiple markers or complex chemical/physical profiles, have been tested over recent years. However, the high variability of these measurements due to weather condition factors reduces their efficiency and limits their use. In this sense, stable isotopes have emerged as an analytical technique with great potential for the authentication of organic agricultural products, due to their lower dependence on weather conditions and capability to reflect the origin of plant nitrogen, in the case of stable nitrogen isotopes. In this work, the feasibility was assessed using stable isotopes of bulk nitrogen for the organic authentication of four important horticultural crops (zucchini, cucumber, tomato, and pepper) produced in Almeria, southern Spain, which is the largest producing region with the highest export levels in Europe. To this end, 360 samples of vegetables were collected and their δ¹⁵N values were determined by combustion coupled to stable isotope ratio mass spectrometry (EA/IRMS). The results allowed an authentication framework to be established based on three ranges delimited by δ¹⁵N = 2‰ and δ¹⁵N = 5‰, which made it possible to detect with a high degree of confidence vegetables produced under proper organic practices (δ¹⁵N > 5‰), conventional practices (δ¹⁵N < 2‰), and samples that should be tracked over time to be considered organically produced (middle range). The results of this study demonstrated the potential of using δ¹⁵N as a single measure to authenticate organic vegetables, providing official bodies with a tool to make decisions about the organic accreditation of regularly inspected farmers. Full article

The grains and milling fractions of common buckwheat (Fagopyrum esculentum Moench) and Tartary buckwheat (Fagopyrum tataricum (L.) Gaertn.) are widely used for both industrial and small-scale food and non-food products. This paper represents a preliminary study of the isotopic signature (δ¹³C, δ¹⁵N, and δ³⁴S) to differentiate between buckwheat species (common vs. Tartary), organic and conventional cultivation farming, and different buckwheat fractions (light flour, semolina, and hulls) obtained by a traditional cereal stone-mill. Stable isotope ratios were analyzed using an elemental analyzer coupled to an isotope ratio mass spectrometer (EA/IRMS). The results indicated that δ¹³C, δ¹⁵N, and δ³⁴S values could be used to verify the origin and production practices of buckwheat and even its products. Full article

The present study investigated the effects of cultivation practices on grain (oats) yield and yield components, such as straw yield, harvest index, thousand kernel weight, and plant lodging. In addition, multi-element composition and isotopic signature (δ¹³C, δ¹⁵N) of the oat grains were studied. The spring oat cultivar ‘Noni’ was grown in a long-term field experiment during 2015–2020, using three management practices: control without organic amendment, incorporation of manure every third year and incorporation of crop residues/cover crop in the rotation. Synthetic nitrogen (N) (0, 55, 110 and 165 kg/ha) was applied during oat development in each system. Multi-element analysis of mature grains from two consecutive years (2016 and 2017) was performed using EDXRF spectroscopy, while stable isotope ratios of carbon (C) and nitrogen (N) were obtained using an elemental analyzer coupled to an isotope ratio mass spectrometer (EA/IRMS). The results show how cultivation practices affect yield components and isotopic and elemental signatures. Increasing the N rate improved both the oat grain and straw yields and increased susceptibility to lodging. The results show how the elemental content (Si, Ca, Zn, Fe, Ti, Br and Rb) in the oat grains were influenced by intensification, and a noticeable decrease in elemental content at higher N rates was the result of a dilution effect of increased dry matter production. The mean δ¹⁵N values in oat grains ranged from 2.5‰ to 6.4‰ and decreased with increasing N rate, while δ¹³C values ranged from −29.9‰ to –28.9‰. Based on the δ¹⁵N values, it was possible to detect the addition of synthetic N above an N rate of 55 kg/ha, although it was impossible to differentiate between different management practices using stable isotopes. Full article

Rice is a staple food for more than half of the world’s population. The discrimination of geographical origin of rice has emerged as an important issue to prevent mislabeling and adulteration problems and ensure food quality. Here, the discrimination of Thai Hom Mali rice (THMR), registered as a European Protected Geographical Indication (PGI), was demonstrated. Elemental compositions (Mn, Rb, Co, and Mo) and stable isotope (δ¹⁸O) in the rice were analyzed using inductively coupled plasma mass spectrometry (ICP-MS) and elemental analyzer isotope ratio mass spectrometry (EA-IRMS), respectively. The recoveries and precisions of all elements were greater than 98% and lower than 9%, respectively. The analytical precision (±standard deviation) was below ±0.2‰ for δ¹⁸O measurement. Mean of Mn, Rb, Co, Mo, and δ¹⁸O levels was 14.0 mg kg⁻¹, 5.39 mg kg⁻¹, 0.049 mg kg⁻¹, 0.47 mg kg⁻¹, and 25.22‰, respectively. Only five valuable markers combined with radar plots and multivariate analysis, linear discriminant analysis (LDA) could distinguish THMR cultivated from three contiguous provinces with correct classification and cross-validation of 96.4% and 92.9%, respectively. These results offer valuable insight for the sustainable management and regulation of improper labeling regarding geographical origin of rice in Thailand and other countries. Full article

Landscape multifunctionality is increasingly recognized as an important aspect in sustainability and developmental debates. Yet, how and why a multifunctional landscape configuration develops over time has not been sufficiently studied. Here we present the geoarchaeological investigation of the Santa Mariña de Augas Santas site, in northwestern Spain. We focus on the role of religious practice, and of its interplay with productive strategies, in landscape transformation. A geochemical, mineralogical, and geochronological characterization of the pedo-sedimentary record (including XRF, EA-IRMS, XRD, OSL and 14C measurements) allowed to characterize catchment scale sedimentation processes in relation to agricultural activities. The geographical and chronological coincidence of production functions with documented religious activities demonstrate that both aspects shared geographical spaces during the last millennium. Current landscape multifunctionality at Santa Mariña is thus not the final outcome of a specific evolution, but an essential aspect of traditional land use strategies through history and a driver of change. This work highlights the need of a long-term study of the processes of landscape configuration when assessing the sustainability of traditional productive systems. Full article

In the Adriatic lagoons of northern Italy, manila clam (Ruditapes philippinarum) farming provides important socio-economic returns and local clams should be registered with the Protected Designations of Origin scheme. Therefore, there is a need for the development of rapid, cost-effective tests to guarantee the origin of the product and to prevent potential fraud. In this work, an elemental analysis (EA) coupled with isotope ratio mass spectrometry (IRMS) was employed to identify the isotopic fingerprints of clams directly collected onsite in three Adriatic lagoons and bought at a local supermarket, where they exhibited certification. In particular, a multivariate analysis of C/N, δ¹³C and δ¹⁵N in manila clam tissues as well as δ¹³C in shells and $\Delta$¹³C (calculated as δ¹³C_shell–δ¹³C_tissues) seems a promising approach for tracking the geographical origin of manila clams at the regional scale. Full article

The knowledge of the isotopic composition of virgin olive oil (VOO) allows the evaluation of authenticity and geographical origin, being an important tool against fraud. This study aimed to assess if VOOs produced in three Mediterranean regions could be discriminated on the basis of multivariate statistical analysis of geoclimatic and isotopic data. A total of 138 geo-referenced VOO samples from Portugal, France and Turkey from two different cultivation years were collected. The isotopic composition (δ¹³C, δ²H and δ¹⁸O) of VOOs was obtained using an elemental analyzer coupled to an isotope ratio mass spectrometer (EA-IRMS). One-way analysis of variance for δ¹³C, δ²H and δ¹⁸O showed some significant differences either between crop years or geoclimatic conditions. Based on multiple regression analyses using meteorological and geographical parameters, a meteoric water line for olive oil from Portugal, France and Turkey, in two harvest years, were created to assess the impact of climate change on their δ²H and δ¹⁸O values. Principal component analysis and Linear Discriminant Analysis, used to sort samples according to geoclimatic origin, performed best for French and Portuguese olive oils. In light of the results, multivariate isotopic analysis of VOO samples may discriminate not only between geoclimatic regions but also among cultivation years. Full article