Amadeo R Fernández-Alba

• Professor
• Professor (Full) at University of Almería

Microplastics in agricultural ecosystems have gained recent attention due to their widespread prevalence and the reported impacts. The current study reviews close to 90 relevant publications. Seventy studies were selected using ResNetBot, a tool designed to identify key works based on their significance to other studies matching the search criteria...

This study introduces an analytical methodology that combines passive sampling with ultra-high pressure liquid chromatography coupled with a high-end quadrupole-time-of-flight mass spectrometer (UHPLC-QTOF-MS) for monitoring the honeybee (Apis mellifera L.) exposome across various European regions and seasons. The sampling methodology employs the r...

This presentation reports the “Laboratory Triple-A Rating” results obtained for the EU/EFTA laboratories participating in the Proficiency Tests (PTs) organised between 2018 and 2022 by the EU Reference Laboratory for Pesticides in Fruits and Vegetables (EUPT-FV20 to EUPT-FV24) which were performed on the matrices of green bean, red cabbage, onion,...

Environmental monitoring is crucial for assessing the overall state of the ecosystems in terms of contaminant impact and chemical landscape. The use of honey bee (Apis mellifera) colonies considerably eases the sampling activities, as honey bees are exposed to a wide range of substances that are transported and accumulated within the beehives. In t...

Primary Processed Foods are a class of food items that are ready for consumption after minimal processing in the supply chain. These products are ubiquitous in our daily diet, but so far a limited number of studies dealt with the optimization of quality control methods to check their content of contaminants. Among primary processed foods, bee polle...

Primary Processed Foods are a class of food items that are ready for consumption after minimal processing in the supply chain. These products are ubiquitous in our daily diet, but so far a limited number of studies dealt with the optimization of quality control methods to check their content of contaminants. Among primary processed foods, bee polle...

Continuous exposure of honey bee colonies to acaricides can affect Varroa destructor populations and their susceptibility to veterinary treatments. In this study, two groups of colonies were established using decontaminated wax or commercial wax (containing more pesticide residues). Both groups received two amitraz treatments and Varroa levels were...

The performance of the QuEChERS method in this study, as indicated by a high percentage (>90%) of recovery observations falling within the range of 60-140% and a sample replicate deviation (% RSD) of <20%, for the routine analysis of isoprocarb and carbaryl pesticides, has been evaluated over a 14-month period for the export of Indonesian coffee. F...

The analysis of pesticide residues and mycotoxins in baby food demands exceptionally low limits of quantitation, necessitating the use of highly sensitive instruments capable of conducting trace analyses. High-resolution instruments typically fail to detect such low levels. However, the latest advancements in liquid time-of-flight technology, when...

This manuscript presents a comprehensive review of high‐resolution mass spectrometry in the field of food analysis and metabolomics. We have followed the historical evolution of metabolomics, its associated techniques and technologies, and its increasing role in food science and research. The review provides a critical comparison and synthesis of t...

Background The application of ion mobility coupled with mass spectrometry in food metabolomics has become increasingly popular since 2014, although it is still a niche combination in the field of food metabolomics and authentication. This growth can be attributed to its unique capability of offering detailed molecular analysis, which is crucial fo...

In this comprehensive study, we evaluated the feasibility of using hydrogen instead of helium as a carrier gas in a GC-MS/MS system for pesticide residue analysis, spanning three matrices: pepper, tomato, and zucchini.

This study confirms the uptake, translocation and bioaccumulation of 100 nm polystyrene nanoplastics in the root, stem and leaves of the plant Lepidum sativum at exposure concentrations ranging from environmentally realistic 10 μg/L up to a high of 100 mg/L. Accumulation in plant tissues was characterised by aggregation in the intercellular spaces...

The analysis of highly polar pesticides is challenging due to their unique physicochemical properties, requiring specialized chromatographic techniques for their accurate and sensitive detection. Furthermore, the high level of co-extracted polar matrix components that can co-elute with the analytes can interfere with the analysis. Consequently, the...

Spices such as paprika, curry, turmeric, dry chilli, and black pepper are grown in various geographic locations and widely used by consumers across the world. Pesticides applied during crop production practices could contaminate the produce, affecting the quality and posing a health risk for consumers. The complexity of the spice matrix and the wid...

Mānuka honey is a valuable commodity produced by bees foraging the flowers of Leptospermum scoparium, a bush native to New Zealand and Australia. Due to its high value and proven health benefits, authenticity fraud in the sale of this food is a significant risk, as recounted in the literature. Four compulsory natural products must be present at min...

The sorption and vector effect of microplastics on the transfer of pesticides and polycyclic aromatic hydrocarbons (PAHs), as well as its impact on agriculture remain largely unexplored. This comparative study is first to investigate the sorption behavior of different pesticides and PAHs at environmentally realistic concentrations by model micropla...

The use of apicultural matrices for the environmental monitoring of pesticides is a widely employed approach that facilitates to a great extent the sampling procedures. Honey bees are one of the most commonly employed matrices in these studies due to their abundance in the colonies and their direct contact with the beehive and the environment. Howe...

Clean-up step is essential during the multiresidue sample preparation process to remove undesired matrix components that may cause analytical interferences or suppression effect. However, its application generally by specific sorbents entails time-consuming work producing low recoveries for some compounds. Moreover, it usually needs to be adapted t...

Microwavable plastic food containers can be a source of toxic substances. Plastic materials such as polypropylene polymers are typically employed as safe materials in food packaging, but recent research demonstrates the migration of plastic substances or their by-products to food simulants, to foodstuff, and, more recently, to the human body throug...

The use of reclaimed water for crop irrigation has been proposed as a suitable alternative for farmers in the coastal areas of Mediterranean countries, which suffer from greater water scarcity. In this work we study the impact on the water-soil-plant continuum of using reclaimed water for commercial crops irrigated over a long period, as well as th...

The direct injection of acetonitrile sample extracts using GC-MS/MS is a challenging task in specific matrices of high polar components, like strawberries. In the current study, strawberry samples were extracted by acetonitrile and subsequently cleaned up using increased amounts of primary secondary amine and anhydrous magnesium sulfate. Furthermor...

Solanum lycopersicum cv. Ramyle was cultivated using different amounts of synthetic and natural crop protection agents, combined with organic and chemical fertilisers. Chemometric studies on the LC-Q-Orbitrap metabolite profiles of tomatoes distinguished a compound [M+H]⁺ at m/z 291.1075 (C12H19O8⁺, 0.0 ppm). The compound, identified as gerberin, i...

This nationwide monitoring aimed to investigate the prevalence of residues of plant protection products (PPPs) and veterinary medicine products (VMPs) based on random selection of apiaries of Apis mellifera. For a three-year period (2012, 2013 and 2016), this study targeted 306 PPPs, VMPs and other active substances in 442 samples of bee bread hone...

Beeswax is known for its ability to retain pesticides for a long time, and the progressive accumulation of pesticides in wax has had adverse health effects on bees. This study aimed to determine the residue levels of pesticides in Brazilian beeswax and assess the health risk to bees due to exposure to these pesticides using hazard quotient calculat...

Background Pesticide quantitation in foods relies on the availability of matrix reference materials, which, however, are scarce because of the general instability of pesticides. In particular, no avocado reference material has been developed. Objective This research aimed to develop a reference material to support the determination of pesticide re...

There is an increasing concern about the use of synthetic acaricides to fight the ectoparasitic mite Varroa destructor . Natural products such as formic acid (FA) and oxalic acid (OA) have emerged as a possible alternative control strategy. However, given the difficulty of analysing these highly polar compounds and the lack of robust and reliable m...

Pesticide analysis in bee-related matrices is a well-established methodology mainly based on LC-MS/MS and GC-MS/MS instrumentation that allows the determination of the chemical origin of certain colony disorders, as well as the assessment of the environmental contamination and the safety of apicultural products of human interest. The present work a...

Nontarget data acquisition for target analysis (nDATA) workflows using liquid chromatography-high-resolution accurate mass (LC-HRAM) spectrometry, spectral screening software, and a compound database have generated interest because of their potential for screening of pesticides in foods. However, these procedures and particularly the instrument pro...

A fast and sensitive method was validated for the analysis of pesticide residues in baby food. After an QuEChERS-based extraction, the samples were analysed with a dual-channel liquid chromatography instrument coupled to a triple quadrupole mass spectrometer. The method consisted of two independent injections per sample. In the first injection the...

Using reclaimed water to irrigate crops can be an important route for organic contaminants of emerging concern (CECs) to be introduced into agricultural production and thus find their way into the food chain. This work aims to establish accumulation models for the different parts of a crop (fruit/leaves/roots) and the soil of some of the most commo...

In this study, we aimed to validate and apply a quick and easy extraction method for the simultaneous determination of 27 pesticide residues at trace levels in agricultural samples (soil, fruit, and leaf) to monitor the presence of these contaminants released from reclaimed water. The procedure was based on a salting-out extraction method with acid...

Due to their extensive use in both agricultural and non-agricultural applications, pesticides are a major source of environmental contamination. Honey bee colonies are proven sentinels of these and other contaminants, as they come into contact with them during their foraging activities. However, active sampling strategies involve a negative impact...

Abundant studies have been published evaluating different parameters of reverse-phase liquid chromatography (LC) and supercritical fluid chromatography (SFC), both coupled to electrospray (ESI)/mass spectrometry (MS) for pesticide residue analysis. However, there is a lack of a comprehensive comparative study that facilitates deep knowledge about t...

Thymol has been considered as an organic varroacide with less toxicity than synthetic chemicals such as amitraz, coumaphos or tau-fluvalinate. The present study evaluates the presence, persistence and distribution of thymol during a five-month sampling period; before, during and after the application of thymol treatment in field conditions. Moreove...

In this study, sample processing and preparation conditions, including the selection of a proper extract solvent between ACN, EtAC, and its mixture, were optimised for the residue analysis of a large number of pesticides in different herbal plants (fennel seed, camomile, and dry mint). The number of pesticides that had acceptable accuracy and preci...

The active substances coumaphos, tau-fluvalinate and amitraz are among the most commonly employed synthetic miticides to control varroa infestations in apiculture. These compounds can persist inside the beehive matrices and can be detected long time after their application. The present study describes the application of a new passive sampling metho...

In the present study, a batch mode procedure has been developed to remove pesticides from beeswax coming from bee farms. The beeswax is treated by an Extraction Process with methanol at 65 °C followed by an Adequation Process with water at 70 °C. This procedure can reduce the beeswax contamination load by values of around 80% – 90% for the acaricid...

Highly polar pesticides are frequently used in agriculture. However, their physicochemical properties make very difficult the analysis of these compounds following common procedures. Polar pesticides show poor retention and peak shapes in the common stationary phases used for multiresidue methods of pesticides. For this reason, multiple columns wit...

In this study, we aimed to develop and validate a quick, easy, and robust extraction method for the simultaneous determination of 30 organic contaminants of emerging concern (CECs) including some transformation products in soil samples. Three different extraction methods based on an ultrasonic cylindrical probe (UAE), a pressurized liquid extractio...

Serious difficulties in evaluating the fungicides captan and folpet by the usual chromatography systems coupled to mass spectrometry are well known. These compounds are highly prone to degradation due to different conditions into tetrahydrophthalimide (THPI) and phthalimide (PHI). Such an effect can be produced at different stages of the analytical...

The use of high-resolution mass spectrometry (HRMS) for the simultaneous target and non-target analysis of pesticide residues in food control is a subject that has been studied over the last decade. However, proving its efficacy compared to the more established triple quadrupole mass spectrometers (QQQ-MS2) is challenging. Various HRMS platforms ha...

Treated wastewater is currently used in the agricultural sector to solve the lack of availability of freshwater in many regions. However, reclaimed water can contain multiclass of organic contaminants. Therefore, the soil can become a reservoir of agricultural (e.g pesticides) and urban (e.g. pharmaceuticals) contaminants. Consequently, the evaluat...

In 2016, Valverde et al. proposed a new three-dimensional (XYZ) classification, with three categories (A, B or C) within each dimension, to evaluate performance-underperformance of laboratories participating in the EU Proficiency Test for pesticide residues in fruits and vegetables (EUPT-FV), which is known as “Laboratory Triple-A Rating” approach...

Anthraquinone (9,10-dioxoanthracene) is an aromatic organic compound that has been the cause of concern in recent years due to its presence in commodities such as coffee and tea. Anthraquinone has been linked to potential adverse effects on human health and the environment. The most commonly employed methods for the analysis of coffee and tea cause...

Microplastics are ubiquitous and their sampling is a difficult task. Honeybees interact with the environment inside their foraging range and take pollutants with them. In this work, we demonstrated for the first time that worker bees can act as active samplers of microplastics. We collected honeybees from apiaries located in the centre of Copenhage...

The main objective of this study is to develop, optimize and validate a new automatic extraction method based on pressurized liquid extraction that avoids the matrix effects associated to these dry, high-fat and difficult matrices, thus allowing the detection of a wide range of pesticides and contaminants at low concentration levels. The developed...

Dual-channel chromatography was evaluated for pesticide residue analysis in fruits and vegetables and for unknown compounds detection. A dual-channel system was tested coupled to triple quadrupole and high-resolution mass spectrometry. The first part of the investigation was related to the improvement of the sample throughput with a 100 mm column....

Despite the restriction of the use of neonicotinoids in the EU, including thiamethoxam and clothianidin, the debate over their risk on honey bees has not been fully settled. This study presents results of a three-year study working with 180 honey bee colonies in ten replicates. Colonies were sorted into three treatments (60 colonies per treatment)...

The objectives of this study are (i) to evaluate the difficulties associated with the currently used multiresidue methods for food within the European Union; (ii) to develop an automated extraction method that allows the control of anthraquinone at very low concentrations –below the current maximum residue limit (MRL) of 20 μg/kg for tea, coffee, h...

Honeybee colonies are proven bio-samplers in their foraging area, as organic contaminants such as pesticides are continuously deposited in their hives. However, the use of honeybee colonies for the biomonitoring of contaminants requires the sampling of biological matrices such as bees, pollen, honey or beeswax. This active sampling alters the colon...

Two high-resolution instruments (a QToF and a QOrbitrap) were used to evaluate a segmented non-target MS2 (SWATH/vDIA) acquisition for pesticide residue analysis. Three matrices (tomato, orange, and leek) and 163 pesticides were used for this study. Samples were analysed by use of 1, 5, 8, and 20 mass windows. The last one only in the QToF. The obj...

Evaluation of chiral pesticides remains a frequently neglected matter in routine food control laboratories. This fact is due to the existence of many residue definitions but also due to the lack of robust instrumental methods for the evaluation of these isomeric compounds. However, supercritical fluid chromatography coupled to mass spectrometry (SF...

In the last decade, the consumption trend of organic food has increased dramatically worldwide. Since only a few pesticides are authorized in organic crops, concentrations are expected to range at zero or ultra-trace levels. In this context, the aim of the present study was to investigate the need for an improvement in the residue controls at very...

Honeybee (Apis mellifera) is one of the most important crop and wild plant pollinators, playing an essential role in the agricultural production and the natural ecosystems. However, the number of honeybee colonies is decreasing alarmingly, which has motivated extensive research on the factors affecting their development and survival in some regions...

Reclaimed wastewater usage is increasing worldwide, particularly, its use in crop irrigation shows a growing trend. However, the potential risks associated with these waters have not been extensively studied to date. The presence of organic microcontaminants (pesticides, drugs, etc.) is one of such hazards. As an illustrative case, in Spain one thi...

The influence of genetic diversity and exposure to xenobiotics on the prevalence of pathogens was studied within the context of a voluntary epidemiological study in Spanish apiaries of Apis mellifera iberiensis, carried out during the spring season of years 2014 and 2015. As such, the evolutionary lineages of the honey bee colonies were identified,...

This review is focused on the application of Orbitrap™ mass spectrometry for pesticide residue analysis. The importance of mass accuracy and resolution is explained. Also, the most typical acquisition modes available in QOrbitrap™ are discussed.

This study describes the high sensitivity and the reduced ion suppression and matrix effect that can be achieved by supercritical fluid chromatography (SFC) in the analysis of dried spices as complex matrices. Samples selected for the evaluation were cayenne and black pepper, which are representative of complex dried spices. To carry out the evalua...

This study describes a comprehensive comparison between supercritical fluid chromatography (SFC) and gas chromatography (GC) coupled to mass spectrometry for the analysis of pyrethroids in vegetable matrices. The ionization process used was electrospray ionization in SFC and electron ionization in GC. In general, liquid chromatography coupled to ma...

Plastic multilayers are widely used for baby food packaging. However, it is important to consider that migration of food contact materials (FCM) into the baby food can occur. The comprehensive identification of potential migrants, including intentionally added substances (IAS) and non-intentionally added substances (NIAS), is required to assess the...

Two straightforward methods for glyphosate and AMPA analysis in honey through ion chromatography coupled to Q-Orbitrap accurate high-resolution mass spectrometry as well as their application to real samples are presented. The sample preparation step is accomplished through dilution with methanol-water or water. No pH adjustment is necessary. Recove...

The introduction of sequential mass isolation window acquisition mode in high-resolution quadrupole time-of-flight analysers undoubtedly represents an important improvement in the MS/MS spectra obtained when working in non-target analysis. However, the advantages and limitations of this approach have not been sufficiently defined and evaluated. The...

Most widely developed approaches for pesticide residues analysis in spices and herbs present serious limitations; this is because of the high number of interferences that they typically contain, which makes it difficult to identify/quantify compounds in a considerable percentage of cases. Different strategies are applied to overcome these difficult...

Interest in the identification of potential migrants, including non-intentionally added substances (NIASs), referring to objects intended to come into contact with food, has recently been growing. Such substances have been found at trace levels in simulants and in food products placed in contact with plastic materials. However, the identification o...

Identification and quantitative determination of analytes released from food contact materials (FCMs) is still an analytical challenge for scientists since neither chemical nor spectral databases nor analytical standards are available. Gas and liquid chromatography hyphenated to a variety of accurate mass analyzers based on the use of high-resoluti...

Double-acting electro-spun membranes for water treatment. The present invention consists of a process for the manufacture of active membranes based on submicron fibers that combine an antimicrobial action with the ability to retain apolar pollutants in aqueous solution. The membranes are produced by an electro-spinning process in aqueous solution f...

Thermally labile pesticides (captafol, captan, dicofol, and folpet) are highly prone to suffer thermal degradation during sample introduction into a gas chromatograph (GC) to tetrahydrophthalimide (THPI), 4,4′-dichlorobenzophenone (DCBP), and phthalimide (PI), respectively, mainly produced in the glass liner of the injector. This undesired behavior...

This study reports an analytical approach by gas chromatography and high-resolution mass spectrometry (HRMS) intended to be used for investigation of non-targeted environmental contaminants in honeybees. The approach involves a generic extraction and analysis with two GC-HRMS systems: time-of-flight and Orbitrap analyzers, GC-TOF-MS, and GC-Orbitra...

There is an increasing concern about the negative impacts of veterinary drugs in beehive compartments. This study evaluates the presence and distribution of chemical residues in beeswax, bee bread and honey and determinates in what extension honeybees are exposed to them. Samples were analyzed by LC-MS/MS and GC–MS/MS with a wide scope of 322 chemi...

EU legislation requires that chemicals migrating from food packaging into food do not endanger human health. A proper safety assessment must go further than simply testing for known ingredients used to make the packaging materials. The identification of all potential migrants, including non-intentionally added substances (NIAS), is required to asse...

Spices are known as difficult matrices that contain variable amounts of fats, piperine or many other matrix constituents. The increasing sensitivity of new GC-MS/MS platforms opens new approaches to analyze pesticide residue in complex matrices such as spices, by sample dilution. The aim of this work is to develop and validate an effective multires...

In this work, 260 pesticide residues, including insecticides, acaricides, fungicides, and herbicides, were extracted from honeybees using the QuEChERS methodology modified by applying an ultrasonic probe, which avoided the homogenization step and reduced the extraction time. Gas and liquid chromatography, both coupled to triple-quadrupole mass spec...

The efficiency of a data independent acquisition by the sequential window acquisition of all theoretical fragment ions (SWATH®) in high resolution accurate mass spectrometry was evaluated for pesticide residue analysis. Selection of various mass range windows over 100–950 Da was studied to produce MS/MS spectra with selectivity improvement. The num...

In the period 2008-2017, the EU Reference Laboratory for Pesticide Residues in Fruits and Vegetables organized ten EUPT-FVs (EUPT-FV10 to EUPT-FV19) using ten different matrices (carrot, cauliflower, leek, mandarin, pear, potato, pepper, broccoli, spinach and lemon). The number of pesticides evaluated in each test item ranged between 11 (EUPT-FV17)...

In the last decade, the consumption trend of organic food has increased dramatically worldwide. However, the lack of reliable chemical markers to discriminate between organic and conventional products makes this market susceptible to food fraud in products labeled as “organic”. Metabolomic fingerprinting approach has been demonstrated as the best o...