Optimization of LC–MS/MS using triple quadrupole mass analyzer for the simultaneous analysis of carbosulfan and its main metabolites in oranges
This paper describes an analytical method involving a simple solvent extraction for the simultaneous liquid chromatography coupled to quadrupole tandem mass spectrometry (LC-MS/MS) determination of carbosulfan, its most toxic metabolite--carbofuran--, and its other main metabolites--3-hydroxycarbofuran, 3-ketocarbofuran, 3-hydroxy-7-phenolcarbofuran, 3-keto-7-phenolcarbofuran, 7-phenolcarbofuran and dibutylamine--in oranges. Chromatography was performed on a Zorbax Bonus-RP (150 mm x 2.1 mm, 5 microm). The mobile phase was a ternary gradient water-methanol-acetonitrile with 1.0 mM ammonium acetate at flow rate of 0.2 ml min(-1). The LC separation and MS/MS optimization were studied to selec…
Analysis of Chlorpyrifos in Water, Fruit Juice, and Honeybee Extract by Chemiluminescent Elisa
Abstract The suitability of competitive enzyme-linked immunosorbent assays (ELISAs) with chemiluminescent detection-based immobilized antigen (indirect assay) for rapid and accurate determination of chlorpyrifos in various food matrices was tested. The limit of detection (LOD) values were 1–1.75 ng mL−1, the standard curve midpoint (IC50) was 3.5 ng mL−1, and the assay duration was 1.5 h. Assay application to the analysis of honeybee extract resulted in chlorpyrifos recoveries varying between 62 and 83% in 5–15 ng mL−1 herbicide concentration range.
Occurrence of Aflatoxins in Tigernuts and Their Beverages Commercialized in Spain
A method based on matrix solid phase dispersion extraction was applied to determine aflatoxins B(1), B(2), G(1), and G(2) from tigernuts and tigernut beverages. Recoveries of each aflatoxin from tigernut (spiked at 10 microg/kg level) and from tigernut beverages (spiked at 10 microg/L level) ranged from 72.3 to 82.1% and from 74.0 to 86.3%, respectively. The limits of quantification ranged from 0.21 to 1.49 microg/kg (for tigernuts) and from 0.13 to 0.57 microg/L (for tigernut beverages) studied using liquid chromatography with fluorescence detection. The proposed extraction method followed by liquid chromatography-fluorescence detection determination was applied to 37 and 25 samples of tig…
COVID Obesity: A One-Year Narrative Review
On 11 March 2020, coronavirus disease 2019 (COVID-19) was declared a pandemic by the World Health Organization (WHO). This study focuses on a narrative review about the illness during the first year of the pandemic in relation to obesity. Databases were used to search studies published up to 8 December 2020. In total, 4430 articles and other scientific literature were found, and 24 articles were included in this one-year narrative review. The mean BMI value of severe COVID-19 patients ranged from 24.5 to 33.4 kg/m2, versus 2 for non-severe patients. Articles using the terms obesity or overweight without indicating the BMI value in these patients were common, but this is not useful, as the a…
Volver a lo básico: líneas estratégicas 2018
En el editorial publicado a finales de 2016, el Comité Editorial vislumbró varias líneas estratégicas que debían ser trabajadas para mejorar la calidad y posición de la Revista Española de Nutrición Humana y Dietética. Termina el año 2017, y lo apropiado es revisar y evaluar qué temas y cómo se han abordado, y qué ha quedado pendiente.
Body Mass Index (BMI) and Coronavirus Disease 2019 (COVID-19): A Living Systematic Review
On March 11, 2020, coronavirus disease 2019 (COVID-19) was declared a pandemic by the World Health Organization (WHO). This review focuses on where the body mass index (BMI) value can be used as a tool to evaluate the risk of development and/or aggravation of this disease. Databases were used to search studies published up to April 18, 2020. In total, 4285 articles and other scientific literature were found, and twelve articles were included in this systematic review. The mean BMI value of severe COVID-19 patients ranged from 24.5 to 33.4 kg/m2, versus 22.0 to 24.3 kg/m2 for non-severe patients Articles using the terms obesity or overweight, without indicating the BMI value, in these patien…
Application of hybrid linear ion trap-high resolution mass spectrometry to the analysis of mycotoxins in beer
This paper reports the application of liquid chromatography electrospray ionization ion trap-orbitrap mass spectrometry for the determination of 18 mycotoxins (aflatoxins, fumonisins, trichothecenes, ochratoxin A, sterogmatocystin, beauvaricin, zearalenone and zearalenol) in beer. The extraction procedure was carried out by solid phase extraction (SPE): SPE columns were conditioned with acetonitrile/methanol and water. Beer was loaded onto the column which was washed with water. In these conditions, the recoveries were more than 65% and the relative standard deviation (RSD) were below 18%. The lowest limits of quantification (LLOQ) ranged from 9 to 155 ng ml(-1). Matrix-matched calibration …
Capabilities of different liquid chromatography tandem mass spectrometry systems in determining pesticide residues in food
Abstract Three different liquid chromatography–mass spectrometry (LC–MS) instruments equipped with triple quadrupole (QqQ), quadrupole ion trap (QIT) and quadrupole-time-of-flight (QqTOF), suitable to carry out tandem mass spectrometry, were examined to determine pesticide residues in food. Twelve pesticides (acrinathrin, bupirimate, buprofezin, cyproconazole, λ-cyhalothrin, fluvalinate, hexaflumuron, kresoxim-methyl, propanil, pyrifenox, pyriproxyfen and tebufenpyrad) and six matrices (oranges, strawberries, cherries, peaches, apricots and pears) were taken as model. The comparison was focused on two aspects: the quantitative, covering sensitivity, precision and accuracy as well as the qua…
Liquid chromatography–electrospray quadrupole ion-trap mass spectrometry of nine pesticides in fruits
A liquid chromatographic method, with electrospray ionization tandem mass spectrometry (LC-ESI-MS-MS), has been developed for determining acrinathrin, carbosulfan, cyproconazole, lambda-cyhalothrin, kresoxim methyl, pyrifenox, pyriproxyfen, propanil, and tebufenpyrad in fruits. The ions prominent in ESI spectra were [M + H]+ and [M + Na]+. In the mass analyzer, collision-induced dissociation fragmentation involved common pathways, for example, product ions of [M + H]+ resulted from the cleavage of the carbamic group or an oxygen bound. The utility of the method is demonstrated by the analysis of crude extracts obtained by matrix solid-phase dispersion (MSPD) using C18 as dispersant and dich…
Comparison of four mass analyzers for determining carbosulfan and its metabolites in citrus by liquid chromatography/mass spectrometry
Four liquid chromatography/mass spectrometry (LC/MS) systems, equipped with single quadrupole, triple quadrupole (QqQ), quadrupole ion trap (QIT) and quadrupole time-of-flight (QqTOF) mass analyzers, were evaluated for the analysis of carbosulfan and its main transformation products. The comparison of quantitative aspects (sensitivity, precision and accuracy) was emphasized. Results showed that the triple quadrupole instrument reaches at least 20-fold higher sensitivity (LOD from 0.04 to 0.4 microg kg(-1)) compared to the single quadrupole (4-70 microg kg(-1)), the QIT (4-25 microg kg(-1)) and the QqTOF (4-23 microg kg(-1)) instruments. Recoveries were over 70% for all the analytes, except …
Occurrence of fourteen mycotoxins in tiger-nuts
Abstract A previous developed matrix solid-phase dispersion (MSPD) extraction method was applied for the routine analysis of aflatoxins (AFs), ochratoxin A (OTA), fumonisins (FB 1 and FB 2 ), beauvericin (BEA), nivalenol (NIV), deoxynivalenol (DON), the toxin T-2 (T-2), toxin HT-2 (HT-2), diacetoxyscirpenol (DAS) and zearalenone (ZEN) in tiger-nuts by liquid chromatography–triple-quadrupole linear ion trap (HPLC–QTRAP ® ). The extraction solid support used was C 18 , while the elution solvent was acetonitrile/methanol (50/50, v/v) 1 mM ammonium formate. Using matrix-matched calibration, recoveries and repeatabilities were in the range 67–89% and 2–11% relative standard deviation (RSD), resp…
Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry Analysis of Carbosulfan, Carbofuran, 3-Hydroxycarbofuran, and Other Metabolites in Food
The potential of liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QqTOF-MS) to identify and confirm carbosulfan and seven of its main metabolites (carbofuran, 3-hydroxycarbofuran, 3-ketocarbofuran, 3-hydroxy-7-phenol carbofuran, 3-keto-7-phenolcarbofuran, 7-phenolcarbofuran, dibutylamine) at trace levels from food is explored for the first time. The analytical method developed consists of pressurized liquid extraction (PLE) and LC-QqTOF-MS in positive ion mode, which attains unequivocal identification and quantification of the studied compounds in food, at levels well below of those of concern (0.05 mg/kg for the sum of carbosulfan, carbofuran, and 3-hydroxycarbofuran).…
Applicability of hybrid linear ion trap-high resolution mass spectrometry and quadrupole-linear ion trap-mass spectrometry for mycotoxin analysis in baby food.
Abstract Recent developments in mass spectrometers have created a paradoxical situation; different mass spectrometers are available, each of them with their specific strengths and drawbacks. Hybrid instruments try to unify several advantages in one instrument. In this study two of wide-used hybrid instruments were compared: hybrid quadrupole-linear ion trap-mass spectrometry (QTRAP ® ) and the hybrid linear ion trap-high resolution mass spectrometry (LTQ-Orbitrap ® ). Both instruments were applied to detect the presence of 18 selected mycotoxins in baby food. Analytical parameters were validated according to 2002/657/CE. Limits of quantification (LOQs) obtained by QTRAP ® instrument ranged …
Determination of mycotoxins in multicereal flour by matrix solid phase dispersion and LC–MS/MS
Application of an HPLC-MS/MS method for mycotoxin analysis in commercial baby foods
Abstract This article describes the validation of an analytical method for the detection of 21 mycotoxins in baby food. The analytical method is based on the simultaneous extraction of selected mycotoxins by matrix solid-phase dispersion (MSPD) followed by liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) using a hybrid triple quadrupole-linear ion trap mass spectrometer (QTRAP®). Information Dependent Acquisition (IDA), an extra confirmation tool for samples that contain the selected mycotoxins, was used. The matrix effects were evaluated, and the corrections for the matrix effects were performed using two calibration approaches: external matrix-matched calibration and…
Rapid whole protein quantitation of staphylococcal enterotoxins A and B by liquid chromatography/mass spectrometry
Abstract Staphylococcus aureus is an important pathogen and has been indicated as the fifth causative agent of food-borne human illness throughout the world. Staphylococcal enterotoxins (SEs) are toxic compounds excreted mainly by strains of S. aureus. Among these toxins, enterotoxins A (SEA) and B (SEB) are both of the most prevalent compounds in staphylococcal food poisoning. In this work, reverse phase liquid chromatography coupled to ESI mass spectrometry (LC–ESI/MS) has been applied for its rapid identification and quantification. Limit of detection (LOD) values were 0.5 and 0.2 ng for SEA and SEB, respectively and limit of quantification (LOQ) value was 1 ng for both enterotoxins. SEA…
Evolutionary Trends in the Mitochondrial Genome of Archaeplastida: How Does the GC Bias Affect the Transition from Water to Land?
[EN] Among the most intriguing mysteries in the evolutionary biology of photosynthetic organisms are the genesis and consequences of the dramatic increase in the mitochondrial and nuclear genome sizes, together with the concomitant evolution of the three genetic compartments, particularly during the transition from water to land. To clarify the evolutionary trends in the mitochondrial genome of Archaeplastida, we analyzed the sequences from 37 complete genomes. Therefore, we utilized mitochondrial, plastidial and nuclear ribosomal DNA molecular markers on 100 species of Streptophyta for each subunit. Hierarchical models of sequence evolution were fitted to test the heterogeneity in the base…
Occurrence of fumonisins in organic and conventional cereal-based products commercialized in France, Germany and Spain
A fast and effective method for quantitative determination of fumonisins B1 and B2 (FB1 and FB2) in different cereal-based products was developed. Fumonisins were extracted combining a solid liquid extraction (SLE) pre-treatment and immunoaffinity columns (IACs), which were applied for an effective clean-up. Consecutively, high pressure liquid chromatography (HPLC) coupled to hybrid triple quadrupole-linear ion trap mass spectrometer (QTrap®) was used for the separation, detection and quantification of targeted mycotoxins. The analytical method showed acceptable recoveries ranged from 89.7% to 99.1%, as well as a relative standard deviation (%, RSD) lower than 12%. A total of 1250 samples f…
An Internet-based treatment for Flying Phobia using 360° images: Study protocol for a feasibility pilot study
Background Flying Phobia (FP) is a prevalent disorder that can cause serious interference in a person's life. ICBT interventions have already shown their efficacy in several studies, but studies in the field of specific phobias are still scarce. Moreover, few studies have investigated the feasibility of using different types of images in exposure scenarios in ICBTs and no studies have been carried out on the role of sense of presence and reality judgement. The aim of the present study is to explore the feasibility of an ICBT for FP (NO-FEAR Airlines) using two types of images with different levels of immersion (still and navigable images). A secondary aim is to explore the potential effecti…
An Internet-based program for depression using activity and physiological sensors: efficacy, expectations, satisfaction, and ease of use
Cristina Botella,1,2 Adriana Mira,1 Inés Moragrega,2,3 Azucena García-Palacios,1,2 Juana Bretón-López,1,2 Diana Castilla,1,2 Antonio Riera López del Amo,1 Carla Soler,1 Guadalupe Molinari,1 Soledad Quero,1,2 Verónica Guillén-Botella,2,3 Ignacio Miralles,1,2 Sara Nebot,1 Berenice Serrano,1,2 Dennis Majoe,4 Mariano Alcañiz,2,5 Rosa María Baños2,31Department of Basic, Clinical Psychology and Psychobiology, Universitat Jaume, Castellón, Spain; 2CIBER Physiopathology of Obesity and Nutrition, CIBERobn, Instituto de Salud Carlos III, Santiago de Compostela, Spain; 3Department o…
Microbial contamination of milk and dairy products from restaurants in Spain
This study was carried out to evaluate the microbiological quality of milk and some dairy products, including 95 lots of warm milk, 95 lots of milk conserved at room temperature, and 75 lots of dairy products collected from restaurants in Spain. According to the European microbiological criteria (92/46/EEC, 93/43/EEC, and Commission Regulation No. 2073/2005), 31% and 35% of the total examined lots exceed the adopted limits of mesophilic aerobic counts and Enterobacteriaceae, respectively. This may be due to incorrect handling of milk and dairy products and inadequate cleaning and sanitization of milk container. Further, 2% of all the lots examined were positive for the presence of Escherich…
Stability and bioaccessibility of EGCG within edible micro-hydrogels. Chitosan vs. gelatin, a comparative study
Micro-hydrogels are very promising systems for the protection and controlled delivery of sensitive bioactives, but limited knowledge exists regarding the impact of this encapsulation on their bioaccessibility. In this work, two different hydrogel-forming biopolymers (gelatin and chitosan) were compared as wall materials for the microencapsulation of a model flavonoid, (−)-epigallocatechin gallate (EGCG). Results showed that gelatin was more adequate as wall material for the encapsulation of EGCG than chitosan, achieving higher encapsulation efficiencies (95% ± 6%), being more effective in delaying EGCG release and degradation in aqueous solution and exhibiting a 7 times higher bioaccessibil…
A survey of mycotoxins in random street-vended snacks from Lagos, Nigeria, using QuEChERS-HPLC-MS/MS
Abstract A survey in African snacks was carried out in order to evaluate the intake of 23 mycotoxins. The African snack samples were purchased from street vendors within Lagos metropolis (Nigeria) and evaluated for the presence of 23 mycotoxins using a modified QuEChERS procedure coupled with liquid chromatography-triple quadrupole linear ion trap mass spectrometer. The snacks included akara, baked coconut, coconut candy, donkwa, groundnut cake (kulikuli), lafun, milk curd (wara), fresh and dried tiger-nuts, and yam flour. Only three mycotoxins were detected in 23.8% of the studied snacks, and at concentrations ranging from 6 to 54 μg kg−1. The concentrations of aflatoxin B1 (AFB1) and AFB2…
Natural co-occurrence of mycotoxins in wheat grains from Italy and Syria
This article describes the application of an analytical method for the detection of 25 mycotoxins in wheat grain based on simultaneous extraction using matrix solid-phase dispersion (MSPD) followed by liquid chromatography coupled to tandem mass spectrometry, a hybrid triple quadrupole-linear ion trap mass spectrometer (QTrapÒ). Information Dependent Acquisition (IDA), an extra confirmation tool for samples that contain the target mycotoxins, was used. The analysis of 40 Syrian and 46 Italian wheat grain sam- ples interestingly showed that Syrian samples were mainly contaminated with ochratoxin A and aflatox- ins, whereas Italian samples with deoxynivalenol and 15-acetyldeoxynivalenol. Emer…
Mass spectrometry applications
The history of proteomics dates back to the discovery of two-dimensional gels in the 1970s, which provided the first feasible way of displaying hundreds or thousands of proteins on a single gel. Despite mass spectrometry being restricted for a long time to small and thermostable compounds, the development in the late 1980s of two techniques for the routine and general formation of molecular ions of intact biomolecules changed this situation and mass spectrometry has become an indispensable tool for proteomics research. The aim of this chapter is to review the major types of MS instruments used in proteomics analysis and to discuss strategies for the analysis of whole proteins and peptides o…
One-year monitoring of aflatoxins and ochratoxin A in tiger-nuts and their beverages.
A sensitive and selective liquid chromatography-triple quadrupole-tandem mass spectrometry (LC-ESI-MS-MS) method was developed for the routine analysis of aflatoxins (AFB(1), AFB(2), AFG(1) and AFG(2)) and ochratoxin A (OTA) in tiger nuts and tiger-nut beverage (horchata). A matrix solid phase dispersion was adapted to eliminate lipidic interferences. The solid support was C(18), while the elution solvent was acetonitrile. Mean recoveries obtained at two fortification levels were 72-83% and 71-81% for horchata and tiger nut respectively with relative standard deviations (RSDs) <13% and 15% respectively. The LC-MS-MS method allowed quantification and identification at low levels in two matri…
Evaluation of matrix solid-phase dispersion (MSPD) extraction for multi-mycotoxin determination in different flours using LC-MS/MS
An existing matrix solid-phase dispersion (MSPD) method for aflatoxins (AFs) and ochratoxin A (OTA) extraction was extended by further 14 mycotoxins. After it careful optimization, this method was applied to determine the occurrence of these mycotoxins on commercial flour samples (with different cereals composition) collected from local markets. In a total of 49 samples investigated, 9 mycotoxins were identified. Nivalenol (NIV) and Beauvericin (BEA) were the mycotoxins found most frequently. The samples that presented major contamination were wheat flours and bakery preparations. Despite of the great number of positives finding, only one wheat flour sample exceeded the maximum limits (ML) …
Confirmation of Fenthion Metabolites in Oranges by IT-MS and QqTOF-MS
14 pages, 4 figures, 4 tables.-- PMID: 18020315 [PubMed].-- Printed version published Dec 15, 2007.
Propuesta de valores de referencia ambientales microbiológicos en los servicios de restauración
Introducción: Proponer una nueva referencia microbiológica ambiental en los servicios de restauración. Objetivo: El presente trabajo muestra la determinación y evaluación de la contaminación microbiológica generada en un establecimiento de servicio de alimentos. Método: Se basa en el muestreo microbiológico de superficie utilizando filtros de membrana de ésteres mixtos de celulosa y en el muestreo de aire utilizando placas de Petri. Resultados: Los límites de contaminación se establecieron antes y durante la elaboración de alimentos, mediante el análisis microbiológico de las superficies y del medio ambiente, sistemas de equipos, hasta límites confiables y estableciendo niveles de aceptació…
Rapid mycotoxin analysis in human urine: A pilot study
A simple and rapid method effective for quantitative determination of deoxynivalenol (DON), T-2 toxin (T-2), HT-2 toxin (HT-2), zearalenone (ZEN), ochratoxin A (OTA), aflatoxins (AFs) B(1), B(2), G(1) and G(2) and fumonisins FB(1) and FB(2) in urine was developed. The urine was diluted with phosphate buffer solution (PBS) and thoroughly mixed. For clean-up and extraction, the mixture was loaded on a MYCO 6in1 IAC. Hybrid triple quadrupole-linear ion trap mass spectrometer (QTrap) was used for the detection. Extra tools for confirmation of selected mycotoxins in positive samples, Information Dependent Acquisition (IDA) experiments, were also developed. The use of immunoaffinity columns follo…
The Role of the Liquid Chromatography-Mass Spectrometry in Pesticide Residue Determination in Food
The use of liquid chromatography (LC) in pesticide residue determination was usually limited to groups of compounds or single compounds for which no suitable gas chromatographic (GC) conditions were available. However, recent developments have significantly enlarged the LC scope in this field of analysis. One of the most important advances was the on-line coupling of efficient LC separation with mass spectrometry detectors (LC-MS and LC-MS/MS) that makes this technique an excellent method for the determination of pesticides and their transformation products in complex matrices such as food. This review considers the application of LC-MS/MS in this field. Emphasis is placed on the tandem MS …
Determination of amitraz and its transformation products in pears by ethyl acetate extraction and liquid chromatography-tandem mass spectrometry.
A method has been developed for identification and quantification of the acaricide amitraz and its transformation products, 2,4-dimethylaniline (DMA), 2,4-dimethylformamidine (DMF) and N-2,4-dimethylphenyl-N-methylformamidine (DMPF) in pears. The analytes were extracted using ethyl acetate and anhydrous sodium sulphate. Analysis was performed by liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS) in the positive ion mode using a triple quadrupole (QqQ) instrument. Two precursor-product ion transitions were monitored for each compound in the selected reaction monitoring (SRM) mode. The method was validated with pears taken from the orchard before the amitraz treatment …
Determination of carbosulfan and its metabolites in oranges by liquid chromatography ion-trap triple-stage mass spectrometry.
Liquid chromatography ion-trap mass spectrometry LC-MSn has been successfully applied to identify and confirm carbosulfan and seven of its metabolites in oranges after pressurized liquid extraction (PLE) with dichloromethane. Mass spectra of carbosulfan and its metabolites were investigated using multiple stages of mass spectrometry. Although interpretation of the fragmentation pathways, based on mass spectra, enables structural elucidation and identification of these compounds, the proposed fragmentation pathways and ion structures need verification by exact mass measurements. The analytical method--PLE and LC-MS3 --was validated: limits of quantification (LOQ) ranged from 0.01 to 0.07 mg …
Analysis of mycotoxins in barley using ultra high liquid chromatography high resolution mass spectrometry: comparison of efficiency and efficacy of different extraction procedures.
The effectiveness of four extraction methods (modified QuEChERS, matrix solid-phase dispersion (MSPD), solid-liquid extraction (SLE) and solid-phase extraction (SPE) clean-up) were evaluated for simultaneous determination of 32 mycotoxins produced by the genus Fusarium, Claviceps, Aspergillus, Penicillium and Alternaria in barley by ultra high pressure liquid chromatography coupled to ultra-high resolution mass spectrometry (UHPLC-Orbitrap(®) MS). The efficiency and efficacy of extraction methods were evaluated and compared in number of extracted mycotoxins and obtained recoveries. From the one point of view, QuEChERS procedure was fast and easy, as well as it was able to successfully extra…
Key analytical features of mycotoxins
Apple-products phytochemicals and processing: a review.
Epidemiological studies have linked the consumption of apples with reduced risk of some cancers, cardiovascular disease, asthma, and diabetes. Extensive research exists on apples and the health benefits of their beverages and phytochemicals. The purpose of this paper is to review the most recent literature in this area focusing on phytochemicals, phytochemical bioavailability and antioxidant behavior.
Proposal of reference values of microbiological environment monitoring in foodservice establishments
Introducción: Proponer una nueva referencia microbiológica ambiental en los servicios de restauración. Objetivo: El presente trabajo muestra la determinación y evaluación de la contaminación microbiológica generada en un establecimiento de servicio de alimentos. Método: Se basa en el muestreo microbiológico de superficie utilizando filtros de membrana de ésteres mixtos de celulosa y en el muestreo de aire utilizando placas de Petri. Resultados: Los límites de contaminación se establecieron antes y durante la elaboración de alimentos, mediante el análisis microbiológico de las superficies y del medio ambiente, sistemas de equipos, hasta límites confiables y estableciendo niveles de aceptació…
Study of mycotoxin calibration approaches on the example of trichothecenes analysis from flour
The aim of this study was to evaluate the applicability of different calibration approaches in trichothecenes analysis from wheat flour. Concretely eight trichothecenes (five type B trichothecenes and three type A trichothecenes) were analyzed by matrix solid-phase dispersion (MSPD) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). In the first set of experiments the presence of matrix effects was evaluated; values ranged between 59% and 79%. In the second set of experiments, solutions to compensate these signal suppressions were examined. Different calibration methods showed to tackle matrix effects obtaining values between 69% and 85% for external matrix matched calibration a…
“Five Keys to Safer Food” and COVID-19
On 11 March 2020, coronavirus disease 2019 (COVID-19) was declared a pandemic by the World Health Organization (WHO) and, up to 18:37 a.m. on 9 December 2021, it has produced 268,440,530 cases and 5,299,511 deaths. This disease, in some patients, included pneumonia and shortness of breath, being transmitted through droplets and aerosols. To date, there is no scientific literature to justify transmission directly from foods. In this review, we applied the precautionary principle for the home and the food industry using the known “Five Keys to Safer Food” manual developed by the World Health Organization (WHO) and extended punctually in its core information from five keys, in the light of new…
Chitosan films for the microbiological preservation of refrigerated sole and hake fillets
The effect of chitosan films for shelf-life extension of fresh fillets of hake (Merluccius merluccius) and sole (Solea solea) was evaluated over a 15-day storage at 4 ± 1 °C. Fish fillets wrapped in a chitosan matrix were individually packaged in air (AP) and under vacuum (VP). Microbiological analyses (total aerobic mesophilic bacteria, Pseudomonas, H2S-producing bacteria, lactic acid bacteria, Enterobacteriaceae and Listeria monocytogenes were carried out during the shelf-life. The microbial species were inhibited (p < 0.05) by the presence of chitosan films, especially under VP conditions. A significant (p < 0.05) increase of the lag phase and a reduction of the final microbial populatio…
Exploring the Relationship Between the Acceptability of an InternetBased Intervention for Depression in Primary Care and Clinical Outcomes: Secondary Analysis of a Randomized Controlled Trial
Background: Depression is one of the most prevalent psychological disorders worldwide. Although psychotherapy for depression is effective, there are barriers to its implementation in primary care in Spain. The use of the Internet has been shown to be a feasible solution. However, the acceptability of Internet-based interventions has not been studied sufficiently. Objective: To assess the acceptability of an Internet-based intervention (IBI) for depression in primary care, and explore the relationship between expectations and satisfaction and the improvement in the clinical variables in primary care patients receiving this intervention. Furthermore, it offers data about the effects of some s…
Identification of unknown pesticides in fruits using ultra-performance liquid chromatography–quadrupole time-of-flight mass spectrometry
Abstract Ultra-high-performance liquid chromatography–quadrupole time-of-flight mass spectrometry (UPLC-QqTOF-MS) is an emerging technique offering more rapid and efficient separation, as well as the possibility to obtain accurate mass measurement and tandem mass spectrometry (MS/MS). This paper deals with the use of UPLC-QqTOF-MS to identify the pesticide residues present in complex pear extracts. Carbendazim, imazalil, and ethoxyquin were successfully identified because of the accurate mass determination of their protonated molecule and their major fragments in the product ion mass spectra. A few plastic and latex additives were also found, most of them probably coming from the packaging …
Optimization of Matrix Solid-Phase Dispersion method for simultaneous extraction of aflatoxins and OTA in cereals and its application to commercial samples
Abstract A method based on Matrix Solid-Phase Dispersion (MSPD) has been developed for the determination of 5 mycotoxins (ochratoxin A and aflatoxins B and G) in different cereals. Several dispersants, eluents and ratios were tested during the optimization of the process in order to obtain the best results. Finally, samples were blended with C 18 and the mycotoxins were extracted with acetonitrile. Regarding to matrix effects, the results clearly demonstrated the necessity to use a matrix-matched calibration to validate the method. Analyses were performed by liquid chromatography–triple quadrupole-tandem mass spectrometry (LC–QqQ-MS/MS). The recoveries of the extraction process ranged from …
Evaluation of mycotoxins and their metabolites in human breast milk using liquid chromatography coupled to high resolution mass spectrometry
Humans can be exposed to mycotoxins through the food chain. Mycotoxins are mainly found as contaminants in food and could be subsequently excreted via biological fluids such as urine or human breast milk in native or metabolised form. Since breast milk is usually supposed as the only food for new-borns, the occurrence of mycotoxins in thirty-five human milk samples was evaluated by a newly developed method based on QuEChERS extraction and UHPLC-HRMS detection. The method described here allows the detection of target mycotoxins in order to determine the quality of this initial feeding. The method has been fully validated, with recoveries ranging from 64% to 93% and relative standard deviatio…
Recent trends in liquid chromatography-tandem mass spectrometry to determine pesticides and their metabolites in food
Abstract The applications of liquid chromatography-mass spectrometry (LC-MS) have exploded in innumerable analytical fields, including pesticide-residue determination. There is no doubt that LC-MS is currently competing with gas chromatography (GC)-MS for the status of ‘reference’ analytical technique to determine pesticide residues and that its ever-increasing application is bound to the evolution of modern instruments and their growing performance qualities. We highlight the large number and variety of pesticides that can be readily determined using such instruments, the respective merits of the different mass analyzers, and the improvements brought about by tandem MS (MS 2 ). We also dis…
Routine application using single quadrupole liquid chromatography-mass spectrometry to pesticides analysis in citrus fruits.
Abstract A rapid and sensitive liquid chromatography–electrospray ionization–mass spectrometry method has been developed for the routine analysis of buprofezin, bupirimate, hexaflumuron, tebufenpyrad, fluvalinate and pyriproxyfen in citrus fruits. Extracts were obtained by matrix solid-phase dispersion (MSPD) using C 18 as dispersant and dichloromethane-methanol (80:20, v/v) as eluent. Matrix effects were tested for all matrices by addition of standard to sample blank extracts (samples containing no detectable residues). Mean recoveries obtained at fortification levels between 0.01 and 5 mg kg −1 were 57–97% with relative standard deviations (RSDs) from 5 to 19%. The limits of quantificatio…
Mass spectrometry strategies for mycotoxins analysis in European beers
In this work, an existent solid-phase extraction (SPE) procedure was used to study the occurrence of mycotoxins in different European beers. HPLC-QqQ-MS/MS and ultra high resolution mass analyser have been optimized for the analysis of 18 mycotoxins: the methods were validated according to the EU Commission Decision 2002/657/EC guidelines. In this sense, matrix-matched calibration was performed for each type of beer, obtaining an effective quantification. The recoveries ranged from 63 to 91% and repeatability and reproducibility expressed as relative standard deviation (RSD%) were lower than 17%. On one hand, HPLC-LTQ-Orbitrap ® was used for unambiguous identification of target mycotoxins, …
Comparison of liquid chromatography using triple quadrupole and quadrupole ion trap mass analyzers to determine pesticide residues in oranges.
Liquid chromatography-triple quadrupole/mass spectrometry (LC-TQ/MS) and liquid chromatography-quadrupole ion trap/mass spectrometry (LC-QIT/MS) for determining bupirimate, hexaflumuron, tebufenpyrad, buprofezin, pyriproxyfen, and fluvalinate in fruits have been compared. The differences in the mass spectra obtained by triple and ion trap quadrupoles are discussed, showing how both of them provide interesting features. The evaluation of the two instruments was carried out by ethyl acetate extraction of oranges spiked with the studied pesticides at LOQ and 10 times the LOQ. Results obtained by LC-TQ/MS correlated well with those obtained by LC-QIT/MS. Recoveries were 70-94% by LC-TQ/MS and 7…