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1.
Food Chem ; 304: 125428, 2020 Jan 30.
Artigo em Inglês | MEDLINE | ID: mdl-31476548

RESUMO

To protect allergic patients and guarantee correct food labeling, robust, specific and sensitive detection methods are urgently needed. Mass spectrometry (MS)-based methods could overcome the limitations of current detection techniques. The first step in the development of an MS-based method is the identification of biomarkers, which are, in the case of food allergens, peptides. Here, we implemented a strategy to identify the most salient peptide biomarkers in peanuts. Processed peanut matrices were prepared and analyzed using an untargeted approach via high-resolution MS. More than 300 identified peptides were further filtered using selection criteria to strengthen the analytical performance of a future, routine quantitative method. The resulting 16 peptides are robust to food processing, specific to peanuts, and satisfy sequence-based criteria. The aspect of multiple protein isoforms is also considered in the selection tree, an aspect that is essential for a quantitative method's robustness but seldom, if ever, considered.

2.
Food Chem ; : 125679, 2019 Oct 19.
Artigo em Inglês | MEDLINE | ID: mdl-31718834

RESUMO

The interest of using LC-MS/MS as a method for detection of allergens in food is growing. In such methods, peptides are used as biomarkers for the detection and quantification of the allergens. The selection of good biomarker peptides is of high importance to develop a specific, universal and sensitive method. Biomarkers should, for example, be robust to food processing. To evaluate robustness, test material incurred with hazelnut having undergone different food processing techniques was produced. Proteins of these materials were extracted, digested and further analyzed using HRMS. After peptide identification, selection was carried out using several criteria such as hazelnut specificity and amino acid composition. Further selection was done by comparing peptide MS intensities in the different food matrices. Only peptides showing processing robustness were retained. Eventually, eight peptides coming from three major hazelnut proteins were selected as the best biomarkers for hazelnut detection in processed foods.

3.
Mycotoxin Res ; 35(4): 341-351, 2019 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-31119557

RESUMO

Degradation of the mycotoxin patulin (PAT) and the generation of (less toxic) breakdown products, such as (E/Z)-ascladiol (ASC-E/Z) and desoxypatulinic acid (D-PAT), can occur due to chemical, physical and biological treatments. Our study focused on the chemical degradation of PAT in the presence of ascorbic acid (AA) both for pure PAT standard in acidified aqueous solution and for PAT-contaminated cloudy apple juice (CAJ) (obtained via addition of apple mash produced from apples inoculated with Penicillium expansum). Within this framework, different concentrations of AA were evaluated, as well as the presence/absence of oxygen and different storage temperatures. In order to do so, an in-house methodology allowing a good separation of PAT from its reaction and breakdown products was optimized first. The highest PAT reduction (60%) in CAJ with an initial PAT concentration of 100 µg/kg and 0.25% (w/v) AA was achieved after 6 days of incubation at 22 °C in the presence of oxygen. It was also found that the treatment by AA resulted in the generation of degradation products less toxic than PAT (such as (E/Z)-ASC). In conclusion, AA used to improve numerous product quality aspects (e.g. colour (less browning), nutritional value, etc.) and considered as a safe food additive (Food and Drug Administration (FDA) (1999)) has an effect on PAT degradation. It was shown that such degradation generated less toxic compounds in the presence of oxygen. In view of consumers' safety, fortification of apple juice (and possibly apple-based products) with AA could be helpful within an integrated system to ensure products with low levels of patulin. The optimum conditions for such an approach within a legal and practical point of view need to be further explored.

4.
Metabolites ; 8(3)2018 Aug 24.
Artigo em Inglês | MEDLINE | ID: mdl-30149593

RESUMO

Bioactive compounds present in plant-based foods, and their metabolites derived from gut microbiota and endogenous metabolism, represent thousands of chemical structures of potential interest for human nutrition and health. State-of-the-art analytical methodologies, including untargeted metabolomics based on high-resolution mass spectrometry, are required for the profiling of these compounds in complex matrices, including plant food materials and biofluids. The aim of this project was to compare the analytical coverage of untargeted metabolomics methods independently developed and employed in various European platforms. In total, 56 chemical standards representing the most common classes of bioactive compounds spread over a wide chemical space were selected and analyzed by the participating platforms (n = 13) using their preferred untargeted method. The results were used to define analytical criteria for a successful analysis of plant food bioactives. Furthermore, they will serve as a basis for an optimized consensus method.

5.
Artigo em Inglês | MEDLINE | ID: mdl-29912638

RESUMO

This research aimed at evaluating the safety, and the type, level and prevalence of mycotoxins in grain sorghum of four sub-Saharan African (SSA) countries (Burkina Faso, Ethiopia, Mali and Sudan). A multi-analyte LC-MS/MS method for quantification of 23 mycotoxins (nivalenol, deoxynivalenol, fusarenon X, neosolaniol, 3-acetyl deoxynivalenol, 15-acetyl deoxynivalenol, diacetoxyscirpenol, roquefortine C, HT-2 toxin, alternariol, T-2 toxin, FB1, FB2, FB3, zearalenone, aflatoxin G1, aflatoxin G2, aflatoxin B1, aflatoxin B2, sterigmatocystin, OTA, altenuene, alternariol monomethylether) was applied to different sorghum matrices. Of the 1533 analysed samples, 33% were contaminated with at least one of the following mycotoxins: aflatoxins, fumonisins, sterigmatocystin, Alternaria toxins, OTA and zearalenone. Country of origin, colour, source and collection period of sorghum samples significantly influenced the type, level and prevalence of mycotoxins. Sterigmatocystin (15%), fumonisins (17%) and aflatoxins (13%) were the most prevalent. FB1 (274 ± 585 µg/kg) had the highest mean concentration followed by FB2 (214 ± 308 µg/kg) while diacetoxyscirpenol (8.12 ± 19.2 µg/kg) and HT-2 (11.9 ± 0.00 µg/kg) had the lowest concentrations. Neosolaniol, fusarenon-X, 3-acetyl deoxynivalenol, 15-acetyl deoxynivalenol, T-2 toxin, nivalenol and roquefortine C were not detected in any of the samples. Sudan had the lowest prevalence and mean concentration of all mycotoxins. Pink sorghum had the highest concentrations of fumonisins and aflatoxins. Mycotoxins from Aspergillus spp. and Alternaria spp. are the mycotoxins of concern in SSA grain sorghum with regard to prevalence, concentration and possible health risk from exposure. Based on the performed risk characterisation, daily consumption of sorghum containing aflatoxins, alternariol, alternariol monomethyl ether, sterigmatocystin and OTA could result in exceeding the established health-based guidance values for these toxins.


Assuntos
Alternaria/química , Aspergillus/química , Exposição Dietética/análise , Contaminação de Alimentos/análise , Micotoxinas/análise , Sorghum/química , Burkina Faso , Etiópia , Humanos , Mali , Sudão
6.
Food Chem ; 254: 359-366, 2018 Jul 15.
Artigo em Inglês | MEDLINE | ID: mdl-29548464

RESUMO

Heat-induced color changes of crustaceans are commonly described as the release of astaxanthin. In this study on Crangon crangon, it was found that astaxanthin plays a minor role in the (dis)coloration. By LC-HRMS, two polar, process dependent pigments were found. One pigment was identified as riboflavin and one as drosopterin (level-2 certainty). Thermal treatments had highest effect on drosopterin concentration changes and were chosen as indicator for a kinetic study of heat-induced color changes. The kinetic data fitted a consecutive step model (r2 = 0.971), including a first step in which drosopterin was released (kd,85°C = 0.95 ±â€¯0.09 min-1; Ead = 105 ±â€¯4 kJ/mol) and a second step where drosopterin is degraded (kb,85°C = 0.02 ±â€¯0.002 min-1; Eab = 190 ±â€¯15 kJ/mol). The kinetic model shows that shrimp should be heated at lower temperatures (<80 °C) than the heating temperatures used by fishermen (86-101 °C), creating opportunities for quality optimization. Therefore, this study delivers essential information needed in a comprehensive quality optimization study of the cooked brown shrimp.


Assuntos
Culinária , Crangonidae/química , Pigmentos Biológicos , Pteridinas/farmacocinética , Animais , Cor , Temperatura Alta , Cinética , Pteridinas/análise , Riboflavina/análise , Frutos do Mar , Xantofilas/análise
7.
J AOAC Int ; 101(3): 627-632, 2018 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-28964272

RESUMO

A simple, reliable method for the detection of free and modified Fusarium mycotoxins in beer using state-of-the-art ultra-high-performance supercritical fluid chromatography (UHPSFC) with low-resolution tandem MS (MS/MS) is presented in this paper. The UHPSFC-MS/MS method was developed for nivalenol, deoxynivalenol, 15-acetyl-deoxynivalenol, 3-acetyl-deoxynivalenol, deoxynivalenol-3-glucoside, HT-2 toxin, T-2 toxin, T-2 toxin-3-glucoside, neosolaniol, diacetoxyscirpenol, zearalenone, α-zearalenol, and ß-zearalenol and their internal standards deepoxy-deoxynivalenol and zearalanone. Due to the broad range of the physicochemical properties of the aforementioned, the sample preparation step was minimized to avoid analyte losses. Extraction with acetonitrile-water-acetic acid (79 + 20 + 1, v/v/v) and hexane in combination with solid-phase extraction (C18) was followed by a filtration step. After filtration, the extract was evaporated, and the remaining residue was redissolved in a mobile phase for injection (methanol-water; 90 + 10, v/v). A mobile phase consisting of supercritical CO2 and a small portion of methanol was used. The developed multimycotoxin method permits the simultaneous determination of multiple fusariotoxins in an one-step chromatographic run using UHPSFC-MS/MS. SFC is a promising strategy; however, the retention mechanism is complex, leading to the unpredictable nature of elution and to some mycotoxins not being retained on the column. This restricts the applicability of UHPSFC in multimycotoxin analyses. The present study is the first report on the use of UHPSFC for the analysis of free and modified Fusarium mycotoxins.

8.
Anal Bioanal Chem ; 409(22): 5201-5207, 2017 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-28744561

RESUMO

The recent detection of nuts (including peanut) in spices across the globe has led to enormous recalls of several spices and food products in the last two years. The lack of validated detection methods specific for spices makes it difficult to assess allergen presence at trace levels. Because of the urgent need for confirmation of possible peanut presence in chili peppers, an LC-MS/MS method was optimized and developed for this particular food matrix. Although several studies optimized LC-MS detection strategies specific for peanuts, the presence of complex components in the spices (e.g., phenolic components) makes method optimization and validation necessarily. Focus was laid on validation of the method with real incurred chili peppers (whereby a known amount of peanut is added) at low concentrations, to deal with possible matrix interferences. LC-MS/MS proves to be a good alternative to the currently most applied methods (ELISA and RT-PCR) and can be used as a complementary method of analysis when results are unclear. Peanut marker peptides were selected based on their abundancy in digested incurred chili peppers. The limit of detection was determined to be 24 ppm (mg peanut/kg), a level whereby the risk for potential allergic reactions is zero, considering the typical portion size of spices. The chili pepper powder under investigation proved to contain low levels of peanuts after LC-MS/MS, ELISA, and RT-PCR testing. Graphical abstract Standard curve of the detected peanuts in chili pepper samples using the novel LC-MS/MS method.


Assuntos
Alérgenos/análise , Arachis/química , Capsicum/química , Análise de Alimentos/métodos , Alérgenos/química , Cromatografia Líquida , Ensaio de Imunoadsorção Enzimática , Contaminação de Alimentos/análise , Limite de Detecção , Peptídeos/análise , Peptídeos/química , Reação em Cadeia da Polimerase , Espectrometria de Massas em Tandem
9.
Crit Rev Food Sci Nutr ; 57(8): 1584-1592, 2017 May 24.
Artigo em Inglês | MEDLINE | ID: mdl-25898143

RESUMO

Following the discovery of aflatoxins in the early 1960s, there have been many studies leading to the uncovering of many mycotoxins and the understanding of associated health effects in animals and humans. Consequently, there has been a global increase in the number of countries with mycotoxin regulations in foods. However, many African countries have only regulations for aflatoxins (or a few other mycotoxins) in specific foods, or no regulations at all. This paper critically reviews the challenges thwarting the establishment of mycotoxin regulations and their impacts on human dietary mycotoxin exposure in Africa. Mycotoxin regulatory limits for different countries are compared with mycotoxin tolerable daily intakes established by international food safety bodies taking into account consumption patterns. The agrarian setup, food insecurity, and mycotoxin analytical challenges in African countries are discussed; and more feasible mycotoxin dietary exposure reduction strategies are proposed.


Assuntos
Contaminação de Alimentos/prevenção & controle , Microbiologia de Alimentos , Abastecimento de Alimentos/legislação & jurisprudência , Legislação sobre Alimentos/normas , Micotoxinas/análise , África , Contaminação de Alimentos/análise , Inocuidade dos Alimentos
10.
Food Chem ; 209: 177-84, 2016 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-27173550

RESUMO

The effect of protein oxidation on proteolysis during meat digestion was investigated following storage and subsequent in vitro digestion of beef and pork patties. Protein oxidation was evaluated as thiol oxidation, total carbonylation, and specific carbonylation (α-amino adipic and γ-glutamic semialdehyde). Furthermore, 4-hydroxyphenylalanine, a hydroxylation product of phenylalanine, was identified and quantified as a new protein oxidation marker. After 7days of chilled illuminated storage (4°C), significant oxidative modifications were quantified and the oxidative degradation was continued during in vitro digestion. The observed effects were more abundant in beef patties. Protein oxidation before digestion resulted in impaired proteolysis during digestion.


Assuntos
Produtos da Carne/análise , Proteínas/química , Animais , Fenômenos Bioquímicos , Bovinos , Digestão , Armazenamento de Alimentos , Humanos , Modelos Biológicos , Oxirredução , Proteólise , Suínos
11.
J Chromatogr A ; 1429: 248-57, 2016 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-26739912

RESUMO

In this study, a fast, simple and selective ultra high performance liquid chromatographic-tandem mass spectrometric (UHPLC-MS/MS) method for the simultaneous detection and quantification of colistin, sulfadiazine, trimethoprim, doxycycline, oxytetracycline and ceftiofur and for the detection of tylosin A in swine manure was developed and validated. First, a simple extraction procedure with acetonitrile and 6% trichloroacetic acid was carried out. Second, the supernatant was evaporated and the pellet was reconstituted in 1 ml of water/acetonitrile (80/20) and 0.1% formic acid. Extracts were filtered and analyzed by UHPLC-MS/MS on a Kinetex C18 column using gradient elution. The method developed was validated according to the criteria of Commission Decision 2002/657/EC. Recovery percentages varied between 94% and 106%, repeatability percentages were within the range of 1.7-9.2% and the intralaboratory reproducibility varied between 2.8% and 9.3% for all compounds, except for tylosin A for which more variation was observed resulting in a higher measurement uncertainty. The limit of detection and limit of quantification varied between 1.1 and 20.2 and between 3.5 and 67.3 µg/kg, respectively. This method was used to determine the presence and concentration of the seven antibiotic residues in swine manure sampled from ten different manure pits on farms where the selected antibiotics were used. A link was found between the antibiotics used and detected, except for ceftiofur which is injected at low doses and degraded readily in swine manure and was therefore not recovered in any of the samples. To the best of our knowledge, this is the first method available for the simultaneous extraction and quantification of colistin with other antibiotic classes. Additionally, colistin was never extracted from swine manure before. Another innovative aspect of this method is the simultaneous detection and quantification of five different classes of antibiotic residues in swine manure.


Assuntos
Antibacterianos/análise , Técnicas de Química Analítica/métodos , Cromatografia Líquida de Alta Pressão , Esterco/análise , Espectrometria de Massas em Tandem , Animais , Reprodutibilidade dos Testes , Suínos
12.
Mol Plant Pathol ; 17(6): 805-17, 2016 08.
Artigo em Inglês | MEDLINE | ID: mdl-26456797

RESUMO

Brown spot disease, caused by Cochliobolus miyabeanus, is currently considered to be one of the most important yield reducers of rice (Oryza sativa L.). Despite its agricultural importance, little is known about the virulence mechanisms deployed by the fungus. Therefore, we set out to identify novel virulence factors with a role in disease development. This article reports, for the first time, the production of tentoxin by C. miyabeanus as a virulence factor during brown spot disease and the identification of the non-ribosomal protein synthetase (NRPS) CmNps3, responsible for tentoxin biosynthesis. We compared the chemical compounds produced by C. miyabeanus strains differing in virulence ability using ultra-high-performance liquid chromatography (UHPLC) coupled to high-resolution Orbitrap mass spectrometry (HRMS). The production of tentoxin by a highly virulent strain was revealed by principal component analysis of the detected ions and confirmed by UHPLC coupled to tandem-quadrupole mass spectrometry (MS/MS). The corresponding NRPS was identified by in silico genome analysis and confirmed by gene deletion. Infection tests with wild-type and Cmnps3 mutants showed that tentoxin acts as a virulence factor and is correlated with chlorosis development during the second phase of infection. Although rice has previously been classified as a tentoxin-insensitive plant species, our data demonstrate that tentoxin production by C. miyabeanus affects symptom development.


Assuntos
Ascomicetos/genética , Oryza/microbiologia , Peptídeos Cíclicos/genética , Doenças das Plantas/microbiologia , Fatores de Virulência/genética , Ascomicetos/crescimento & desenvolvimento , Ascomicetos/patogenicidade , Cromatografia Líquida de Alta Pressão , Sequência Conservada , Proteínas Fúngicas/genética , Proteínas Fúngicas/metabolismo , Deleção de Genes , Genes Fúngicos , Peptídeos Cíclicos/química , Peptídeos Cíclicos/metabolismo , Reprodutibilidade dos Testes , Homologia de Sequência de Aminoácidos , Esporos Fúngicos/fisiologia , Espectrometria de Massas em Tandem , Fatores de Virulência/metabolismo
13.
Mol Plant Microbe Interact ; 28(10): 1130-41, 2015 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-26168137

RESUMO

The Sfp-type 4'-phosphopantetheinyl transferase Ppt1 is required for activation of nonribosomal peptide synthetases, including α-aminoadipate reductase (AAR) for lysine biosynthesis and polyketide synthases, enzymes that biosynthesize peptide and polyketide secondary metabolites, respectively. Deletion of the PPT1 gene, from the maize pathogen Cochliobolus heterostrophus and the rice pathogen Cochliobolus miyabeanus, yielded strains that were significantly reduced in virulence to their hosts. In addition, ppt1 mutants of C. heterostrophus race T and Cochliobolus victoriae were unable to biosynthesize the host-selective toxins (HST) T-toxin and victorin, respectively, as judged by bioassays. Interestingly, ppt1 mutants of C. miyabeanus were shown to produce tenfold higher levels of the sesterterpene-type non-HST ophiobolin A, as compared with the wild-type strain. The ppt1 strains of all species were also reduced in tolerance to oxidative stress and iron depletion; both phenotypes are associated with inability to produce extracellular siderophores biosynthesized by the nonribosomal peptide synthetase Nps6. Colony surfaces were hydrophilic, a trait previously associated with absence of C. heterostrophus Nps4. Mutants were decreased in asexual sporulation and C. heterostrophus strains were female-sterile in sexual crosses; the latter phenotype was observed previously with mutants lacking Nps2, which produces an intracellular siderophore. As expected, mutants were albino, since they cannot produce the polyketide melanin and were auxotrophic for lysine because they lack an AAR.


Assuntos
Ascomicetos , Proteínas Fúngicas/genética , Oryza/microbiologia , Doenças das Plantas/microbiologia , Sideróforos/metabolismo , Zea mays/microbiologia , Ascomicetos/enzimologia , Ascomicetos/genética , Ascomicetos/patogenicidade , Ascomicetos/fisiologia , Proteínas de Bactérias/genética , Proteínas de Bactérias/metabolismo , Proteínas Fúngicas/metabolismo , Regulação Fúngica da Expressão Gênica , Ferro/metabolismo , L-Aminoadipato-Semialdeído Desidrogenase/genética , L-Aminoadipato-Semialdeído Desidrogenase/metabolismo , Mutação , Micotoxinas/metabolismo , Estresse Oxidativo , Peptídeo Sintases/genética , Peptídeo Sintases/metabolismo , Fenótipo , Policetídeo Sintases/genética , Policetídeo Sintases/metabolismo , Esporos Fúngicos , Transferases (Outros Grupos de Fosfato Substituídos)/genética , Transferases (Outros Grupos de Fosfato Substituídos)/metabolismo , Virulência
14.
Artigo em Inglês | MEDLINE | ID: mdl-25785488

RESUMO

Maize is one of the major staple foods of Sub-Saharan Africa and is consumed as whole or dehulled grain. In this region, where the environmental conditions favour fungal growth and mycotoxin production, the majority of the population are subsistence consumers who, unfortunately, have little or no access to mycotoxin testing of their food. In an attempt to develop feasible reduction strategies in dietary mycotoxin exposure of the population, a three-factorial design experiment was conducted to examine and compare the efficacy of hand sorting, flotation, dehulling and combinations thereof in removing naturally occurring aflatoxins, fumonisins, nivalenol, deoxynivalenol and alternariol in shelled white maize. Regression analysis was used to determine the significant (p < 0.05) process variables on the removal of mycotoxins from the maize. Results from this experiment indicated that hand sorting had the greatest effect on mycotoxin removal, while flotation yielded the least effect. In particular hand sorting left < 6% of aflatoxin B1 and < 5% of fumonisin B1. Based on these results, hand sorting of maize grains is being recommended as a last line of defence against mycotoxin exposure among subsistence consumers.


Assuntos
Descontaminação/métodos , Contaminação de Alimentos/análise , Manipulação de Alimentos/métodos , Micotoxinas/análise , Zea mays/microbiologia , Análise de Regressão
15.
Food Chem ; 177: 397-404, 2015 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-25660903

RESUMO

An LC-MS/MS method was developed and validated for the detection and quantification of 23 mycotoxins in different varieties of sorghum. The method performance characteristics were as follows: suitable linearity ranges for all 23 mycotoxins with p-value >0.05; limits of detection (1.2-50 µg/kg), limits of quantification (2.5-100 µg/kg), repeatability (RSDr, 7-22%), intermediate precision (RSDR, 14-44%) and apparent recovery (0.2-11%, expressed as bias). The method was applied to analyze 10 samples obtained from retail shops in Belgium (n=8) and Germany (n=2). Nine of the 10 samples (90%) were positive for the following mycotoxins: aflatoxin B1 (50 µg/kg), alternariol monomethyl ether (

Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Micotoxinas/química , Sorghum/química , Espectrometria de Massas em Tandem/métodos , Alemanha , Estrutura Molecular , Sorghum/classificação
16.
Mycotoxin Res ; 31(1): 57-62, 2015 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-25194830

RESUMO

We report an unusual aflatoxin profile in maize and groundnuts from Malawi, with aflatoxin G1 found routinely at equal or even higher levels than aflatoxin B1. Aflatoxin B1 (AFB1) ratio in a contaminated sample is generally greater than 50% of total aflatoxin (sum of aflatoxin B1, B2, G1, and G2). In Malawi, the aflatoxin occurrence ratios were determined by examining LC-MS/MS and HPLC fluorescence detection (FLD) data of 156 naturally contaminated raw maize and 80 groundnut samples collected in 2011 and 2012. Results showed that natural aflatoxin occurrence ratio differed. In 47% of the samples, the concentration of AFG1 was higher than that of AFB1. The mean concentration percentages of AFB1/AFB2/AFG1/AFG2 in reference to total aflatoxins were found to be 47:5:43:5%, respectively. The AFG1 and AFB1 50/50 trend was observed in maize and groundnuts and was consistent for samples collected in both years. If the AFB1 measurement was used to check compliance of total aflatoxin regulatory limit set at 10, 20, 100, and 200 µg/kg with an assumption that AFB1≥50% of the total aflatoxin content, 8, 13, 24, and 26% false negative rates would have occurred respectively. It is therefore important for legislation to consider total aflatoxins rather than AFB1 alone.


Assuntos
Aflatoxinas/análise , Arachis/química , Contaminação de Alimentos/análise , Zea mays/química , Cromatografia Líquida , Análise de Perigos e Pontos Críticos de Controle/métodos , Malaui , Espectrometria de Massas em Tandem
17.
J Chromatogr A ; 1297: 1-11, 2013 Jul 05.
Artigo em Inglês | MEDLINE | ID: mdl-23726353

RESUMO

A reliable and rapid method for the determination of multiple mycotoxins was developed using a QuEChERS (quick, easy, cheap, effective, rugged and safe) based extraction procedure in highly pigmented and complex spice matrices, namely red chilli (Capsicum annum ssp.), black and white pepper (Piper nigrum ssp.). High-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was used for the quantification and confirmation of 17 chemically diversified mycotoxins. Different extraction procedures were studied and optimized in order to obtain better recoveries. Mycotoxins were extracted from the hydrated spices using acidified acetonitrile (1% formic acid), followed by partitioning with NaCl and anhydrous MgSO4; excluding the use of dispersive-solid phase extraction. Significant matrix effect was compensated using the matrix matched calibration curves. Electrospray ionization at positive mode was applied to simultaneously detect all the mycotoxins in a single run time of 20min. Multiple reaction monitoring mode, choosing at least two abundant fragment ions per analyte was applied. Coefficients of determination obtained were in the range of 0.9844-0.9997. Recoveries (ranging from 75% to 117%) were in accordance with the performance criteria required by the European Commission. Intra-day reproducibility ranged from 4% to 22% for most of the mycotoxins. The limit of quantification ranged from 2.3 to 146µgkg(-1). The validated method was finally applied to screen mycotoxins in ten of each spice matrix. Aflatoxins, ochratoxin, fumonisins, sterigmatocystin and citrinin were among the detected analytes. Positive findings were further confirmed using relative ion intensities. The potentiality of the method to be used for confirmatory purposes according to Commission Decision 2002/657/EC was assessed.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Micotoxinas/análise , Especiarias/análise , Espectrometria de Massas em Tandem/métodos , Modelos Lineares , Micotoxinas/isolamento & purificação , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
18.
J Agric Food Chem ; 61(26): 6259-64, 2013 Jul 03.
Artigo em Inglês | MEDLINE | ID: mdl-23782015

RESUMO

An LC-MS/MS method was developed and validated for the determination of deoxynivalenol in wheat dust. Extraction was carried out with acetonitrile/water/acetic acid (79/20/1, v/v/v) followed by a hexane defatting step. Analysis was performed using a Waters Acquity UPLC system coupled to a Quattro Premier XE mass spectrometer. The method was validated according to the criteria mentioned in Commission Decision 2002/657/EC. Due to a high contamination level of wheat dust compared to wheat, limit of detection and limit of quantitation levels of 358 ng/g and 717 ng/g, respectively, were obtained. A small survey was executed on raw wheat materials and their corresponding dust samples (n = 12). The samples were analyzed according to the developed procedure. A linear correlation (R² = 0.941) was found for the deoxynivalenol concentration in dust versus the deoxynivalenol concentration in wheat. Therefore, it would be possible to estimate the cereal contamination through dust contamination.


Assuntos
Poeira/análise , Contaminação de Alimentos , Inspeção de Alimentos/métodos , Micotoxinas/análise , Sementes/química , Tricotecenos/análise , Triticum/química , Bélgica , Farinha/análise , Farinha/economia , Indústria de Processamento de Alimentos/economia , Resíduos Industriais/análise , Resíduos Industriais/economia , Micotoxinas/química , Tricotecenos/química
19.
Artigo em Inglês | MEDLINE | ID: mdl-22150477

RESUMO

The current entrance quality control used in the french fries industry is done based on colour evaluation with a United States Department of Agriculture/Munsell colour chart (after a short frying test, typically 180°C for 3 min). On the basis of a study carried out during two consecutive potato storage seasons, the possibility of a more effective entrance control of the raw potato tubers in order to identify batches of potatoes prone to acrylamide formation was evaluated. The current entrance control was compared to two other colour evaluation methods (CIE L*a*b* colour parameters and a process-specific Agtron analyser) and to reducing sugar content determination. Seasonal variability did not affect the slopes of the linear correlation models, for most of the parameters studied. The determination of colour formation measured by the Agtron methodology and reducing sugar content allowed a better identification of batches of potatoes prone to acrylamide formation compared with the current entrance control. Different scenarios represented by decision trees for quality control measures for incoming potatoes were evaluated while considering the investigation value of 600 µg kg⁻¹ for french fries recently prescribed by the European Commission. Samples were categorised based on predictions of threshold values and acrylamide levels in the final product.


Assuntos
Acrilamida/análise , Contaminação de Alimentos/prevenção & controle , Indústria de Processamento de Alimentos/métodos , Alimentos Congelados/análise , Tubérculos/química , Solanum tuberosum/química , Cor , Árvores de Decisões , Carboidratos da Dieta/análise , União Europeia , Alimentos Congelados/normas , Temperatura Alta/efeitos adversos , Controle de Qualidade , Estações do Ano
20.
Anal Bioanal Chem ; 400(9): 2837-46, 2011 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-21559760

RESUMO

The detection of corticosteroids and sex steroids in samples with no content indication, which are confiscated for forensic investigation, is a challenge in doping analysis. A screening method based on the identification of androgens, estrogens, gestagens, and their esters by means of a mass spectral library, along with a fast ultra-performance liquid chromatography-mass spectrometry (UPLC-MS) method, was recently developed in our lab for the analysis of dietary supplements. However, for forensic investigations, it is important to extend the scope of the method to corticosteroids in various matrices. Therefore, 36 corticosteroids were added to the mass spectral library, and the sample preparation step was modified so that androgens, gestagens, corticosteroids, and their esters could be analyzed with only one injection with the UPLC-MS method. A complementary tool to the existing library identification was found in the extraction of common fragment ions out of the full scan data obtained for the library search. The fragment ion with m/z 147 was found to be a good marker for the detection of steroids. Extra confirmation was obtained from the fragment ions with m/z 135 (for all steroids) and 237 (specific for corticosteroids) or from the fragment ions with m/z 77, 91, and 105. The effectiveness of this approach was evaluated on some samples previously screened for forensic investigation with thin-layer chromatography and confirmed with a targeted gas chromatography-mass spectrometry method. This study shows that the combination of the library identification and the common fragment ions approach can be a valuable tool in the detection of steroids without defining any target at the start of the analysis.


Assuntos
Corticosteroides/análise , Suplementos Nutricionais/análise , Espectrometria de Massas/métodos , Androgênios/análise , Cromatografia Líquida de Alta Pressão/métodos , Doping nos Esportes , Ciências Forenses , Humanos , Progestinas/análise
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