scholarly journals Screening of Regulated and Emerging Mycotoxins in Bulk Milk Samples by High-Resolution Mass Spectrometry

Foods ◽  
2021 ◽  
Vol 10 (9) ◽  
pp. 2025
Author(s):  
Gabriele Rocchetti ◽  
Francesca Ghilardelli ◽  
Francesco Masoero ◽  
Antonio Gallo
Keyword(s):  
Mass Spectrometry ◽  
High Resolution Mass Spectrometry ◽  
Corn Silage ◽  
Feeding System ◽  
Fusarium Mycotoxins ◽  
Milk Samples ◽  
Bulk Milk ◽  
Low Levels ◽  
Contamination Levels ◽  
Resolution Mass

In this work, a retrospective screening based on ultra-high-performance liquid chromatography (UHPLC) coupled with high-resolution mass spectrometry (HRMS) based on Orbitrap-Q-Exactive Focus™ was used to check the occurrence of regulated and emerging mycotoxins in bulk milk samples. Milk samples were collected from dairy farms in which corn silage was the main ingredient of the feeding system. The 45 bulk milk samples were previously analyzed for a detailed untargeted metabolomic profiling and classified into five clusters according to the corn silage contamination profile, namely: (1) low levels of Aspergillus- and Penicillium-mycotoxins; (2) low levels of fumonisins and other Fusarium-mycotoxins; (3) high levels of Aspergillus-mycotoxins; (4) high levels of non-regulated Fusarium-mycotoxins; (5) high levels of fumonisins and their metabolites. Multivariate statistics based on both unsupervised and supervised analyses were used to evaluate the significant fold-change variations of the main groups of mycotoxins detected when comparing milk samples from clusters 3, 4, and 5 (high contamination levels of the corn silages) with cluster 1 and 2 (low contamination levels of the corn silages). Overall, 14 compounds showed a significant prediction ability, with antibiotic Y (VIP score = 2.579), bikaverin (VIP score = 1.975) and fumonisin B2 (VIP score = 1.846) being the best markers. The k-means clustering combined with supervised statistics showed two discriminant groups of milk samples, thus revealing a hierarchically higher impact of the whole feeding system (rather than the only corn silages) together with other factors of variability on the final mycotoxin contamination profile. Among the discriminant metabolites we found some Fusarium mycotoxins, together with the tetrapeptide tentoxin (an Alternaria toxin), the α-zearalenol (a catabolite of zearalenone), mycophenolic acid and apicidin. These preliminary findings provide new insights into the potential role of UHPLC-HRMS to evaluate the contamination profile and the safety of raw milk to produce hard cheese.

scholarly journals Changes of Milk Metabolomic Profiles Resulting from a Mycotoxins-Contaminated Corn Silage Intake by Dairy Cows

Metabolites ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 475
Author(s):  
Gabriele Rocchetti ◽  
Francesca Ghilardelli ◽  
Paolo Bonini ◽  
Luigi Lucini ◽  
Francesco Masoero ◽  
...  
Keyword(s):  
High Performance ◽  
High Resolution Mass Spectrometry ◽  
Milk Composition ◽  
Corn Silage ◽  
Cow Milk ◽  
Fusarium Mycotoxins ◽  
Multivariate Statistical ◽  
Milk Samples ◽  
Chemical Profiles ◽  
Low Levels

In this study, an untargeted metabolomics approach based on ultra-high-performance liquid chromatography coupled with high-resolution mass spectrometry (UHPLC-HRMS) was used for investigating changes in chemical profiles of cow milk considering diets based on mycotoxins-contaminated corn silages. For this purpose, 45 milk samples were classified into five clusters according to the corn silage contamination profile, namely (1) low levels of Aspergillus- and Penicillium-mycotoxins; (2) low levels of fumonisins and other Fusarium-mycotoxins; (3) high levels of Aspergillus-mycotoxins; (4) high levels of non-regulated Fusarium-mycotoxins; (5) high levels of fumonisins and their metabolites, and subsequently analyzed by UHPLC-HRMS followed by a multivariate statistical analysis (both unsupervised and supervised statistical approaches). Overall, the milk metabolomic profile highlighted potential correlations between the quality of contaminated corn silages (as part of the total mixed ration) and milk composition. Metabolomics allowed to identify 628 significant milk metabolites as affected by the five levels of corn silage contamination considered, with amino acids and peptides showing the highest metabolite set enrichment (134 compounds). Additionally, 78 metabolites were selected as the best discriminant of the prediction model built, possessing a variable importance in projection score >1.2. The average Log Fold-Change variations of the discriminant metabolites provided evidence that sphingolipids, together with purine and pyrimidine-derived metabolites were the most affected chemical classes. Also, metabolomics revealed a significant accumulation of oxidized glutathione in milk samples belonging to the silage cluster contaminated by emerging Aspergillus toxins, likely involved in the oxidative imbalance. These preliminary findings provide new insights into the potential role of milk metabolomics to provide chemical indicators of mycotoxins-contaminated corn silage feeding systems.

scholarly journals A rapid multiclass method for antibiotic residues in goat dairy products by UPLC-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry

2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Lu Zhang ◽  
Liang Shi ◽  
Qiang He ◽  
Ying Li
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Electrostatic Field ◽  
High Resolution Mass Spectrometry ◽  
Simultaneous Detection ◽  
Goat Milk ◽  
Veterinary Antibiotics ◽  
Milk Samples ◽  
High Resolution Mass ◽  
Resolution Mass

Abstract Background Sulfanilamides, quinolones, nitroimidazoles, tetracyclines, cephalosporins, macrolides, and β-lactam are common tools in agriculture and can be found in animal-based foods such as goat milk and goat dried milk. To evaluate the risk of these species, reliable analytical methods are needed for accurate concentration determination, especially in goat milk and goat dried milk. Method We describe a method based on PRiME extraction coupled with UPLC-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry to accomplish this task. Result Under optimal conditions, the limit of quantification for all antibiotics was 0.5–100 μg/L in goat milk and goat dried milk samples. The recoveries were 60.6–110.0% for goat milk and 60.1–109.6% for goat dried milk with a coefficient of variation less than 15%. The detection limits were 0.5–1.0 μg/kg. The limits of quantification for the analytes were 5.0–10.0 μg/kg. Finally, the method was used to screen veterinary antibiotics in 50 local goat milk and goat dried milk samples; metronidazole and enrofloxacin were detected in goat milk. Conclusion This method offers good reliability and the capacity for simultaneous detection can be used to detect residual contents and evaluate health risks in goat milk and goat dried milk.

scholarly journals Free Saturated Oxo Fatty Acids (SOFAs) and Ricinoleic Acid in Milk Determined by a Liquid Chromatography-High-Resolution Mass Spectrometry (LC-HRMS) Method

Metabolites ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 46
Author(s):  
Maroula G. Kokotou ◽  
Charikleia S. Batsika ◽  
Christiana Mantzourani ◽  
George Kokotos
Keyword(s):  
Mass Spectrometry ◽  
Fatty Acids ◽  
Liquid Chromatography ◽  
High Resolution ◽  
Ricinoleic Acid ◽  
High Resolution Mass Spectrometry ◽  
Goat Milk ◽  
Milk Samples ◽  
High Resolution Mass ◽  
Resolution Mass

Oxidized saturated fatty acids, containing a hydroxyl or an oxo functionality, have attracted little attention so far. Recent studies have shown that saturated hydroxy fatty acids, which exhibit cancer cell growth inhibition and may suppress β-cell apoptosis, are present in milk. Herein, we present the application of a liquid chromatography-high-resolution mass spectrometry (LC-HRMS) method for the detection and quantification of various saturated oxo fatty acids (SOFAs) previously unrecognized in milk. This robust and rapid analytical method, which involves simple sample preparation and a single 10-min run, revealed the presence of families of oxostearic acids (OSAs) and oxopalmitic acids (OPAs) in milk. 8OSA, 9OSA, 7OSA, 10OSA and 10OPA were found to be the most abundant SOFAs in both cow and goat milk. Higher contents of SOFAs were found in cow milk in comparison to goat milk. Together with SOFAs, ricinoleic acid, which is isobaric to OSA, was detected and quantified in all milk samples, following a “suspect” HRMS analysis approach. This unique natural fatty acid, which is the main component (>90%) of castor oil triglycerides, was estimated at mean content values of 534.3 ± 6.0 μg/mL and 460 ± 8.1 μg/mL in cow and goat milk samples, respectively.

scholarly journals Evaluation of High-Resolution Mass Spectrometry for the Quantitative Analysis of Mycotoxins in Complex Feed Matrices

Toxins ◽  
2019 ◽  
Vol 11 (9) ◽  
pp. 531 ◽  
Author(s):  
Jensen ◽  
de Boevre ◽  
Preußke ◽  
de Saeger ◽  
Birr ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
High Resolution Mass Spectrometry ◽  
Resolving Power ◽  
Fusarium Mycotoxins ◽  
Maize Silage ◽  
Forage Maize ◽  
High Resolution Mass ◽  
Mycotoxin Analysis ◽  
Resolution Mass

The selective and sensitive analysis of mycotoxins in highly complex feed matrices is a great challenge. In this study, the suitability of OrbitrapTM-based high-resolution mass spectrometry (HRMS) for routine mycotoxin analysis in complex feeds was demonstrated by the successful validation of a full MS/data-dependent MS/MS acquisition method for the quantitative determination of eight Fusarium mycotoxins in forage maize and maize silage according to the Commission Decision 2002/657/EC. The required resolving power for accurate mass assignments (<5 ppm) was determined as 35,000 full width at half maximum (FWHM) and 70,000 FWHM for forage maize and maize silage, respectively. The recovery (RA), intra-day precision (RSDr), and inter-day precision (RSDR) of measurements were in the range of 94 to 108%, 2 to 16%, and 2 to 12%, whereas the decision limit (CCα) and the detection capability (CCβ) varied from 11 to 88 µg/kg and 20 to 141 µg/kg, respectively. A set of naturally contaminated forage maize and maize silage samples collected in northern Germany in 2017 was analyzed to confirm the applicability of the HRMS method to real samples. At least four Fusarium mycotoxins were quantified in each sample, highlighting the frequent co-occurrence of mycotoxins in feed.

Exploring the Active Compounds of Traditional Mongolian Medicine Agsirga in Intervention of Novel Coronavirus (2019-nCoV) Based on HPLC-Q-Exactive-MS/MS and Molecular Docking Method

2020 ◽  
Author(s):  
Jie Cheng ◽  
Yuchen Tang ◽  
Baoquan Bao ◽  
Ping Zhang
Keyword(s):  
Mass Spectrometry ◽  
Molecular Docking ◽  
High Resolution ◽  
Mass Spectra ◽  
High Resolution Mass Spectrometry ◽  
Structural Formula ◽  
Active Compounds ◽  
High Resolution Mass ◽  
Q Exactive ◽  
Resolution Mass

<p><a></a><a></a><a></a><a><b>Objective</b></a>: To screen all compounds of Agsirga based on the HPLC-Q-Exactive high-resolution mass spectrometry and find potential inhibitors that can respond to 2019-nCoV from active compounds of Agsirga by molecular docking technology.</p> <p><b>Methods</b>: HPLC-Q-Exactive high-resolution mass spectrometry was adopted to identify the complex components of Mongolian medicine Agsirga, and separated by the high-resolution mass spectrometry Q-Exactive detector. Then the Orbitrap detector was used in tandem high-resolution mass spectrometry, and the related molecular and structural formula were found by using the chemsipider database and related literature, combined with precise molecular formulas (errors ≤ 5 × 10<sup>−6</sup>) , retention time, primary mass spectra, and secondary mass spectra information, The fragmentation regularities of mass spectra of these compounds were deduced. Taking ACE2 as the receptor and deduced compounds as the ligand, all of them were pretreated by discover studio, autodock and Chem3D. The molecular docking between the active ingredients and the target protein was studied by using AutoDock molecular docking software. The interaction between ligand and receptor is applied to provide a choice for screening anti-2019-nCoV drugs.</p> <p><b>Result</b>: Based on the fragmentation patterns of the reference compounds and consulting literature, a total of 96 major alkaloids and stilbenes were screened and identified in Agsirga by the HPLC-Q-Exactive-MS/MS method. Combining with molecular docking, a conclusion was got that there are potential active substances in Mongolian medicine Agsirga which can block the binding of ACE2 and 2019-nCoV at the molecular level.</p>

Determination of quaternary ammonium compounds in food products by the method of ultra-performance liquid chromatography/high resolution mass-spectrometry

2020 ◽  
Vol 86 (8) ◽  
pp. 23-31
Author(s):  
V. G. Amelin ◽  
D. S. Bolshakov
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Quaternary Ammonium ◽  
High Resolution Mass Spectrometry ◽  
Food Products ◽  
Quaternary Ammonium Compounds ◽  
High Resolution Mass ◽  
Ammonium Compounds ◽  
Resolution Mass

The goal of the study is developing a methodology for determination of the residual amounts of quaternary ammonium compounds (QAC) in food products by UHPLC/high-resolution mass spectrometry after water-acetonitrile extraction of the determined components from the analyzed samples. The identification and determination of QAC was carried out on an «UltiMate 3000» ultra-high-performance liquid chromatograph (Thermo Scientific, USA) equipped with a «maXis 4G» high-resolution quadrupole-time-of-flight mass spectrometric detector and an ion spray «ionBooster» source (Bruker Daltonics, Germany). Samples of milk, cheese (upper cortical layer), dumplings, pork, chicken skin and ground beef were used as working samples. Optimal conditions are specified for chromatographic separation of the mixture of five QAC, two of them being a mixture of homologues with a linear structure (including isomeric forms). The identification of QAC is carried out by the retention time, exact mass of the ions, and coincidence of the mSigma isotopic distribution. The limits for QAC detection are 0.1 – 0.5 ng/ml, the determination limits are 1 ng/ml for aqueous standard solutions. The determinable content of QAC in food products ranges within 1 – 100 ng/g. The results of analysis revealed the residual amount of QAC present in all samples, which confirms data of numerous sources of information about active use of QAC-based disinfectants in the meat and dairy industry. The correctness of the obtained results is verified by introduction of the additives in food products at a level of 10 ng/g for each QAC. The relative standard deviation of the analysis results does not exceed 0.18. The duration of the analysis is 30 – 40 min.

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