scholarly journals Analysis by LC-MS/MS of polar pesticides in fruits and vegetables using new hybrid stationary phase

MethodsX ◽  
2021 ◽  
Vol 8 ◽  
pp. 101306
Author(s):  
Víctor Cutillas ◽  
Amadeo R. Fernández-Alba
Foods ◽  
2020 ◽  
Vol 9 (5) ◽  
pp. 553
Author(s):  
Lorena Manzano-Sánchez ◽  
José Antonio Martínez-Martínez ◽  
Irene Domínguez ◽  
José Luis Martínez Vidal ◽  
Antonia Garrido Frenich ◽  
...  

Nowadays, highly polar pesticides are not included in multiresidue methods due to their physico-chemical characteristics and therefore, specific analytical methodologies are required for their analysis. Laboratories are still looking for a pluri-residue method that encompasses the largest number of polar pesticides. The aim of this work was the simultaneous determination of ethephon, 2-hydroxyethylphosphonic acid (HEPA), fosetyl aluminum, glyphosate, aminomethylphosphonic acid (AMPA), N-acetyl-glyphosate and N-acetyl-AMPA in tomatoes, oranges, aubergines and grapes. For that purpose, an ultra high performance liquid chromatography (UHPLC) coupled to a high resolution single mass spectrometer Orbitrap-MS were used. Different stationary phases were evaluated for chromatographic separation, and among them, the stationary phase Torus DEA provided the best separation of the selected compounds. The QuPPe method was used for the extraction of the analytes, but slight modifications were needed depending on the matrix. The developed method was validated, observing matrix effect in all matrices. Intra- and inter-day precision were estimated, and relative standard deviation were lower than 19%. Recoveries were satisfactory, and mean values ranged from 70% to 110%. Limits of quantification were between 25 and 100 µg kg−1. Finally, the analytical method was applied to different fruits and vegetables (oranges, tomatoes, aubergines and grapes).


2018 ◽  
Vol 101 (2) ◽  
pp. 352-359 ◽  
Author(s):  
Łukasz Rajski ◽  
Francisco José Díaz Galiano ◽  
Víctor Cutillas ◽  
Amadeo R Fernández-Alba

Abstract Ion chromatography coupled to a quadrupole Orbitrap mass analyzer was used to develop a multiresidue method for the determination of highly polar pesticides and their metabolites (chlorate, perchlorate, fosetyl-aluminum, glyphosate, aminomethylphosphonic acid (AMPA), phosphonic acid, N-acetyl AMPA, and N-acetyl glyphosate) in fruits and vegetables. After extraction with methanol, samples were diluted 5× with water. No derivatization was applied. Pesticides were separated in an anion-exchange column. Water was used as the ion chromatography mobile phase. A gradient was created by increasing the concentration of KOH in the mobile phase. Ion chromatography provided good and stable retention and separation for all studied compounds. All investigated pesticides had an LOQ of 0.01 mg/kg and a linear range of 0.01–0.50 mg/kg. The ion ratio of the m/z ions produced was stable and adequate (deviation <30%) in all cases. The obtained mass errors (always in full-scan MS and MS2 mode) were <0.2 mDa. The high resolution (>100 000) provided by the Orbitrap analyzer with the low m/z ions obtained (e.g., m/z 80) was effective in obtaining low background matrix signals. The influence of postcolumn infusion of organic solvent on sensitivity was investigated. Acetonitrile was found to be more effective than methanol, increasing the sensitivity 3× with respect to water. The method was validated for five vegetable-based matrixes. Both the sample processing and the analytical measurement were very fast. Hence, the methodology is ideal for high-throughput work.


Author(s):  
B. L. Soloff ◽  
T. A. Rado

Mycobacteriophage R1 was originally isolated from a lysogenic culture of M. butyricum. The virus was propagated on a leucine-requiring derivative of M. smegmatis, 607 leu−, isolated by nitrosoguanidine mutagenesis of typestrain ATCC 607. Growth was accomplished in a minimal medium containing glycerol and glucose as carbon source and enriched by the addition of 80 μg/ ml L-leucine. Bacteria in early logarithmic growth phase were infected with virus at a multiplicity of 5, and incubated with aeration for 8 hours. The partially lysed suspension was diluted 1:10 in growth medium and incubated for a further 8 hours. This permitted stationary phase cells to re-enter logarithmic growth and resulted in complete lysis of the culture.


2020 ◽  
Vol 134 (12) ◽  
pp. 1403-1432 ◽  
Author(s):  
Manal Muin Fardoun ◽  
Dina Maaliki ◽  
Nabil Halabi ◽  
Rabah Iratni ◽  
Alessandra Bitto ◽  
...  

Abstract Flavonoids are polyphenolic compounds naturally occurring in fruits and vegetables, in addition to beverages such as tea and coffee. Flavonoids are emerging as potent therapeutic agents for cardiovascular as well as metabolic diseases. Several studies corroborated an inverse relationship between flavonoid consumption and cardiovascular disease (CVD) or adipose tissue inflammation (ATI). Flavonoids exert their anti-atherogenic effects by increasing nitric oxide (NO), reducing reactive oxygen species (ROS), and decreasing pro-inflammatory cytokines. In addition, flavonoids alleviate ATI by decreasing triglyceride and cholesterol levels, as well as by attenuating inflammatory mediators. Furthermore, flavonoids inhibit synthesis of fatty acids and promote their oxidation. In this review, we discuss the effect of the main classes of flavonoids, namely flavones, flavonols, flavanols, flavanones, anthocyanins, and isoflavones, on atherosclerosis and ATI. In addition, we dissect the underlying molecular and cellular mechanisms of action for these flavonoids. We conclude by supporting the potential benefit for flavonoids in the management or treatment of CVD; yet, we call for more robust clinical studies for safety and pharmacokinetic values.


2015 ◽  
Vol 85 (3-4) ◽  
pp. 202-210 ◽  
Author(s):  
Ivona Višekruna ◽  
Ivana Rumbak ◽  
Ivana Rumora Samarin ◽  
Irena Keser ◽  
Jasmina Ranilović

Abstract. Results of epidemiologic studies and clinical trials have shown that subjects following the Mediterranean diet had lower inflammatory markers such as homocysteine (Hcy). Therefore, the aim of this cross-sectional study was to assess female diet quality with the Mediterranean diet quality index (MDQI) and to determine the correlation between MDQI, homocysteine, folate and vitamin B12 levels in the blood. The study participants were 237 apparently healthy women (96 of reproductive age and 141 postmenopausal) between 25 and 93 years. For each participant, 24-hour dietary recalls for 3 days were collected, MDQI was calculated, and plasma Hcy, serum and erythrocyte folate and vitamin B12 levels were analysed. Total MDQI ranged from 8 to 10 points, which represented a medium-poor diet for the subjects. The strength of correlation using biomarkers, regardless of group type, age, gender and other measured parameters, was ranked from best (0.11) to worst (0.52) for olive oil, fish, fruits and vegetables, grains, and meat, in this order. Hcy levels showed the best response among all markers across all groups and food types. Our study shows significant differences between variables of the MDQI and Hcy levels compared to levels of folate and vitamin B12 in participants with medium-poor diet quality, as evaluated according to MDQI scores.


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