Occurrence of mono- and di-glycosylated conjugates of T-2 and HT-2 toxins in naturally contaminated cereals

2012 ◽  
Vol 5 (3) ◽  
pp. 231-240 ◽  
Author(s):  
Z. Veprikova ◽  
M. Vaclavikova ◽  
O. Lacina ◽  
Z. Dzuman ◽  
M. Zachariasova ◽  
...  

An increasing incidence of T-2 and HT-2 toxins (T-2 and HT-2) representing group A trichothecenes has been observed in Fusarium infected small grain cereals in the last decade. Quite recently, the existence of glucosides of T-2 and HT-2 has also been proved next to the common parent forms. There is a strong desire to deepen the knowledge of the occurrence of these conjugates and the possibilities of their analytical determination. A new analytical procedure has been developed for monitoring T-2/HT-2 conjugates in cereal samples. Four different sample preparation methods based on crude acetonitrile:water extraction, QuEChERS, solid phase extraction and immunoaffinity clean-up, were tested. The latter approach employing dedicated immunoaffinity cross-reactive cartridges was shown to be the best option for selective isolation and pre-concentration of the target conjugated analytes. The samples obtained in this way were examined by ultra-high performance liquid chromatography hyphenated to high resolution tandem mass spectrometry that enabled the confirmation of the presence of conjugated T-2 and HT-2. In addition to mono-glycosylated forms of T-2 and HT-2 detected in naturally contaminated barley, wheat and oats, we have also documented for the first time the existence of diglucosides of HT-2 in barley.

Molecules ◽  
2018 ◽  
Vol 23 (11) ◽  
pp. 2869 ◽  
Author(s):  
Iván Taima-Mancera ◽  
Priscilla Rocío-Bautista ◽  
Jorge Pasán ◽  
Juan Ayala ◽  
Catalina Ruiz-Pérez ◽  
...  

Four metal-organic frameworks (MOFs), specifically UiO-66, UiO-66-NH2, UiO-66-NO2, and MIL-53(Al), were synthesized, characterized, and used as sorbents in a dispersive micro-solid phase extraction (D-µSPE) method for the determination of nine pollutants of different nature, including drugs, phenols, polycyclic aromatic hydrocarbons, and personal care products in environmental waters. The D-µSPE method, using these MOFs as sorbents and in combination with high-performance liquid chromatography (HPLC) and diode-array detection (DAD), was optimized. The optimization study pointed out to UiO-66-NO2 as the best MOF to use in the multi-component determination. Furthermore, the utilization of isoreticular MOFs based on UiO-66 with the same topology but different functional groups, and MIL-53(Al) to compare with, allowed us for the first time to evaluate the influence of such functionalization of the ligand with regards to the efficiency of the D-µSPE-HPLC-DAD method. Optimum conditions included: 20 mg of UiO-66-NO2 MOF in 20 mL of the aqueous sample, 3 min of agitation by vortex and 5 min of centrifugation, followed by the use of only 500 µL of acetonitrile as desorption solvent (once the MOF containing analytes was separated), 5 min of vortex and 5 min of centrifugation. The validation of the D-µSPE-HPLC-DAD method showed limits of detection down to 1.5 ng·L−1, average relative recoveries of 107% for a spiked level of 1.50 µg·L−1, and inter-day precision values with relative standard deviations lower than 14%, for the group of pollutants considered.


2020 ◽  
Vol 12 (16) ◽  
pp. 2114-2122
Author(s):  
Idera Fabunmi ◽  
Natalie Sims ◽  
Kathryn Proctor ◽  
Aderonke Oyeyiola ◽  
Temilola Oluseyi ◽  
...  

This reports for the first time a simple and robust approach in determining pharmaceuticals in different fish species in Nigeria.


2012 ◽  
Vol 56 (3) ◽  
pp. 329-333 ◽  
Author(s):  
Ewelina Patyra ◽  
Ewelina Kowalczyk ◽  
Krzysztof Kwiatek

Abstract High performance liquid chromatography method with diode array detection (HPLC-DAD) was developed and optimised for the determination of tetracyclines (TCs) in medicated feedingstuffs. The extraction of the analyte from feedingstuffs was performed with Na2EDTA-McIlvaine buffer (pH 2.5 and pH 4). The extracts were cleaned up by solid phase extraction using octadecyl cartridges (C18). The samples were dried up and redissolved in the mixture of oxalic acid and methanol. Separation was performed on reserved phase column (Phenomenex C18, 250 x 4.6 mm, 5 μm) by multistep gradient elution, which provided better chromatographic separation. The analysis was performed at a wavelength of 390 nm. Validation study of the method revealed that all obtained calibration curves showed good linearity R= 0.9985 for doxycycline (DC) and R= 0.9981 for chlorotetracycline (CTC) over the range of 25-2,000 mg/kg. The analytical procedure was successfully adapted for quantitative determination of DC and CTC in medicated feedingstuff samples. Validation included determination of specificity, linearity, and repeatability. Mean recovery for spiked samples was 93.1% for CTC and 93.2% for DC. The results of validation of the analytical procedure proved that presented method is efficient, precise and useful for quantification of DC and CTC in medicated feedingstuffs.


2013 ◽  
Vol 469 ◽  
pp. 444-449
Author(s):  
Yu Zi Liu ◽  
Ying Hao Xing ◽  
Jun Wu

In this study, High Performance Liquid Chromatography (HPLC), combined with Triple Quadruple mass Spectrometry (QQQ) were developed and applied in the analysis of 16 phthalic acid esters (PAEs) in the common drinking water. Qualitative and quantitative analysis were carried out by Multiple Reaction Monitoring (MRM). The method, combined with Solid Phase Extraction, was established to detect the PAEs in drinking water. As showed by the results, 16 PAEs had a good linearity in the range of 1.14~101.4μg/L, with correlation coefficient between 0.996~0.999. The mean recoveries were in the range of 87.53~131.37%, with the relative standard deviation be 0.71~5.09%. The limit of quantification (LOQ) of 16 PAEs were between 1.14~32.51μg/L, with the limit of detection (LOD) be 0.34~10.67μg/L. There were five PAEs which were detected in the range of <1.7~17.2μg/L in bottled water. Some products have some PAEs which havent been shown in the national or the international standard of the drinking water.


2020 ◽  
Vol 16 (5) ◽  
pp. 776-780
Author(s):  
Behrouz Akbari-adergani ◽  
Asghar Ahmadi ◽  
Gholamreza Jahedkhanki ◽  
Ramin N. Nodehi ◽  
Parisa Sadighara

Background: Due to the heating of amino acids with edible oils to high temperatures, different amounts of acrylamide are produced. Objective: The purpose of this study was to compare the level of acrylamide in the tahdig of bread and tahdig of potato prepared with the common liquid and solid edible oils, including sunflower, corn, canola, frying oil and solid oils. Methods: The tahdig of bread and potato was prepared under the same temperature and time with different oils. Acrylamide isolation was performed on a solid-phase extraction (SPE) cartridge and acrylamide was determined using High-performance liquid chromatography (HPLC). Results: The highest amount of acrylamide was obtained with sunflower oil in the tahdig of potato (194.091 mg/Kg) and the lowest amount of acrylamide was obtained with solid oil in the tahdig of bread (48.54 mg/Kg). For all the oils, the acrylamide content of the tahdig of potato was higher than bread. Conclusion: This study clearly demonstrated the involvement of the kind of oils in the formation of acrylamide in the tahdig of bread.


2020 ◽  
Vol 12 (39) ◽  
pp. 4798-4805
Author(s):  
Donghao Liu ◽  
Jun Peng ◽  
Li Chen ◽  
Yan Zhang ◽  
Xiaoyang Han ◽  
...  

Tyrosine kinase inhibitors were detected by MCN/BIF-20, and this is the first time that BIFs were used for solid-phase extraction.


2019 ◽  
Author(s):  
Kent Griffith ◽  
Clare Grey

Nb18W8O69 (9Nb2O5×8WO3) is the tungsten-rich end-member of the Wadsley–Roth crystallographic shear (cs) structures within the Nb2O5–WO3 series. It has the largest block size of any known, stable Wadsley–Roth phase, comprising 5 ´ 5 units of corner-shared MO6 octahedra between the shear planes, giving rise to 2 nm ´ 2 nm blocks. Rapid lithium intercalation is observed in this new candidate battery material and 7Li pulsed field gradient nuclear magnetic resonance spectroscopy – measured in a battery electrode for the first time at room temperature – reveals superionic lithium conductivity. In addition to its promising rate capability, Nb18W8O69 adds a piece to the larger picture of our understanding of high-performance Wadsley–Roth complex metal oxides.


2020 ◽  
Vol 62 ◽  
pp. 32-38
Author(s):  
E. A. Dolmatov ◽  
R. B. Borzayev ◽  
A. N. Shaipov

The results of the study of the duration of the juvenile period of indigenous Chechen willow leaf pear genotypes (Pyrus salicifolia Pall.) are given in connection with the acceleration of the breeding process and the use of selected forms in pear breeding for high precocity. The studies were carried out in 2016-2019 at OOO “Orchards of Chechnya” in accordance with the Agreement on creative cooperation with the Russian Research Institute of Fruit Crop Breeding. The work was carried out in accordance with generally accepted programs and methods. The objects of the study were one-year and two-year-old pear seedlings obtained from sowing seeds of selected dwarf and low-growing local Chechen forms of willow pear (P. salicifolia Pall.), laying fruit buds on annual growths and seedlings of Caucasian pear (P. caucasica Fed.), 20 500 pcs. of each specie. The aim of the research was to study the potential of precocity of willow pear seedlings and to reveal of selected forms with the greatest degree of this trait. Stratified seeds were sown in the sowing department of the OOO “Orchards of Chechnya” production nursery in April, 2017. The seedlings were grown according to the common technology in dryland conditions on the plot with chestnut soil. The first fl owering of plants was noted in the spring, 2019. As a result of the research, for the first time on a large number of the experimental material it was found that in the off spring of the indigenous Chechen willow leaf pear genotypes, the selection of a little more than 2% of seedlings with a very short juvenile period (2 years) was possible. They are of great interest in accelerating the breeding process and in the selection of new pear varieties with high precocity. 20 willow leaf pear genotypes were selected for the further use in breeding for high precocity and as sources of the trait of short juvenile period.


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