Browse
Submit Data
Databases
API
Help

Dataset Information

14 Views

0 Connections

0 Citations

0 Reanalyses

0 Downloads

Omics score: 0

Chromatographic Determination of Total Selenium in Biofortified Allium sp. following Piazselenol Formation and Micro-Solid-Phase Extraction

ABSTRACT: Herein, a method based on selective piazselenol formation is applied for total selenium determination in biofortified Allium species. Piazselenol is formed by reacting Se(IV) with an aromatic diamine, namely 4-nitro-1,2-phenylenediamine, in acidic medium. Samples were digested in a nitric acid/hydrogen peroxide open system, followed by selenate reduction in hydrochloric acid. Reaction conditions were optimized in terms of pH, temperature, reaction time, and other auxiliary reagents for interference removal, namely, EDTA and hydroxylamine. For the extraction of the selectively formed 4-nitro-piazselenol, micro-solid-phase extraction (μSPE) was applied, and the analysis and detection of the corresponding complex was performed by HPLC coupled with DAD. An external standard calibration curve was developed (R2 = 0.9994) with good sensitivity, and was used to calculate the total selenium content from several Allium plants material, with good intermediate precision (RSD% < 16%). The accuracy of the method was evaluated using both, a comparison with an accepted reference method from our previously published data, as well as three certified reference material with recoveries between 84–126%. The limit of detection was determined to be 0.35 μg/g (in solids) and 1.1 μg/L (in solution), while the limit of quantification was 1.07 μg/g and 3.4 μg/L (in solution). Using the proposed method, selenium content can be quickly and accurately determined in several types of samples. In addition, this study present experimental conditions for overcoming the interferences that might be encountered in selenium determination using piazselenol.

SUBMITTER: Bosca B

PROVIDER: S-EPMC8588065 | biostudies-literature |

REPOSITORIES: biostudies-literature

ACCESS DATA

Json Xml

Similar Datasets

Determination of Volatile Water Pollutants Using Cross-Linked Polymeric Ionic Liquid as Solid Phase Micro-Extraction Coatings.

Project description:Ionic liquids found a wide application in catalysis and extraction due to their unique properties. Herein, ethylene glycol dimethacrylate as the cross-linker and 1-vinyl-3- butylimidazolium tetrafluoroborate as functional monomer via thermally initiated free-radical polymerization was prepared as a novel copolymer solid phase micro-extraction (SPME) coating. A surface modified stainless-steel wire was implemented as the substrate. Factors affecting the extraction performances of the copolymer, including the molar ratio of monomers to cross-linkers, the amount of porogen agent, and polymerization time were evaluated and optimized. To evaluate the extraction performance, five commonly seen polycyclic aromatic hydrocarbons (PAHs) were taken as the analytical targets. The potential factors affecting extraction efficiency were optimized. The as-prepared SPME device, coupled with gas chromatography, was successfully applied for the determination of PAHs in water samples. The wide linear range, low detection limit, good reproducibility, selectivity, and excellent thermal stability indicate the promising application of the newly developed SPME fiber in environmental monitoring as well as in other samples having complex matrices.

| S-EPMC7077427 | biostudies-literature

Microwave-Assisted Extraction Followed by Solid-Phase Extraction for the Chromatographic Analysis of Alkaloids in Stephania cepharantha.

Project description:A procedure involving microwave-assisted extraction (MAE) followed by solid-phase extraction (SPE) was established for the extraction and purification of three bisbenzylisoquinoline alkaloids from Stephania cepharantha, and a reversed-phase high-performance liquid chromatography (HPLC) method was developed for the quantification of the target alkaloids. Chromatographic separation was achieved on a Phenomenex Luna Phenyl-Hexyl column. Prior to the HPLC analysis, the alkaloids were rapidly extracted by an optimized MAE process using 0.01 mol/L hydrochloric acid as the solvent. The MAE extract was subsequently purified by SPE using a cation-exchange polymeric cartridge. The MAE-SPE procedure extracted the three alkaloids with satisfactory recoveries ranging from 100.44 to 102.12%. In comparison with the MAE, Soxhlet and ultrasonic-assisted extractions, the proposed MAE-SPE method showed satisfactory cleanup efficiency. Thus, the validated MAE-SPE-HPLC method is specific, accurate and applicable to the determination of alkaloids in S. cepharantha.

| S-EPMC4885395 | biostudies-literature

Magnetic Micro-Solid-Phase Extraction Using a Novel Carbon-Based Composite Coupled with HPLC-MS/MS for Steroid Multiclass Determination in Human Plasma.

Project description:A micron-sized sorbent, Magn-Humic, has been prepared by humic acids pyrolysis onto silica-coated magnetite. The material was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), thermogravimetric analysis (TGA), and Brunauer, Emmett, and Teller (BET) surface area measurements and applied for simultaneous magnetic solid-phase extraction (MSPE) of glucocorticoids, estrogens, progestogens, and androgens at ng mL-1 levels from human plasma followed by high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS/MS). Due to the low affinity for proteins, steroids extraction was done with no need for proteins precipitation/centrifugation. As highlighted by a design of experiments, MSPE was performed on 250 µL plasma (after 1:4 dilution) by 50 mg Magn-Humic (reusable for eight extractions) achieving quantitative recovery and satisfying clean-up. This was improved by washing (2 mL 2% v/v formic acid) prior to analytes elution by 0.5 mL 1:1 v/v methanol-acetonitrile followed by 0.5 mL methanol; eluate reduction to 0.25 mL compensated the initial sample dilution. The accuracy was assessed in certified blank fetal bovine serum and in human plasma, gaining satisfactory recovery in the range 65-122%, detection limits in the range 0.02-0.3 ng mL-1 (0.8 ng mL-1 for 17-β-estradiol) and suitable inter-day precision (relative standard deviation (RSD) <14%, n = 3). The method was evaluated in terms of selectivity, sensitivity, matrix-effect, instrumental carry-over, and it was applied to human plasma samples.

| S-EPMC8038327 | biostudies-literature

Deep Eutectic Solvent Micro-Functionalized Graphene Assisted Dispersive Micro Solid-Phase Extraction of Pyrethroid Insecticides in Natural Products.

Project description:Deep eutectic solvent micro-functionalized graphene (DES-G) was synthesized and first applied as the adsorbent of dispersive micro solid-phase extraction (DMSPE) to extract five pyrethroid insecticides. In DMSPE, the target analytes were absorbed by DES-G and then desorbed by trace eluent, next, the treated samples were quantified via ultra-high performance liquid chromatography equipped with diode-array detection. A scanning electron microscope, transmission electron microscopy and Fourier transform infrared spectrometer were used to characterize the prepared DES-G. Furthermore, this method was verified under the selected conditions with the precision for retention times ranging from 0.43 to 0.57%, and repeatability ranged from 0.04 to 2.41% for peak areas. The developed method was successfully applied to determine pyrethroid insecticides residues in beebread, Curcuma wenyujin and Dendrobium officinale with the recoveries in the range of 80.9-114.1%.

| S-EPMC6716533 | biostudies-literature

Chromium-based metal organic framework for pipette tip micro-solid phase extraction: an effective approach for determination of methyl and propyl parabens in wastewater and shampoo samples.

Project description:BackgroundA chromium-based metal organic framework was synthesized and employed as an efficient sorbent for pipette tip micro-solid phase extraction and preconcentration of parabens from wastewater and shampoo samples up to sub-ppb level before their spectrophotometric analysis.ResultsFactors affecting preconcentration including volume and type of solvent, amount of sorbent, number of extraction, and volume and pH of samples were optimized employing one-variable-at-a-time and response surface methodology. Obtained analytical characteristics of the method proves its usefulness for analysis of real samples. Linear range of the method for parabens was 1.0-200.0 μg/L. Detection limit of the protocol was 0.24 µg/L for propyl paraben and 0.25 µg/L for methyl paraben. Reproducibility of the protocol defined as % RSD was better than 5.78%. Synthesized adsorbent can be re-used for at least 20 extractions.ConclusionThe method showed a good detection limit and precision for determination of methyl- and propyl-paraben in wastewater and shampoo samples.

| S-EPMC8571821 | biostudies-literature

Extraction and Chromatographic Determination of Shikimic Acid in Chinese Conifer Needles with 1-Benzyl-3-methylimidazolium Bromide Ionic Liquid Aqueous Solutions.

Project description:An ionic liquids-based ultrasound-assisted extraction (ILUAE) method was successfully developed for extracting shikimic acid from conifer needles. Eleven 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were investigated and 1-benzyl-3-methylimidazolium bromide solution was selected as the solvent. The conditions for ILUAE, including the ionic liquid concentration, ultrasound power, ultrasound time, and liquid-solid ratio, were optimized. The proposed method had good recovery (99.37%-100.11%) and reproducibility (RSD, n = 6; 3.6%). ILUAE was an efficient, rapid, and simple sample preparation technique that showed high reproducibility. Based on the results, a number of plant species, namely, Picea koraiensis, Picea meyeri, Pinus elliottii, and Pinus banksiana, were identified as among the best resources of shikimic acid.

| S-EPMC3980885 | biostudies-literature

Analysis of Tomato Carotenoids: Comparing Extraction and Chromatographic Methods.

Project description:Background: Tomatoes (Solanum lycopersicum) are an economically and nutritionally important crop colored by carotenoids such as lycopene and ?-carotene. Market diversification and interest in the health benefits of carotenoids has created the desire in plant, food, and nutritional scientists for improved extraction and quantification protocols that avoid the analytical bottlenecks caused by current methods. Objective: Our objective was to compare standard and rapid extraction as well as chromatographic separation methods for tomato carotenoids. Method: Comparison was based on accuracy and the ability to discriminate between alleles and genetic backgrounds. Estimates of the contribution to variance in the presence of genetic and environmental effects were further used for comparison. Selections of cherry and processing tomatoes with varying carotenoid profiles were assessed using both established extraction and HPLC-diode array detector (HPLC-DAD) methods and rapid extraction and ultra-HPLC-DAD (UHPLC-DAD) protocols. Results: Discrimination of alleles in samples extracted rapidly (<5 min/sample) was similar to samples extracted using a standard method (10 min/sample), although carotenoid concentrations were lower due to reduced extraction efficiency. Quantification by HPLC-DAD (21.5 min/sample) and UHPLC-DAD (4.2 min/sample) were comparable, but the UHPLC-DAD method could not separate all carotenoids and isomers of tangerine tomatoes. Random effects modeling indicated that extraction and chromatographic methods explained a small proportion of variance compared with genetic and environmental sources. Conclusions: The rapid extraction and UHPLC-DAD methods could enhance throughput for some applications compared with standard protocols.

| S-EPMC7077994 | biostudies-literature

Ultrasound-assisted dispersive micro-solid phase extraction using molybdenum disulfide supported on reduced graphene oxide for energy dispersive X-ray fluorescence spectrometric determination of chromium species in water.

Project description:Molybdenum disulfide (MoS2) was supported on graphene oxide (GO) by hydrothermal method. The resulting nanocomposite (MoS2-rGO) was characterized by X-ray photoelectron spectroscopy, scanning electron microscopy, and transmission electron microscopy. The experiments show that at pH 2, MoS2-rGO has a great affinity for adsorption of hexavalent chromium ions while Cr(III) ions remain in aqueous sample. In the adsorption process, the dominant role plays chemisorption. The determined adsorption capacity is 583.5 mg g-1. Parameters affecting the extraction process, namely sample pH, sample volume, contact time, and matrix ions, were investigated by sequential batch tests. Under optimal conditions (pH 2, sample volume 50 mL, sonication time 10 min, adsorbent mass 1 mg), the calibration curve covers the 1-200 ng mL-1 range with a correlation coefficient (R2) of 0.998. The recovery of the method is 97 ± 3%. Other data of merit include a relative standard deviation of < 3.5%, enrichment factor of 3350, and detection limit of 0.050 ng mL-1. The accuracy of the method was confirmed by analysis of the reference materials QC1453 (chromium VI in drinking water) and QC3015 (chromium VI in seawater). The method was successfully applied to chromium speciation in water samples, including high salinity ones. The concentration of Cr(III) was calculated as the difference between the total concentration of chromium (after oxidation of Cr(III) to Cr(VI) with potassium permanganate) and the initial Cr(VI) content.Graphical abstract Schematic presentation of a method for determination of chromium species by energy dispersive X-ray fluorescence spectrometry after preconcentration on molybdenum disulfide supported on reduced graphene oxide.

| S-EPMC7467914 | biostudies-literature

Determination of Thyreostats in Urine Using Supported Liquid Extraction and Mixed-Mode Cation-Exchange Solid-Phase Extraction: Screening and Confirmatory Methods.

Project description:The application of thyreostats in livestock has been banned in the European Union since 1981, but these drugs are currently in the focus due to the natural occurrence of thiouracil (TU). Studies have been published on TU contamination in urine samples of animal and human origins without any drug administration of it. This paper presents new analytical methods to analyze thyreostats to support the legislation on the recommended concentration (RC) levels of these drugs. Both screening and confirmatory methods are developed for analyzing thyreostats in porcine and bovine urines using a liquid chromatography-tandem mass spectrometry technique. The new methods include a chemical derivatization with 3-iodobenzyl bromide, followed by novel purification approaches using supported liquid extraction and mixed-mode cation-exchange solid-phase extraction (SPE) for screening and confirmatory purposes, respectively. The optimized derivatization in combination with the cation-exchange SPE gives high sensitivity and reducing matrix effect of the analysis. The methods are validated in accordance with the guidelines for the validation of screening methods and European Commission Decision 2002/657/EC. The confirmatory method is used in the national monitoring plan. The detected levels of TU in urine samples are below the currently applicable RC level (10 μg L-1).

| S-EPMC6454509 | biostudies-literature

Determination of fungal activity in modified wood by means of micro-calorimetry and determination of total esterase activity.

Project description:Beech and pine wood blocks were treated with 1,3-dimethylol-4,5-dihydroxyethylen urea (DMDHEU) to increasing weight percent gains (WPG). The resistance of the treated specimens against Trametes versicolor and Coniophora puteana, determined as mass loss, increased with increasing WPG of DMDHEU. Metabolic activity of the fungi in the wood blocks was assessed as total esterase activity (TEA) based on the hydrolysis of fluorescein diacetate and as heat or energy production determined by isothermal micro-calorimetry. Both methods revealed that the fungal activity was related with the WPG and the mass loss caused by the fungi. Still, fungal activity was detected even in wood blocks of the highest WPG and showed that the treatment was not toxic to the fungi. Energy production showed a higher consistency with the mass loss after decay than TEA; higher mass loss was more stringently reflected by higher heat production rate. Heat production did not proceed linearly, possibly due to the inhibition of fungal activity by an excess of carbon dioxide.

| S-EPMC2469595 | biostudies-other

OmicsDI is part of the ELIXIR infrastructure

OmicsDI is an Elixir interoperability service. Learn more ›

Tweets

OmicsDI Databases

PRIDE
PeptideAtlas
MassIVE
JPOST Repository
Physiome Model Repository

EGA
EVA
ENA
LINCS
PAXDB
Cell Collective

MetaboLights
Metabolomics Workbench
MetabolomeExpress
GNPS
BioModels
FAIRDOMHub

ArrayExpress
dbGaP
ExpressionAtlas
GEO
NODE

Information

Databases
Help
API
Contact us
Code on GitHub
Terms of use
Submit Data