scholarly journals Evaluation of Polyvinyl Alcohol/Pectin-Based Hydrogel Disks as Extraction Phase for Determination of Steroidal Hormones in Aqueous Samples by GC-MS/MS

Molecules ◽  
2018 ◽  
Vol 24 (1) ◽  
pp. 40 ◽  
Author(s):  
Naiara M. F. M. Sampaio ◽  
Natara D. B. Castilhos ◽  
Bruno C. da Silva ◽  
Izabel C. Riegel-Vidotti ◽  
Bruno J. G. Silva
Keyword(s):  
Polyvinyl Alcohol ◽  
Solid Phase ◽  
Volume Flow Rate ◽  
Low Cost ◽  
Extraction Procedure ◽  
Aqueous Samples ◽  
Sorbent Phase ◽  
Steroidal Hormones ◽  
17Β Estradiol ◽  
Extraction Phase

A new extraction phase based on hydrogel disks of polyvinyl alcohol (PVOH) and pectin was proposed, characterized and evaluated for the extraction of six steroidal hormones (estriol, estrone, 17β-estradiol, 17α-ethinylestradiol, progesterone, and testosterone) in aqueous samples with subsequent determination by gas chromatography-tandem mass spectrometry (GC-MS/MS) after the derivatization procedure. The developed extraction procedure was based on the solid phase extraction (SPE) technique, but employed hydrogel as the sorbent phase. The effects of several parameters, including the amount and composition of the sorbent phase, pH, sample volume, flow rate, and gel swelling over the extraction efficiency, were evaluated. Gels with lower swelling indexes and larger amounts of sorbent ensured higher extraction yields of analytes. The main benefits of using the PVOH/pectin-based hydrogel as the extraction phase are the ease of synthesis, low-cost preparation, and the possibility of reusing the extraction disks. Limits of quantification of 0.5 μg L−1 for estrone and 17β-estradiol, and 1 μg L−1 for testosterone, 17α-ethinylestradiol, progesterone, and estriol were obtained. Accuracy values ranged from 80% to 110%, while the inter-assay precision ranged from 0.23% to 22.2% and the intra-assay from 0.55% to 12.3%. Since the sorbent phase has an amphiphilic character, the use of hydrogels is promising for the extraction of medium-to-high polarity compounds.

scholarly journals Miniaturized Matrix Solid-Phase Dispersion for the Analysis of Ultraviolet Filters and Other Cosmetic Ingredients in Personal Care Products

Separations ◽  
2019 ◽  
Vol 6 (2) ◽  
pp. 30
Author(s):  
Maria Celeiro ◽  
Lua Vazquez ◽  
J. Pablo Lamas ◽  
Marlene Vila ◽  
Carmen Garcia-Jares ◽  
...  
Keyword(s):  
Solid Phase ◽  
Low Cost ◽  
Extraction Procedure ◽  
Personal Care Products ◽  
Uv Filters ◽  
Personal Care ◽  
Factors Affecting ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Cosmetic Ingredients

A method based on micro-matrix solid-phase dispersion (μ-MSPD) followed by gas-chromatography tandem mass spectrometry (GC–MS/MS) was developed to analyze UV filters in personal care products. It is the first time that MSPD is employed to extract UV filters from cosmetics samples. This technique provides efficient and low-cost extractions, and allows performing extraction and clean-up in one step, which is one of their main advantages. The amount of sample employed was only 0.1 g and the extraction procedure was performed preparing the sample-sorbent column in a glass Pasteur pipette instead of the classic plastic columns in order to avoid plastizicer contamination. Factors affecting the process such as type of sorbent, and amount and type of elution solvent were studied by a factorial design. The method was validated and extended to other families of cosmetic ingredients such as fragrance allergens, preservatives, plasticizers and synthetic musks, including a total of 78 target analytes. Recovery studies in real sample at several concentration levels were also performed. Finally, the green extraction methodology was applied to the analysis of real cosmetic samples of different nature.

scholarly journals A low-cost approach using diatomaceous earth biosorbent as alternative SPME coating for the determination of PAHs in water samples by GC-MS

2018 ◽  
Author(s):  
Naysla Reinert ◽  
Vieira Camila ◽  
Cristian Silveira ◽  
Dilma Budziak ◽  
Eduardo Carasek
Keyword(s):  
Water Samples ◽  
Solid Phase Microextraction ◽  
Diatomaceous Earth ◽  
Solid Phase ◽  
Low Cost ◽  
Gas Chromatography Mass Spectrometry ◽  
Polycyclic Aromatic ◽  
Repeatability And Reproducibility ◽  
Extraction Phase

In this study, the use of recycled diatomaceous earth as the extraction phase in a the solid phase microextraction (SPME) technique for the determination of polycyclic aromatic hydrocarbons (PAHs) in river water samples, with separation/detection performed by gas chromatography-mass spectrometry (GC-MS), is proposed. The optimized extraction conditions are extraction time 70 min at 80 ºC with no addition of salt. The limits of quantification were close to 0.5 μg L-1 with RSD values lower than 25% (n = 3). The linear working range was 0.5 μg L-1 to 25 μg L-1 for all analytes. The method was applied to samples collected from the Itajaí River (Santa Catarina, Brazil) and the RSD values for repeatability and reproducibility were lower than 15% and 17%, respectively. The efficiency of the recycled diatomaceous earth fiber was compared with that of commercial fibers and good results were obtained, confirming that this is a promising option for use as the extraction phase in SPME.

scholarly journals A Low-Cost Approach Using Diatomaceous Earth Biosorbent as Alternative SPME Coating for the Determination of PAHs in Water Samples by GC-MS

Separations ◽  
2018 ◽  
Vol 5 (4) ◽  
pp. 55 ◽  
Author(s):  
Naysla Reinert ◽  
Camila Vieira ◽  
Cristian da Silveira ◽  
Dilma Budziak ◽  
Eduardo Carasek
Keyword(s):  
Water Samples ◽  
Solid Phase Microextraction ◽  
Diatomaceous Earth ◽  
Solid Phase ◽  
Low Cost ◽  
Gas Chromatography Mass Spectrometry ◽  
Polycyclic Aromatic ◽  
Repeatability And Reproducibility ◽  
Extraction Phase

In this study, the use of recycled diatomaceous earth as the extraction phase in solid phase microextraction (SPME) technique for the determination of polycyclic aromatic hydrocarbons (PAHs) in river water samples, with separation/detection performed by gas chromatography-mass spectrometry (GC-MS), is proposed. The optimized extraction conditions are extraction time 70 min at 80 °C with no addition of salt. The limits of quantification were close to 0.5 μg L−1 with RSD values lower than 25% (n = 3). The linear working range was 0.5 μg L−1 to 25 μg L−1 for all analytes. The method was applied to samples collected from the Itajaí River (Santa Catarina, Brazil) and the RSD values for repeatability and reproducibility were lower than 15% and 17%, respectively. The efficiency of the recycled diatomaceous earth fiber was compared with that of commercial fibers and good results were obtained, confirming that this is a promising option to use as the extraction phase in SPME.

Improvement of Ti/RuO2–IrO2 Anode Lifetime and Electrocatalytical Properties by Using an Eco-Friendly Thermal Decomposition Method Using Polyvinyl Alcohol as Solvent

2019 ◽  
Author(s):  
Charlys Bezerra ◽  
Géssica Santos ◽  
Marilia Pupo ◽  
Maria Gomes ◽  
Ronaldo Silva ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Polyvinyl Alcohol ◽  
High Efficiency ◽  
Electrochemical Impedance ◽  
Pechini Method ◽  
Low Cost ◽  
Charge Transfer Resistance ◽  
Transfer Resistance ◽  
Calcination Temperatures ◽  
Service Lifetime

<p>Electrochemical oxidation processes are promising solutions for wastewater treatment due to their high efficiency, easy control and versatility. Mixed metal oxides (MMO) anodes are particularly attractive due to their low cost and specific catalytic properties. Here, we propose an innovative thermal decomposition methodology using <a>polyvinyl alcohol (PVA)</a> as a solvent to prepare Ti/RuO<sub>2</sub>–IrO<sub>2</sub> anodes. Comparative anodes were prepared by conventional method employing a polymeric precursor solvent (Pechini method). The calcination temperatures studied were 300, 400 and 500 °C. The physical characterisation of all materials was performed by X-ray diffraction and scanning electron microscopy coupled with energy dispersive spectroscopy, while electrochemical characterisation was done by cyclic voltammetry, accelerated service lifetime and electrochemical impedance spectroscopy. Both RuO<sub>2</sub> and IrO<sub>2</sub> have rutile-type structures for all anodes. Rougher and more compact surfaces are formed for the anodes prepared using PVA. Amongst temperatures studied, 300 °C using PVA as solvent is the most suitable one to produce anodes with expressive increase in voltammetric charge (250%) and accelerated service lifetime (4.3 times longer) besides reducing charge-transfer resistance (8 times lower). Moreover, the electrocatalytic activity of the anodes synthesised with PVA toward the Reactive Blue 21 dye removal in chloride medium (100 % in 30 min) is higher than that prepared by Pechini method (60 min). Additionally, the removal total organic carbon point out improved mineralisation potential of PVA anodes. Finally, this study reports a novel methodology using PVA as solvent to synthesise Ti/RuO<sub>2</sub>–IrO<sub>2</sub> anodes with improved properties that can be further extended to synthesise other MMO compositions.</p>

scholarly journals Development of UHPLC/Q-TOF Analysis Method to Screen Glycerin for Direct Detection of Process Contaminants 3-Monochloropropane-1,2-diol Esters (3-MCPDEs) and Glycidyl Esters (GEs)

Molecules ◽  
2021 ◽  
Vol 26 (9) ◽  
pp. 2449
Author(s):  
Lauren Girard ◽  
Kithsiri Herath ◽  
Hernando Escobar ◽  
Renate Reimschuessel ◽  
Olgica Ceric ◽  
...  
Keyword(s):  
Renal Failure ◽  
Solid Phase ◽  
Direct Detection ◽  
Screening Method ◽  
Extraction Procedure ◽  
Biodiesel Production ◽  
Food Contaminants ◽  
Exact Mass ◽  
Glycidyl Esters

The U.S. Food and Drug Administration’s (FDA′s) Center for Veterinary Medicine (CVM) has been investigating reports of pets becoming ill after consuming jerky pet treats since 2007. Renal failure accounted for 30% of reported cases. Jerky pet treats contain glycerin, which can be made from vegetable oil or as a byproduct of biodiesel production. Glycidyl esters (GEs) and 3-monochloropropanediol esters (3-MCPDEs) are food contaminants that can form in glycerin during the refining process. 3-MCPDEs and GEs pose food safety concerns, as they can release free 3-MCPD and glycidol in vivo. Evidence from studies in animals shows that 3-MCPDEs are potential toxins with kidneys as their main target. As renal failure accounted for 30% of reported pet illnesses after the consumption of jerky pet treats containing glycerin, there is a need to develop a screening method to detect 3-MCPDEs and GEs in glycerin. We describe the development of an ultra-high-pressure liquid chromatography/quadrupole time-of-flight (UHPLC/Q-TOF) method for screening glycerin for MCPDEs and GEs. Glycerin was extracted and directly analyzed without a solid-phase extraction procedure. An exact mass database, developed in-house, of MCPDEs and GEs formed with common fatty acids was used in the screening.

scholarly journals Improvement of long-term cycling performance of high-nickel cathode materials by ZnO coating

2021 ◽  
Vol 10 (1) ◽  
pp. 210-220
Author(s):  
Fangfang Wang ◽  
Ruoyu Hong ◽  
Xuesong Lu ◽  
Huiyong Liu ◽  
Yuan Zhu ◽  
...  
Keyword(s):  
Electrochemical Performance ◽  
Lithium Ion Batteries ◽  
Solid Phase ◽  
Low Cost ◽  
Specific Capacity ◽  
High Capacity ◽  
Lithium Ion ◽  
Side Reaction ◽  
Chemical Route ◽  
High Nickel

Abstract The high-nickel cathode material of LiNi0.8Co0.15Al0.05O2 (LNCA) has a prospective application for lithium-ion batteries due to the high capacity and low cost. However, the side reaction between the electrolyte and the electrode seriously affects the cycling stability of lithium-ion batteries. In this work, Ni2+ preoxidation and the optimization of calcination temperature were carried out to reduce the cation mixing of LNCA, and solid-phase Al-doping improved the uniformity of element distribution and the orderliness of the layered structure. In addition, the surface of LNCA was homogeneously modified with ZnO coating by a facile wet-chemical route. Compared to the pristine LNCA, the optimized ZnO-coated LNCA showed excellent electrochemical performance with the first discharge-specific capacity of 187.5 mA h g−1, and the capacity retention of 91.3% at 0.2C after 100 cycles. The experiment demonstrated that the improved electrochemical performance of ZnO-coated LNCA is assigned to the surface coating of ZnO which protects LNCA from being corroded by the electrolyte during cycling.

scholarly journals Adsorption of copper ions on Magnolia officinalis residues after solid-phase fermentation with Phanerochaete chrysosporium

2019 ◽  
Vol 17 (1) ◽  
pp. 1173-1184 ◽  
Author(s):  
Fengyun Tao ◽  
Yangping Liu ◽  
Junliang Chen ◽  
Peng Wang ◽  
Qing Huo
Keyword(s):  
Chinese Medicine ◽  
Phanerochaete Chrysosporium ◽  
Solid Phase ◽  
Copper Ions ◽  
Removal Rate ◽  
Low Cost ◽  
Preparation Technique ◽  
Adsorption Enthalpy ◽  
Pseudo Second Order ◽  
Magnolia Officinalis

AbstractThe disposal of residues while manufacturing Chinese medicine has always been an issue that concerns pharmaceutical factories. Phanerochaete chrysosporium was inoculated into the residues of Magnolia officinalis for solid-phase fermentation to enzymatically hydrolyze the lignin in the residues and thus to improve the efficiency of removal of the copper ions from residues for the utilization of residues from Chinese medicine. With the increase in activities of lignin-degrading enzymes, especially during the fermentation days 6 to 9, the removal rate of copper ions using M. officinalis residues increased dramatically. The rate of removal reached the maximum on the 14th day and was 3.15 times higher than the initial value. The rate of adsorption of copper ions on the fermentation-modified M. officinalis residues followed the pseudo-second-order kinetics. The adsorption isotherms were consistent with the Freundlich models. The adsorption enthalpy was positive, indicating that it was endothermic and elevation in temperature was favorable to this adsorption process. The adsorption free energy was negative, implying the spontaneity of the process. The copper ions adsorbed could be effectively recovered using 0.2 M hydrochloric acid solution. After five successive cycles of adsorption-regeneration, the fermentation-modified M. officinalis residues exhibited a stable adsorption capacity and greater reusability. The M. officinalis residues fermented with P. chrysosporium are low-cost and environmentally friendly copper ions adsorbent, and this preparation technique realizes the optimum utilization of Chinese medicine residues.

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