scholarly journals Silica Xerogel Doped with Iron(III) as Sensor Material for Salicylhydroxamic Acid Determination in Urine

Gels ◽  
2021 ◽  
Vol 7 (3) ◽  
pp. 143
Author(s):  
Maria A. Morosanova ◽  
Vitaliy A. Kovalev ◽  
Elena I. Morosanova
Keyword(s):  
Biological Samples ◽  
Solid Phase ◽  
Total Pore Volume ◽  
Bet Surface Area ◽  
Silica Xerogel ◽  
Silica Xerogels ◽  
Salicylhydroxamic Acid ◽  
Sensor Material ◽  
Solid Phase Spectrophotometry ◽  
First Time

Salicylhydroxamic acid (SHA) is used as antimicrobic medicine and its concentration has to be monitored in urine. For the first time, silica xerogels doped with iron(III) have been proposed as sensor materials for SHA determination in biological samples. Three xerogels with iron(III) content in the range of 0.04–1.74% wt have been synthesized. BET surface area of these xerogels has varied in the range of 696–529 m2/g and total pore volume has varied in the range of 0.92–0.23 cm3/g. Complex formation between immobilized iron(III) and salicylhydroxamic acid has been investigated with solid phase spectrophotometry and IR spectroscopy. Orange-brown iron(III)-SHA complex with 1:1 stoichiometry is formed at pH 1–4 with half-reaction time of 17 min. Silica xerogel doped with 0.33% wt iron(III)) has been used as sensor material for SHA solid phase spectrophotometric determination (LOD 1.4 mg/L (n = 3), analytical range 4–230 mg/L). Proposed sensor material has been applied for SHA determination in biological samples of synthetic and human urine. The proposed procedure is characterized by a good level of accuracy (recovery values 97–120%) and precision (RSD values 4–9%) and can be recommended for pharmacokinetic–pharmacodynamic studies of hydroxamic acid-based medications.

scholarly journals Silica and Silica–Titania Xerogels Doped with Iron(III) for Total Antioxidant Capacity Determination

Materials ◽  
2021 ◽  
Vol 14 (8) ◽  
pp. 2019
Author(s):  
Maria A. Morosanova ◽  
Ksenia V. Chaikun ◽  
Elena I. Morosanova
Keyword(s):  
Antioxidant Capacity ◽  
Surface Area ◽  
Total Antioxidant Capacity ◽  
Solid Phase ◽  
Bet Surface Area ◽  
Sensor Material ◽  
Total Antioxidant ◽  
Sensor Materials ◽  
Ascorbic Acids ◽  
Capacity Determination

In order to design a sensor material for total antioxidant capacity determination we have prepared silica and silica–titania xerogels doped with iron(III) and modified with 1,10-phenanthroline. Titanium(IV) tetraethoxyde content in the precursors (titanium(IV) tetraethoxyde and tetraethyl orthosilicate) mixtures has been varied from 0 to 12.5% vol. Iron(III) concentrations in sol has been varied from 1 to 100 mM. The increase of titanium(IV) content has led to a decrease in BET surface area and average pore diameter and an increase of micropore surface area and volume, which has resulted in better iron(III) retention in the xerogels. Iron(III), immobilized in the xerogel matrix, retains its ability to form complexes with 1,10-phenanthroline and to be reduced to iron(II). Static capacities for 1,10-phenanthroline have been determined for all the iron(III) doped xerogels (0.207 mmol/g–0.239 mmol/g) and they are not dependent on the iron(III) content. Sensor materials—xerogels doped with iron(III) and modified with 1,10-phenanthroline—have been used for antioxidants (catechol, gallic and ascorbic acids, and sulphite) solid phase spectrophotometric determination. Limits of detection for catechol, gallic and ascorbic acids, and sulphite equal 7.8 × 10−6 M, 5.4 × 10−6 M, 1.2 × 10−5 M, and 3.1 × 10−4 M, respectively. The increase of titanium(IV) content in sensor material has led to an increase of the reaction rate and the sensitivity of determination. Proposed sensor materials have been applied for total antioxidant capacity (in gallic acid equivalents) determination in soft beverages, have demonstrated high stability, and can be stored up to 6 months at room temperature.

Magnetic mixed hemimicelle solid-phase extraction based on mixed hemi-/ad-micelle SDS-coated magnetic nanoparticles Fe2-xAlxO3 (x = 0.4) for the fluorimetric determination of carvedilol in biological samples

2017 ◽  
Vol 95 (5) ◽  
pp. 512-519 ◽  
Author(s):  
Juanli Du ◽  
Hao Wu ◽  
Xiaohui Du ◽  
Zhimin Zhao ◽  
Xin Zhao ◽  
...  
Keyword(s):  
Magnetic Nanoparticles ◽  
Solid Phase Extraction ◽  
Biological Samples ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Phase Extraction ◽  
Fluorimetric Determination ◽  
First Time ◽  
Efficient Adsorbent

Mixed hemi-/ad-micelle SDS-coated magnetic nanoparticles (Fe2-xAlxO3 (x = 0.4)) were used as an efficient adsorbent for the extraction and preconcentration of carvedilol (CVD) based on magnetic mixed hemimicelle solid-phase extraction. The Fe2-xAlxO3 magnetic nanoparticles not only have better stability and resistance to acidity, as well as alkalinity, but also are easy to prepare, inexpensive, and environmentally friendly. Several parameters that affected the extraction efficiency were investigated, including the type and volume of desorption solvent, extraction and desorption times, pH of the solution, zeta potential, and amounts of adsorbent and surfactant. Under the optimized extraction conditions, the developed method showed good linearity (R2 = 0.9998) within the range of 0.02–2.7 ng mL−1, and the limit of detection was 0.009 ng mL−1. The spiked recoveries of CVD in urine and plasma samples ranged from 101.50% to 111.00%. To the best of our knowledge, this is the first time that a mixed hemi-/ad-micelle solid-phase extraction method based on magnetic separation and nanoparticles has been used as a simple and sensitive method for the monitoring of CVD in biological samples.

scholarly journals The Effect of Surfactant-Modified Montmorillonite on the Cross-Linking Efficiency of Polysiloxanes

Materials ◽  
2021 ◽  
Vol 14 (10) ◽  
pp. 2623
Author(s):  
Monika Wójcik-Bania ◽  
Jakub Matusik
Keyword(s):  
Total Pore Volume ◽  
Cross Linking ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
The Cross ◽  
Chain Lengths ◽  
First Time ◽  
Substituent Influence ◽  
Benzyl Substituent

Polymer–clay mineral composites are an important class of materials with various applications in the industry. Despite interesting properties of polysiloxanes, such matrices were rarely used in combination with clay minerals. Thus, for the first time, a systematic study was designed to investigate the cross-linking efficiency of polysiloxane networks in the presence of 2 wt % of organo-montmorillonite. Montmorillonite (Mt) was intercalated with six quaternary ammonium salts of the cation structure [(CH3)2R’NR]+, where R = C12, C14, C16, and R’ = methyl or benzyl substituent. The intercalation efficiency was examined by X-ray diffraction, CHN elemental analysis, and Fourier transform infrared (FTIR) spectroscopy. Textural studies have shown that the application of freezing in liquid nitrogen and freeze-drying after the intercalation increases the specific surface area and the total pore volume of organo-Mt. The polymer matrix was a poly(methylhydrosiloxane) cross-linked with two linear vinylsiloxanes of different siloxane chain lengths between end functional groups. X-ray diffraction and transmission electron microscopy studies have shown that the increase in d-spacing of organo-Mt and the benzyl substituent influence the degree of nanofillers’ exfoliation in the nanocomposites. The increase in the degree of organo-Mt exfoliation reduces the efficiency of hydrosilylation reaction monitored by FTIR. This was due to physical hindrance induced by exfoliated Mt particles.

The Application of Molecularly Imprinted Polymers to Solid-Phase Extraction

2014 ◽  
Vol 893 ◽  
pp. 283-286
Author(s):  
Hong Ying Pei ◽  
Gui Jun Shen ◽  
Yu Du
Keyword(s):  
Solid Phase Extraction ◽  
Molecularly Imprinted Polymers ◽  
Biological Samples ◽  
Solid Phase ◽  
Phase Extraction ◽  
Molecularly Imprinted ◽  
Imprinted Polymers ◽  
Structural Analogues ◽  
Environmental And Biological Samples

A benefit of imprinted polymers is the possibility to prepare sorbents with selectivity pre-determined for a particular substance, or group of structural analogues. The application most close to a wider acceptance is probably that of solid phase extraction for clean-up of environmental and biological samples. The technique of molecularly imprinted polymers to solid phase extraction (MISPE) is performance and high selectively, compared with traditional sorbents. In this paper, the preparation and application of MIPs would be reviewed.

scholarly journals Preparation of High-Performance Activated Carbon from Coffee Grounds after Extraction of Bio-Oil

Molecules ◽  
2021 ◽  
Vol 26 (2) ◽  
pp. 257
Author(s):  
Jie Ren ◽  
Nanwei Chen ◽  
Li Wan ◽  
Guojian Li ◽  
Tao Chen ◽  
...  
Keyword(s):  
Activated Carbon ◽  
High Performance ◽  
Average Pore Size ◽  
Total Pore Volume ◽  
Micropore Volume ◽  
Bet Surface Area ◽  
Average Pore ◽  
Activation Temperature ◽  
Coffee Grounds ◽  
Bio Oil

In this study, a new method for economical utilization of coffee grounds was developed and tested. The resulting materials were characterized by proximate and elemental analyses, thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and N2 adsorption–desorption at 77 K. The experimental data show bio-oil yields reaching 42.3%. The optimal activated carbon was obtained under vacuum pyrolysis self-activation at an operating temperature of 450 °C, an activation temperature of 600 °C, an activation time of 30 min, and an impregnation ratio with phosphoric acid of 150 wt.%. Under these conditions, the yield of activated carbon reached 27.4% with a BET surface area of 1420 m2·g−1, an average pore size of 2.1 nm, a total pore volume of 0.747 cm3·g−1, and a t-Plot micropore volume of 0.428 cm3·g−1. In addition, the surface of activated carbon looked relatively rough, containing mesopores and micropores with large amounts of corrosion pits.

Sign in / Sign up

Export Citation Format

Share Document