Ice Concentration Linked with Extractive Stirrer (ICECLES)

Clean water is very important for human health. Therefore, drinking water contamination is a significant research concern, especially with the increasing global population. Some contaminants, such as pesticides, can cause health effects even at low levels. Therefore, trace and ultratrace analysis of contaminants in drinking water is essential. Ultratrace analysis typically requires highly effective sample preparation methods and/or highly sensitive instruments. There are currently advanced sample preparations techniques available to analytical chemists that may allow trace analysis of certain analytes. These include liquid-liquid extraction (LLE), solid phase extraction (SPE), solid phase micro extraction (SPME), and stir bar sorpitive extraction (SBSE). Even though these techniques have advantages, some analytes are still extremely difficult to analyse at the trace and ultratrace concentrations necessary to ensure safe drinking water. Therefore, a novel sample preparation method was developed as a combination of SBSE and FC to allow trace analysis of drinking water samples. The technique, ICE Concentration Linked with Extractive Stirrer (ICECLES), illustrated great advantages for ultra-trace analysis of multiple analytes. Parameters affecting the performance of ICECLES were evaluated using benzaldehyde, such as the initial concentration, stir speed and freeze rate. Extraction at low speeds resulted in higher extraction efficiency. However, the freeze rate and initial concentrations had a minor effect on ICECLES extraction efficiency. ICECLES produced linear range of benzaldehyde from 40-5000 nM, with R2 \u3e 0.999, the accuracy was 100 ± 15%, and the precision was ≤ 16% RSD for the QCs. ICECLES provided greater extraction efficiency, signal enhancement (SE) and lower limits of detection (LOD) compared to SBSE method for each analyte tested. ICECLES was evaluated in five different analytes (2-butanol, benzaldehyde, benzyl Alcohol, dimethyl trisulfide and bromobenzene; with log Kow of 0.61, 1.1, 1.48, 1.87 and 2.9, respectively). ICECLES produced the highest SE for 2-butanol, 474 times than SBSE, and the SE generally correlated with decreasing log Kow. ICECLES was shown to be an excellent sample preparation method for analyzing triazine pesticides from aqueous samples. ICECLES achieved greater SE and extraction efficiency for all pesticides, especially for lower log Kow compounds, with trend: metamitron \u3e deethyl-atrazine \u3e deisopropyl-atrazine \u3e metribuzin \u3e atrazine inversely following the log Kow

Determination of Dimethyl Trisulfide in Rabbit Blood Using Stir Bar Sorptive Extraction Gas Chromatography-mass Spectrometry

Cyanide poisoning by accidental or intentional exposure poses a severe health risk. The current Food and Drug Administration approved antidotes for cyanide poisoning can be effective, but each suffers from specific major limitations concerning large effective dosage, delayed onset of action, or dependence on enzymes generally confined to specific organs. Dimethyl trisulfide (DMTS), a sulfur donor that detoxifies cyanide by converting it into thiocyanate (a relatively nontoxic cyanide metabolite), is a promising next generation cyanide antidote. Although a validated analytical method to analyze DMTS from any matrix is not currently available, one will be vital for the approval of DMTS as a therapeutic agent against cyanide poisoning. Hence, a stir bar sorptive extraction (SBSE) gas chromatography – mass spectrometry (GC–MS) method was developed and validated for the analysis of DMTS from rabbit whole blood. Following acid denaturation of blood, DMTS was extracted into a polydimethylsiloxane-coated stir bar. The DMTS was then thermally desorbed from the stir bar and analyzed by GC–MS. The limit of detection of DMTS using this method was 0.06 μM with dynamic range from 0.5–100 μM. For quality control standards, the precision, as measured by percent relative standard deviation, was below 10%, and the accuracy was within 15% of the nominal concentration. The method described here will allow further investigations of DMTS as a promising antidote for cyanide poisoning

Chitosan@Carboxymethylcellulose/CuO-Co2O3 Nanoadsorbent as a Super Catalyst for the Removal of Water Pollutants

In this work, an efficient nanocatalyst was developed based on nanoadsorbent beads. Herein, carboxymethyl cellulose–copper oxide-cobalt oxide nanocomposite beads (CMC/CuO-Co2O3) crosslinked by using AlCl3 were successfully prepared. The beads were then coated with chitosan (Cs), Cs@CMC/CuO-Co2O3. The prepared beads, CMC/CuO-Co2O3 and Cs@CMC/CuO-Co2O3, were utilized as adsorbents for heavy metal ions (Ni, Fe, Ag and Zn). By using CMC/CuO-Co2O3 and Cs@CMC/CuO-Co2O3, the distribution coefficients (Kd) for Ni, Fe, Ag and Zn were (41.166 and 6173.6 mLg−1), (136.3 and 1500 mLg−1), (20,739.1 and 1941.1 mLg−1) and (86.9 and 2333.3 mLg−1), respectively. Thus, Ni was highly adsorbed by Cs@CMC/CuO-Co2O3 beads. The metal ion adsorbed on the beads were converted into nanoparticles by treating with reducing agent (NaBH4) and named Ni/Cs@CMC/CuO-Co2O3. Further, the prepared nanoparticles-decorated beads (Ni/Cs@CMC/CuO-Co2O3) were utilized as nanocatalysts for the reduction of organic and inorganic pollutants (4-nitophenol, MO, EY dyes and potassium ferricyanide K3[Fe(CN)6]) in the presence of NaBH4. Among all catalysts, Ni/Cs@CMC/CuO-Co2O3 had the highest catalytic activity toward MO, EY and K3[Fe(CN)6], removing up to 98% in 2.0 min, 90 % in 6.0 min and 91% in 6.0 min, respectively. The reduction rate constants of MO, EY, 4-NP and K3[Fe(CN)6] were 1.06 × 10−1, 4.58 × 10−3, 4.26 × 10−3 and 5.1 × 10−3 s−1, respectively. Additionally, the catalytic activity of the Ni/Cs@CMC/CuO-Co2O3 beads was effectively optimized. The stability and recyclability of the beads were tested up to five times for the catalytic reduction of MO, EY and K3[Fe(CN)6]. It was confirmed that the designed nanocomposite beads are ecofriendly and efficient with high strength and stability as catalysts for the reduction of organic and inorganic pollutants

ICE Concentration Linked with Extractive Stirrer (ICECLES)

Trace and ultra-trace analysis can be difficult to achieve, especially for polar, more volatile, and/or thermally unstable analytes. A novel technique, coined ICE Concentration Linked with Extractive Stirrer (ICECLES), may help address this problem. The implementation of ICECLES described here combines stir bar sorptive extraction (SBSE) with freeze concentration (FC), where an aqueous solution is frozen during SBSE in order to concentrate analytes into a polydimethylsiloxane (PDMS) coated stir bar. Five test probe molecules with a range of log Kows (2-butanol, benzyl alcohol, benzaldehyde, dimethyl trisulfide and bromobenzene) were prepared from aqueous solutions using ICECLES. Thermal desorption gas–chromatography mass–spectrometry was then used to quantify these analytes. Parameters affecting the performance of ICECLES (e.g., freeze rate) were evaluated, with extraction at lower speeds resulting in higher extraction efficiencies, whereas the freeze rate and initial analyte concentration only had a minor effect. ICECLES produced much higher extraction efficiencies than SBSE alone, with signal enhancements of up to 474× SBSE. ICECLES also provided excellent reproducibility and lower LODs than SBSE for all compounds tested. ICECLES performed well when used to analyze multiple triazine pesticides and breakdown products in environmental surface waters. Overall, the ICECLES technique was excellent at preparing aqueous samples for trace analysis and shows promise as a novel analytical sample preparation technology

Carboxymethyl cellulose nanocomposite beads as super-efficient catalyst for the reduction of organic and inorganic pollutants

Carboxymethyl cellulose/copper oxide-nickel oxide (CMC/CuO-NiO) nanocomposite beads were prepared by facile, simple and environmentally friendlymethod. Initially, CuO-NiOwas prepared and applied for the catalytic reduction of 4-nitrophenol (4-NP). The results showed that CuO-NiO demonstrate high catalytic activity toward the reduction of 4-NP to 4-aminophenol (4-AP) with a rate constant of 2.97 x 10(-2) s(-1). Further, CuO-NiO were well-dispersed in the polymeric matrix of carboxymethyl cellulose to prepare CMC/CuO-NiO beads. CMC/CuO-NiO nanocomposite beads were also applied to catalyze the reduction of potassium ferrocyanide (K3Fe (CN)(6)), 4-NP, Congo red (CR) and Eosin yellow(EY) in the presence of sodiumborohydride. Experimental data indicated that CMC/CuO-NiO nanocomposite has higher catalytic activity and high rate constant compared to CuO-NiO. The rate constant found to be 6.88 x 10(-2), 6.27 x 10(-2), 1.89 x 10(-2) and 2.43 x 10(-2) for K3Fe(CN)(6), 4-NP, CR and EY, respectively, using 5 mg CMC/CuO-NiO beads. FE-SEM, EDX, FTER, XRD and XPS were used to characterize the nanocomposites. CMC/CuO-NiO beads catalytically reduced up to 95-99% of K3Fe(CN)(6), 4-NP, CR and EY within 40, 60, 120 and 120 s. CMC/CuO-NiO beadswere found more selective for the reduction of 4-NP. The catalytic reduction performance of CMC/CuO-NiO beadswas optimized by studying the influence of different parameters on the catalytic reduction of 4-NP. Hence, the effective and super catalytic performance toward the reduction of different organic and inorganic pollutants makes CMC/CuO-NiO beads a smart material and suitable for numerous scientific and industrial applications and may be used as an alternative to high-cost commercial catalysts. (C) 2020 Elsevier B.V. All rights reserved

Chitosan@Carboxymethylcellulose/CuO-Co₂O₃ Nanoadsorbent as a Super Catalyst for the Removal of Water Pollutants

In this work, an efficient nanocatalyst was developed based on nanoadsorbent beads. Herein, carboxymethyl cellulose–copper oxide-cobalt oxide nanocomposite beads (CMC/CuO-Co2O3) crosslinked by using AlCl3 were successfully prepared. The beads were then coated with chitosan (Cs), Cs@CMC/CuO-Co2O3. The prepared beads, CMC/CuO-Co2O3 and Cs@CMC/CuO-Co2O3, were utilized as adsorbents for heavy metal ions (Ni, Fe, Ag and Zn). By using CMC/CuO-Co2O3 and Cs@CMC/CuO-Co2O3, the distribution coefficients (Kd) for Ni, Fe, Ag and Zn were (41.166 and 6173.6 mLg−1), (136.3 and 1500 mLg−1), (20,739.1 and 1941.1 mLg−1) and (86.9 and 2333.3 mLg−1), respectively. Thus, Ni was highly adsorbed by Cs@CMC/CuO-Co2O3 beads. The metal ion adsorbed on the beads were converted into nanoparticles by treating with reducing agent (NaBH4) and named Ni/Cs@CMC/CuO-Co2O3. Further, the prepared nanoparticles-decorated beads (Ni/Cs@CMC/CuO-Co2O3) were utilized as nanocatalysts for the reduction of organic and inorganic pollutants (4-nitophenol, MO, EY dyes and potassium ferricyanide K3[Fe(CN)6]) in the presence of NaBH4. Among all catalysts, Ni/Cs@CMC/CuO-Co2O3 had the highest catalytic activity toward MO, EY and K3[Fe(CN)6], removing up to 98% in 2.0 min, 90 % in 6.0 min and 91% in 6.0 min, respectively. The reduction rate constants of MO, EY, 4-NP and K3[Fe(CN)6] were 1.06 × 10−1, 4.58 × 10−3, 4.26 × 10−3 and 5.1 × 10−3 s−1, respectively. Additionally, the catalytic activity of the Ni/Cs@CMC/CuO-Co2O3 beads was effectively optimized. The stability and recyclability of the beads were tested up to five times for the catalytic reduction of MO, EY and K3[Fe(CN)6]. It was confirmed that the designed nanocomposite beads are ecofriendly and efficient with high strength and stability as catalysts for the reduction of organic and inorganic pollutants

Green Bio-Analytical Study of Gabapentin in Human Plasma Coupled with Pharmacokinetic and Bioequivalence Assessment Using UPLC-MS/MS

Gabapentin (GAB) is a cyclohexane acetic acid, structurally related to the neurotransmitter gamma-aminobutyric acid (GABA), and considered the principal inhibitory neurotransmitter in the central nervous system (CNS) of mammals. An ultra-performance liquid chromatography–tandem mass spectrophotometry (UPLC-MS/MS) method for assessing pregabalin (PRE) in human plasma, was developed and validated, via PRE usage as an internal standard. The plasma underwent protein precipitation using methanol, prior to analysis. Chromatographic separation was completed using a mobile phase of methanol: 0.1% formic acid solution, (65:35, v/v), at a flow rate of 0.2 mL/min, with an isocratic approach, on an Agilent Eclipse plus column (50 × 2.1 mm and 1.8 μm), in 1.6 min of running time. An Agilent triple quadrupole was used for mass analysis, to detect the ion transitions for GAB and PER, respectively, at m/z of 172.1 → 154.1 and 160.10 → 142.10. The calibration curve, over the linear range of 0.050–10.0 μg/mL, showed a high correlation coefficient, r = 0.9993. The limits of detection and quantitation were 13.37 ng/mL and 40.52 ng/mL, respectively, based on the standard deviation and slope equation. The results for intra- and inter-day measurement accuracy and precision were in acceptable ranges. The method was extended into the assessment of oral administrations of GAB at different doses, of one 600 mg/tablet and two capsules (each one of them has 300 mg of GAB), to volunteers who were used in pharmacokinetics and bioequivalent studies. The AGREE assessment tool was used to visualize the proposed method’s greenness degree, which revealed a high AGREE rating score, supporting the accepted method’s greenness profile