An interior needle electropolymerized pyrrole-based coating for headspace solid-phase dynamic extraction

A headspace solid-phase dynamic extraction (HS-SPDE) technique was developed by the use of polypyrrole (PPy) sorbent, electropolymerized inside the surface of a needle, as a possible alternative to solid-phase microextraction (SPME). Thermal desorption was subsequently, employed to transfer the extracted analytes into the injection port of a gas chromatography-mass spectrometry (GC-MS). The PPy sorbent including polypyrrole-dodecyl sulfate (PPy-DS) was deposited on the interior surface of a stainless steel needle from the corresponding aqueous electrolyte by applying a constant deposition potential. The homogeneity and the porous surface structure of the coating were examined using the scanning electron microscopy (SEM).The developed method was applied to the trace level extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample. In order to enhance the extraction efficiency and increase the partition coefficient of analytes, the stainless steel needle was cooled at 5 °C, while the sample solution was kept at 80 °C. Optimization of influential experimental conditions including the voltage of power supply, the time of PPy electrodeposition, the extraction temperature, the ionic strength and the extraction time were also investigated. The detection limits of the method under optimized conditions were in the range of 0.002-0.01 ng mL⁻¹. The relative standard deviations (R.S.D.) at a concentration level of 0.1 ng mL⁻¹ were obtained between 7.54 and 11.4% (n = 6). The calibration curves of PAHs showed linearity in the range of 0.01-10 ng mL⁻¹. The proposed method was successfully applied to the extraction of some selected PAHs from real-life water samples and the relative recoveries were higher than 90% for all the analytes.     

Electrochemical investigations of the various electrolytes for high energy density metal oxide supercapacitor

Journal of Solid State Electrochemistry - In this work, the asymmetric supercapacitor (ASC) devices with three different electrolytes including aqueous, organic, and gel polymer electrolytes have...     

Solubility of sildenafil citrate in propylene glycol + water mixtures at various temperatures

The solubility of sildenafil citrate (SC) in aqueous mixtures of propylene glycol (PG) was investigated. This study was carried out at different mass fractions of PG ranging from 0.1 to 0.9 at T = 293.2–313.2 K. The solubility of SC in the mixed solutions increased with increasing temperature and PG mass fraction.

The solubility values were correlated by two co-solvency models (Jouyban–Acree model and van’t Hoff–Jouyban–Acree model). The mean relative deviations (MRD) were 5.7% and 5.5%, respectively. Density of the SC-saturated solutions over the entire solvent composition and temperature range was also measured and the results correlated with the Jouyban–Acree model. Furthermore, the apparent thermodynamic properties, dissolution enthalpy, dissolution entropy and Gibbs free energy change of dissolution process of SC in all the mixed solvents were calculated according to van’t Hoff and Gibbs equations. Dissolution of SC in these mixed solvents is an endothermic process.     

A novel sol-gel-based amino-functionalized fiber for headspace solid-phase microextraction of phenol and chlorophenols from environmental samples

A novel amino-functionalized polymer was synthesized using 3-(trimethoxysilyl) propyl amine (TMSPA) as precursor and hydroxy-terminated polydimethylsiloxane (OH-PDMS) by sol–gel technology and coated on fused-silica fiber. The synthesis was designed in a way to impart polar moiety into the coating network. The scanning electron microscopy (SEM) images of this new coating showed the homogeneity and the porous surface structure of the film. The efficiency of new coating was investigated for headspace solid-phase microextraction (SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography–mass spectrometry (GC–MS) analysis. Effect of different parameters influencing the extraction efficiency such as extraction temperature, extraction time, ionic strength and pH was investigated and optimized. In order to improve the separation efficiency of phenolic compounds on chromatography column all the analytes were derivatized prior to extraction using acetic anhydride at alkaline condition. The detection limits of the method under optimized conditions were in the range of 0.02–0.05 ng mL⁻¹. The relative standard deviations (R.S.D.) (n = 6) at a concentration level of 0.5 ng mL⁻¹ were obtained between 6.8 and 10%. The calibration curves of chlorophenols showed linearity in the range of 0.5–200 ng mL⁻¹. The proposed method was successfully applied to the extraction from spiked tap water samples and relative recoveries were higher than 90% for all the analytes.     

Alteration in the Mechanical Properties of Human Ovum Zona Pellucida Following Fertilization: Experimental and Analytical Studies

The unfertilized oocyte is surrounded by a spherical layer called the zona pellucida (ZP). The physical hardness of this layer plays a crucial role in fertilization and it is largely unknown because of the lack of appropriate measuring and modeling methods. Recently, considerable biomedical attentions have concentrated on determination of the mechanical properties of oocytes as a single cell. In order to investigate the biophysical characteristics of mammalian oocytes, a change in the elasticity of human ZP has been quantitatively evaluated before and after fertilization. Young’s modulus of ZP of metaphase-II (MII) and pronuclear (PN) stages have been estimated using two different protocols of the micropipette aspiration, step-by-step and continuous increase in pressure, in combination with proportional theoretical models. Experimental results clearly demonstrated that after fertilization the mean Young’s modulus of the ZP calculated from the step-by-step aspiration test (MII: 7.34 ± 1.36 kPa vs PN: 13.18 ± 1.17 kPa.) and continuous aspiration test (MII: 2.41 ± 0.75 kPa vs. PN: 4.43 ± 1.66 kPa) significantly increased, (p < 0.05). Mathematical Evaluation of the results shows that although the results of the two methods are different but both confirm that the hardening of ZP will increase following fertilization. As can be seen, different experimental methods can influence the choice of the models and this in turn will lead the mechanical properties to be found.     

Synthesis of nanoporous TiO2 materials using a doubly surfactant system and applying them as useful adsorbents

Hydrothermal and non-hydrothermal nanoporous TiO₂ materials were synthesized via a doubly surfactant route by using cationic cetyltrimethylammonium bromide and anionic sodium dodecyl sulfate surfactants as the molecular template/structure directing agent. Hydrothermal treatment was performed for comparison. The bulk chemical and phase compositions, crystalline structures, particle morphologies, thermal stabilities and surface texturing were determined by means of X-ray powder analysis, SEM and N₂ sorptiometry. The nanoporous TiO₂ materials were found to have a spherical morphology with a diameter range of 50–200 nm and a high surface area (390 m² g^?1). Hydrothermal and non-hydrothermal nanoporous TiO₂ materials were applied for adsorption of heavy metal cations and the toxic organic compound, copper phthalocyanine, from water for evaluation of their adsorption properties. Both nanoporous TiO₂ materials were found to have similar adsorption capacities toward heavy metal cations and CuPc. Both hydrothermal and non-hydrothermal TiO₂ nanoporous materials were found to have very good potential for application as a new adsorbent especially for adsorbing heavy metal cations from wastewaters.     

Heat Transfer and Hydrodynamic Performance Analysis of a Miniature Tangential Heat Sink Using Al2O3–H2O and TiO2–H2O Nanofluids

In this article, thermal and hydrodynamic performances of a miniature tangential heat sink are investigated experimentally by using Al₂O₃–H₂O and TiO₂–H₂O nanofluids. The effects of flow rate and volume concentration on the thermal performance have been investigated for the Reynolds number range of 210 to 1,100. Experimental results show that the average convective heat transfer coefficient increases 14 and 11% and the bottom temperature of the heat sink decreases 2.2°C and 1.6°C by using Al₂O₃–H₂O and TiO₂–H₂O nanofluid instead of pure distilled water, respectively.     

Pyrrolizidine Alkaloids-Free Extract from the Cell Culture of Lithospermum officinale with High Antioxidant Capacity

The benefits of Lithospermum officinale has encouraged people to continue using its extract (CAS 90063-58-4) in both medicinal and cosmetic industries despite the fact that chemical analysis confirms the presence of pyrrolizidine alkaloids (PAs) in the extract. While the cultivation of L. officinale takes, at least, 2 years to produce usable crops, its callus culture proliferated 8.3 times with 4.9-fold biomass in less than 30 days under the applied conditions in this study. Under the applied conditions, the cell extract contained no toxic PAs while phenylpropanoid pathway was active toward phenolic acids formation not toward naphthoquinone derivatives. Rosmarinic acid was produced as the main constituent. Total phenolic content and antioxidant capacity of the proliferated cell extracts were similar to those of the extracts of the natural plant tissues, in particular from the root. These results support the idea that the extract of L. officinale cells can be a reliable substitute for the extract of the natural plant tissues.

     

A highly selective and sensitive cocaine aptasensor based on covalent attachment of the aptamer-functionalized AuNPs onto nanocomposite as the support platform

Based on the conformational changes of the aptamer-functionalized gold nanoparticles (AuNPs) onto MWCNTs/IL/Chit nanocomposite as the support platform, we have developed a sensitive and selective electrochemical aptasensor for the detection of cocaine. The 5′-amine-3′-AuNP terminated aptamer is covalently attached to a MWCNTs/IL/Chit nanocomposite. The interaction of cocaine with the aptamer functionalized AuNP caused the aptamer to be folded and the AuNPs with negative charge at the end of the aptamer came to the near of electrode surface therefore, the electron transfer between ferricyanide (K₃Fe(CN)₆) as redox probe and electrode surface was inhibited. A decreased current of (K₃Fe(CN)₆) was monitored by differential pulse voltammetry technique. In an optimized condition the calibration curve for cocaine concentration was linear up to 11 μM with detection limit (signal-to-noise ratio of 3) of 100 pM. To test the selectivity of the prepared aptasensor sensing platform applicability, some analgesic drugs as the interferes were examined. The potential of the aptasensor was successfully applied for measuring cocaine concentration in human blood serum. Based on our experiments it can be said that the present method is absolutely beneficial in developing other electrochemical aptasensor.