Glass/SU‐8 microchip for electrokinetic applications

In this communication, we describe the fabrication and electric characterization of a hybrid glass/SU‐8 microchannels for high‐performance electrokinetic applications. The bonding process employed SU‐8 film as intermediate layer with reduced baking times; all the procedure took less than 50 min (only about 10 min disregarding the cleaning and dehydration steps). Additionally, further steps to improve the adhesion of the substrate to the SU‐8 were not needed. The developed configuration aggregates the advantages of both substrates, including (i) simple fabrication techniques; (ii) high compatibility for integration of microelectromechanical, optical, and electrochemical components (SU‐8); (iii) high and stable electroosmotic mobility (μ_EO); and (iv) satisfactory heat dissipation capacity (glass). Electroosmotic mobilities were measured as a function of the pH using the current monitoring method, whereas the heat dissipation capacity was investigated through Ohm's law plots for both glass and glass/SU‐8 microchips. The measured μ_EO values were similar for both microdevices, with mobilities of the order of 4.0–4.5 × 10^?4 cm² V^?1 cm^?1 at 4–12 pH range using phosphate buffer (10 and 20 mmol/L). The heat dissipation assays were carried out in microchannels filled with 20 mmol/L phosphate buffer. A considerable Joule heating was observed only at electric field strengths greater than 580 V cm^?1 in hybrid glass/SU‐8 microdevices, representing a substantial increase of 48% when compared to all SU‐8 microdevices.     

Ruthenium Carbenes Supported on Mesoporous Silicas as Highly Active and Selective Hybrid Catalysts for Olefin Metathesis Reactions under Continuous Flow

In the search for a highly active and selective heterogenized metathesis catalyst, we systematically varied the pore geometry and size of various silica‐based mesoporous (i.e., MCM‐41, MCM‐48, and SBA‐15) and microporous (ZSM‐5 and MWW) versus macroporous materials (D11‐10 and Aerosil 200), besides other process parameters (temperature, dilution, and mean residence time). The activity and, especially, selectivity of such “linker‐free” supports for ruthenium metathesis catalysts were evaluated in the cyclodimerization of cis‐cyclooctene to form 1,9‐cyclohexadecadiene, a valuable intermediate in the flavor and fragrance industry. The optimized material showed not only exceptionally high selectivity to the valuable product, but also turned out to be a truly heterogeneous catalyst with superior activity relative to the unsupported homogeneous complex.     

Simultaneous Square‐Wave Voltammetric Determination of Paracetamol,Caffeine and Orphenadrine in Pharmaceutical Formulations Using a Cathodically Pretreated Boron‐Doped Diamond Electrode

An electroanalytical method for the simultaneous determination of paracetamol (PAR), caffeine (CAF), and orphenadrine (ORPH) using the square‐wave voltammetry (SWV) and a cathodically pretreated boron‐doped diamond electrode was developed. The method exhibits linear responses to PAR, CAF, and ORPH in the concentration ranges 5.4×10^?7–6.1×10^?5 M, 7.8×10^?7–3.5×10^?5 M, and 7.8×10^?7–3.5×10^?5 M, respectively, with detection limits of 2.3×10^?7 M, 9.6×10^?8 M, and 8.4×10^?8 M, respectively. The proposed method was successfully applied in the simultaneous determination of these analytes in pharmaceutical formulations.     

Development and Validation of a RP-HPLC–PDA Method for Determination of Curcuminoids in Microemulsions

A sensitive, specific and rapid high-performance liquid chromatography method was developed in an effort to quantify extremely low curcuminoid levels for the future transdermal experiments where the curcuminoids are incorporated with excipients such as microemulsion, liposomes, and micelles. The chromatographic separation was performed using a Symmetry^® C₁₈, 250 × 4.6 mm, 5-μm column, with a mobile phase composed of 5 mM acetonitrile:phosphoric acid (45:55, v/v) at a flow rate of 1.0 mL min^?1, it was sensitive with a low limit of quantitation for curcuminoids (0.626 ng mL^?1 for curcumin) and good linearity (r ² ≥ 0.999) over the range 1–100 ng mL^?1. All the validation data, such as accuracy and precision, were within the required limits from the ICH guideline. The assay method was successfully applied during forced degradation of curcuminoid solutions. The method retained its accuracy and precision when the standard addition technique was applied.     

Direct synthesis of 2-aryl-1,3-benzoselenazoles by reaction of bis(2-aminophenyl) diselenides with aryl aldehydes using sodium metabisulfite

We present here a general and easy method for the synthesis of several 2-aryl-1,3-benzoselenazoles from the reaction of bis(2-aminophenyl) diselenides with different aryl aldehydes, promoted by the non-toxic inorganic reducing agent sodium metabisulfite (Na₂S₂O₅) in DMSO at 120 °C. This efficient method furnishes in high yields the corresponding 2-aryl substituted 1,3-benzoselenazoles and tolerates a range of substituents at the aryl ring of aldehydes. The use of focused microwave irradiation decreases drastically the reaction time from 48 to 2 h.     

Development and Validation of a RP-HPLC–PDA Method for Determination of Curcuminoids in Microemulsions

A sensitive, specific and rapid high-performance liquid chromatography method was developed in an effort to quantify extremely low curcuminoid levels for the future transdermal experiments where the curcuminoids are incorporated with excipients such as microemulsion, liposomes, and micelles. The chromatographic separation was performed using a Symmetry^® C₁₈, 250 × 4.6 mm, 5-μm column, with a mobile phase composed of 5 mM acetonitrile:phosphoric acid (45:55, v/v) at a flow rate of 1.0 mL min⁻¹, it was sensitive with a low limit of quantitation for curcuminoids (0.626 ng mL⁻¹ for curcumin) and good linearity (r ² ≥ 0.999) over the range 1–100 ng mL⁻¹. All the validation data, such as accuracy and precision, were within the required limits from the ICH guideline. The assay method was successfully applied during forced degradation of curcuminoid solutions. The method retained its accuracy and precision when the standard addition technique was applied.

     

Pulsed amperometric detection (PAD) of diuretic drugs in herbal formulations using a gold electrode following ion-pair chromatographic separation

Herein, we present a new method based on separation by ion-pair chromatography with pulsed amperometric detection for evaluating various diuretics, including hydrochlorothiazide, chlorthalidone, furosemide, and amiloride, which are adulterants in herbal-based pharmaceutical formulations. The amperometric detection cycle (time?=?2 s) was performed at a gold electrode by applying a detection potential (E1) of +800 mV for 0.4 s and an oxidation potential (E2) of +1,000 mV for 0.40 s, followed by a reduction potential (E3) of ?200 mV for 1.20 s. The mobile phase for separating the diuretics was composed of 5 mmol L^?1 phosphate buffer and 0.3 mmol L^?1 sodium dodecyl sulfate in 50 % (v/v) methanol (pH 4.5). This method enabled the quantification of the drugs at low concentrations (i.e., 0.08 mg/capsule for hydrochlorothiazide, 0.01 mg/capsule for chlorthalidone, and 0.007 mg/capsule for furosemide). Twenty-six herbal formulations were analyzed, and eight samples (30.8 %) were found to contain diuretics that were added to the final composition (declared or not).     

Liquid-liquid equilibrium of aqueous two-phase systems composed of poly(ethylene oxide) 1500 and different electrolytes ((NH4)2SO4, ZnSO4 and K2HPO4): Experimental and correlation

Phase diagrams of aqueous two-phase systems composed of PEO1500 + salt (di-potassium phosphate + potassium hydroxide or ammonium sulfate or zinc sulfate) + water were determined at (283.15, 298.15, and 313.15) K. All systems produce a large two-phase region; however the influence of temperature on the binodal position seems to be very small. By analyzing the effects of ammonium sulfate or zinc sulfate, it was observed that zinc was more effective in promoting phase separation than ammonium. The consistency of the tie-line data was ascertained by applying the Othmer-Tobias correlation. In this paper, aqueous two-phase systems data for nine ternary systems are correlated by using the NRTL model and UNIFAC for the activity coefficient. The results are very satisfactory, with root mean square deviations between experimental and calculated compositions as low as 0.99 and 1.21%, respectively. However the NRTL model better represents the systems in study, when compared with UNIFAC.