Optimization of modified dispersive liquid–liquid microextraction coupled with high‐performance liquid chromatography for the simultaneous preconcentration and determination of nitrazepam and midazolam drugs: An experimental design

A simple, sensitive, and rapid microextraction method, namely, ultrasound‐assisted surfactant‐enhanced emulsification microextraction based on the solidification of floating organic droplet method coupled with high‐performance liquid chromatography was developed for the simultaneous preconcentration and determination of nitrazepam and midazolam. The significant parameters affecting the extraction efficiency were considered using Plackett–Burman design as a screening method. To obtain the optimum conditions with consideration of the selected significant variables, a Box–Behnken design was used. The microextraction procedure was performed using 29.1 μL of 1‐undecanol, 1.36% (w/v) of NaCl, 10.0 μL of sodium dodecyl sulfate (25.0 μg mL^?1), and 1.0 μL of Tween80 (25.0 μg mL^?1) as an emulsifier in an extraction time of 20.0 min at pH 7.88. In order to investigate the validation of the developed method, some validation parameters including the linear dynamic range, repeatability, limit of detection, and recoveries were studied under the optimum conditions. The detection limits of the method were 0.017 and 0.086 ng mL^?1 for nitrazepam and midazolam, respectively. The extraction recovery percentages for the drugs studied were above 91.0 with acceptable relative standard deviation. The proposed methodology was successfully applied for the determination of these drugs in a number of human serum samples.     

Fractional stochastic Burgers‐type equation in Hölder space—Wellposedness and approximations

In this work, we use the spectral Galerkin method to prove the existence of a pathwise unique mild solution of a fractional stochastic partial differential equation of Burgers type in a Hölder space. We get the temporal regularity, and using a combination of Galerkin and exponential‐Euler methods, we obtain a full discretization scheme of the solution. Moreover, we calculate the rates of convergence for both approximations (Galerkin and full discretization) with respect to time and to space.     

Validated Simultaneous Gradient Ultra-Performance Liquid Chromatographic Quantification of Some Proton Pump Inhibitor Drug Residues in Saudi Pharmaceutical Industrial Wastewater

Monitoring and quantification of active pharmaceutical ingredients (APIs) in the environment constitute important and challenging tasks, as they are directly associated with human health. Three commonly used proton pump inhibitors (PPIs), namely, omeprazole sodium (OMP), pantoprazole sodium (PNT), and lansoprazole sodium (LNZ) are well separated and quantified using ultra-performance liquid chromatography (UPLC) in pharmaceutical industrial wastewater. The separation of the studied drugs was performed on a stationary phase with a Waters^TM column (100 × 2.1 mm, 1.7 µm). The mobile phase was composed of methanol:0.05 M potassium dihydrogen phosphate buffer (adjusted to pH 7.5 using NaOH) (50:50, v/v). The elution process was done in gradient mode by changing the relative proportions of the mobile phase components with time to get an optimum separation pattern. The flow rate of the developing system was adjusted to 0.8 mL/minute. Detection of the separated drugs was performed at 230 nm. The studied drugs were quantified in the concentration range of 10–200 ng/mL for all drugs. The cited method was fully validated according to the international conference on harmonization (ICH-Q2B) guidelines, then it was applied successfully for quantification of the studied PPIs in real wastewater samples after their solid phase extraction (SPE).     

New palladium(II)-catalyzed asymmetric 1,2-dibromo synthesis

[reaction: see text] The oxidation of olefins by chiral monometallic and bimetallic Pd(II)-Cu(II) catalysts in bromide-containing aqueous-THF reaction mixtures produced chiral 1,2-dibromides. With alpha-olefins, the ee's were about 95% while most of the internal alkenes gave somewhat lower enantioselectivities ( approximately 80%).     

Flow-injection spectrophotometric determination of periodate and iodate by their reaction with pyrogallol red in acidic media

A simple and efficient flow-injection method was used with good results to determine periodate and iodate in water. The method is based on the reaction of periodate or iodate with pyrogallol red in sulfuric acid media. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of pyrogallol red at 470 nm. The chemical and FIA variables were established using the univariate and simplex optimization methods. The calibration curve was linear over the concentration ranges of 0.8-73.0 and 2.0-100.0 microM for IO4- and IO3-, respectively. The detection limits were 0.7 and 1.0 microM for IO4- and IO3-, respectively. The sample throughput was 20 +/- 5 h(-1). The influence of potential interfering ions in the determination of the anions was tested. The relative standard deviations for 4.20 and 5.73 microM periodate and iodate were 1.8 and 2.2%, respectively.     

Synthesis and Characterization of Palladium(II) Complexes with 2‐(2′‐Pyridyl)quinoline. Catalytic Air Oxidation of Olefins by Palladium(II) Complexes

Palladium(II) complexes of 2‐(2′‐pyridyl)quinoline (PQ), namely [PdX₂(PQ)] (X = Br^?, I^?, N₃^?, NO₂^?, SCN^?, acac) and [PdCl(NO₃)(PQ)] have been synthesized via substitution reactions of [PdCl₂(PQ)] with an excess of sodium salts and acetylacetone. The complexes have been characterized by elemental analysis, conductivity measurements, IR, ¹H and ¹³C NMR spectroscopy. Selected complexes have been further characterized using electrospray ionization (ESI) and ion trap mass spectroscopy (ITMS). Some complexes are found to catalyze the rapid air oxidation of α‐olefins under Wacker oxidation. The chlorohydrin products are produced in good to excellent yields while oxidation products are obtained in low yields. The [PdCl₂(PQ)] complex is found to have the highest catalytic activity.     

Flow Injection Spectrophotometric Determination of Trace Amounts of Hydrazine by the Inhibition of the Pyrogallol Red-Iodate Reaction

A simple and sensitive flow injection method is described for the determination of trace amounts of hydrazine, based on its inhibitory effect on the reaction between pyrogallol red and iodate in hydrochloric acid media. The reaction was monitored spectrophotometrically by measuring the change in absorbance of pyrogallol red at 470 nm. The calibration graph was linear over the range of 0.050–1.20 g/mL, with a limit of detection of 0.03 g/mL. The relative standard deviation for ten replicate measurements of 0.060 and 0.70 g/mL was 2.2 and 0.50%, respectively. Potential interfering substances were studied in the presence of hydrazine. The proposed method was applied to the determination of hydrazine in water samples.