Synthesis of 1H-thieno[3,4-c]pyrazoles,thieno[3,4-b]furans,selenolo[3,4-b]furans and pyrrolo[3,4-d]thiazoles

Starting from the readily available aryl 2-methyl-5-phenyl-3-furyl ketones, 5-methyl-1H-1-phenylpyrazole-4-yl ketones and 4-methyl-2-phenyl-5-thiazolylcarboxaldehyde, a series of 2-phenyl-4-arylthieno[3,4-b]-furan, 2-phenyl-4-(p-methoxyphenyl)selenolo[3,4-b]furan, 4-aryl-1H-1-phenylthieno[3,4-c]pyrazole and 5-benzyl-2-phenylpyrrolo[3,4-d]thiazole were prepared in high yield.     

A high selective ion‐imprinted polymer grafted on a novel nanoporous material for efficient gold extraction

In this work, for the first time, an ion‐imprinted polymer was developed for selective extraction and determination of gold ions. To increase the sorbent efficiency, this polymer was coated on a novel nanoporous carbon‐based material, carbohydrate‐derived Max‐Planck Gesellschaft 1, which is also the first example of grafting imprinted polymer on nanoporous‐carbon material. These particles were applied successfully for preconcentration of ultratrace amount of gold ions, following determination by flame atomic absorption spectrometry. Some effective factors on the efficiency of gold ions extraction, such as concentration and volume of eluent, sample and eluent flow rates, and also effect of interfering ions especially palladium and platinum ions, were investigated. The LOD was determined to be 0.27 ng/mL. Furthermore, the precision of the method was calculated to be 2.14% under optimal conditions with recovery more than 97.3%. The technique was also used to determine the concentration of gold ions in mine stone samples with satisfactory results. The accuracy of this method was investigated by determination of gold ions concentrations in several reference materials with certified gold content.     

Determination of Methadone in Biological Samples Using Liquid Phase Microextraction with Back Extraction Combined with LC

Liquid phase microextraction with back extraction (LPME-BE) combined with liquid chromatography-ultra violet (LC-UV) was applied for the extraction and determination of methadone in biological fluids. At the optimized conditions, an enrichment factor of 386 and detection limit (LOD) of 0.2 μg L^?1 were obtained. The calibration curve was linear (r ² = 0.989) in the concentration range of 0.6–1,000 μg L^?1. Within-day relative standard deviation RSD (S/N = 3) and between-day RSD were 2.7 and 5.9%, respectively. The feasibility of the proposed method was evaluated by extraction and determination of methadone in plasma and urine samples and satisfactory results were obtained.     

Topologies on abelian lattice ordered groups induced by a positive filter and completeness

We consider topologies on an abelian lattice ordered group that are determined by the absolute value and a positive filter. We show that the topological completions of these objects are also determined by the absolute value and a positive filter. We investigate the connection between the topological completion of such objects and the Dedekind–MacNeille completion of the underlying lattice ordered group. We consider the preservation of completeness for such topologies with respect to homomorphisms of lattice ordered groups. Finally, we show that topologies defined in terms of absolute value and a positive filter on the space C(X) of all real-valued continuous functions defined on a completely regular topological space X are always complete.     

Near- to mid-infrared picosecond optical parametric oscillator based on periodically poled RbTiOAsO(4)

We describe a Ti:sapphire-pumped picosecond optical parametric oscillator based on periodically poled RbTiOAsO(4) that is broadly tunable in the near to mid infrared. A 4.5-mm single-grating crystal at room temperature in combination with pump wavelength tuning provided access to a continuous-tuning range from 3.35 to 5microm , and a pump power threshold of 90 mW was measured. Average mid-infrared output powers in excess of 100 mW and total output powers of 400 mW in ~1-ps pulses were obtained at 33% extraction efficiency.     

Direct conversion of trimethylsilyl and tetrahydropyranyl ethers into their bromides and iodides under neutral conditions using N-bromo and N-iodosaccharins in the presence of triphenylphosphine

Trimethylsilyl and tetrahydropyranyl ethers were easily converted into their corresponding bromides and iodides with high efficiency and selectivity by N-bromo- and N-iodosaccharins in the presence of triphenylphosphine under neutral conditions. The reaction of trimethyloctyloxysilane as a model compound was studied in different solvents with different ratios of silyl ethers, triphenylphosphine and N-halosaccharin at room temperature, in order to optimize the reaction conditions.     

Efficient second-harmonic generation in birefringently phase-matched GaAs/Al(2)O(3) waveguides

We report efficient second-harmonic generation of femtosecond pulses in birefringently phase-matched GaAs/Al(2)O(3) waveguides pumped at 2.01mum. By use of pump pulses of ~200-fs duration and type I interaction, practical second-harmonic average powers of up to ~650muW were obtained, with an average input power of ~50muW. Waveguides of four different widths and two different lengths were investigated, and a normalized conversion efficiency of greater than 1000%W(-1)cm(-2) was obtained for a 1-mm waveguide. Measurements of pump and second-harmonic spectra provided clear evidence of phase matching and depletion of the pump spectrum. The measured bandwidth of the second harmonic was ~1.3nm. From the measurements of transmitted pump power at the phase-matching wavelength, pump depletions of more than 80% were recorded.     

Analysis of mono-nitrotoluenes in water samples by using nano-structured polypyrrol as a sorbent of solid-phase microextraction

Nano-structured polypyrrole (PPY) was used as a coating of solid-phase microextraction (SPME) fibre to increase the extraction efficiency of headspace solid phase microextraction (HS-SPME) of mono-nitrotoluene (MNT) isomers in water samples. The nano-structured PPY was prepared electrochemically by template-free method in the presence of dodecylbenzene sulphonate (DBS) as dopant. Nano-fibrous structures of PPY with a diameter in the range of 38–129 nm were obtained. The porous surface structure of the film, revealed by scanning electron microscopy (SEM), provided high surface areas and allowed for high extraction efficiency of MNT isomers. The extraction procedure was optimised by selecting the appropriate extraction parameters including the time and temperature of adsorption, salt concentration and stirring rate. The calibration graphs obtained by HS-SPME using the proposed fibre followed by GC-FID analysis were linear in a concentration range of 0.1–500 µg L^?1 (r > 0.999) with detection limits below 0.012 µg L^?1 for three isomers. Repeatability of the method was less than 6% (RSD%, n = 4). Good recoveries (88–108%) were obtained for the extraction of mono-nitrotoluenes in real water samples.     

Dispersive micro-solid-phase extraction of benzodiazepines from biological fluids based on polyaniline/magnetic nanoparticles composite

In this study, diverse types of Fe₃O₄ nanocomposites modified by polyaniline, polypyrrole, and aniline–pyrrole copolymer were synthesized through chemical oxidative polymerization process for dispersive-μ-solid phase extraction (D-μ-SPE) in the presence of various dopants. The results showed that the nanocomposite modified by polyaniline with p-toluene sulfonic acid as a dopant demonstrated higher extraction efficiency for lorazepam (LRZ) and nitrazepam (NRZ). Also the synthesized magnetic sorbents were characterized. The nanocomposite sorbent in combination with high performance liquid chromatography–UV detection was applied for the extraction, preconcentration and determination of lorazepam and nitrazepam in urine and plasma samples. Different parameters influencing the extraction efficiency including: sample pH, amount of sorbent, sorption time, elution solvent and its volume, salt content, and elution time were optimized. The obtained optimal conditions were: sample pH, 6; amount of sorbent, 5 mg; sorption time, 5.0 min; elution solvent and its volume, 0.5 mM cethyltrimethyl ammonium bromide in acetonitrile, 150 μL; elution time, 2.0 min and without addition of NaCl. The calibration curves were linear in the concentration range of 1–2000 μg L⁻¹. The limits of detection (LODs) were achieved in the range of 0.5–1.8 μg L⁻¹ for NRZ and 0.2–2.0 μg L⁻¹ for LRZ, respectively. The percent of extraction recoveries and relative standard deviations (n = 5) were in the range of 84.0–99.0, 6.1–7.8 for NRZ and 90.0–99.0, 4.1–7.0 for LRZ, respectively. Ultimately, the applicability of the method was successfully confirmed by the extraction and determination of NRZ and LRZ in human urine and plasma samples.