Terrace formation with a picoliter sol–gel droplet for spherical cavity Raman laser

We have successfully made terrace-microspheres for laser emission: micrometer-size spherical cavity laser having terrace-shaped pumping-light entrance. Organic–inorganic hybrid materials in the binary system of 3-methacryloxypropyltrimethoxysilane (MOPS) and tetramethoxysilane (TMOS) were used for preparing the terrace on glass microspheres by sol–gel technique. To make terrace portion, a picoliter sol was supplied with a micro-capillary suppliers into the bottom of spheres and subsequently the terrace-shaped sol was solidified. In the MOPS-TMOS binary system, essential sol properties such as viscosity change and sol–gel transformation rate determine the terrace structures. Compositions and volumes of the sol remarkably influenced viscosity increase and subsequent solidification. In this study, we showed that the control of the terrace structure for spherical cavity Raman lasers was possible by choosing the suitable compositions of picoliter-volume sol droplets. Terrace-microspheres from high-refractive-index glass spheres (n _D  = 1.93) was pumped with a CW Ar⁺ laser (514.5 nm wavelength), and stimulated Raman emission was demonstrated above the threshold of 2.5 mW.     

Analysis of particle size distribution in colloidal dispersions by electron microscopy

Summary Particle size distribution data have been determined by electron microscopy for dispersions containing known mixtures of monodisperse polystyrene latices of diameters in the range 0.08–0.4μ, and particle concentrations of 10⁶–10⁸ particles ml⁻¹, and good agreement was found for grid specimens prepared by centrifugation.     

Fractionation of nano- and microparticles in a rotating conoidal coiled column

A method for the continuous-flow fractionation of particles in a transverse centrifugal field in a rotating conoidal coiled (RCC) column has been developed. A model of a planetary centrifuge with a conoidal drum of a special construction has been tested. The effects of the rotation and revolution speed of the conoidal RCC, as well as the direction and pumping rate of the mobile phase on the behavior of particles smaller than 1 μm have been studied. The conditions have been selected and optimized for the retention and elution of spherical particles of the ‘150 nm’, ‘400 nm’, and ‘900 nm’ standard samples of silica gel (Polyscience Inc.). The possibility of using RCC for the analysis and production of monodisperse standard particle samples has been demonstrated. In particular, the ‘900 nm’ particles have been separated from admixtures of small (100–200 nm) particles and nonspherical 1–2 μm particles present in the sample. The separated fractions have been characterized by electron microscopy.     

Nanosized zirconium diboride: Synthesis and properties

The thermolysis of Zr(BH₄)₄ vapor at 573 and 623 K in a vacuum of 1.33 × 10⁻¹ Pa was studied. Nanosized zirconium diboride was produced as an X-ray amorphous powder and a crystalline film. According to electron microscopy data, the X-ray amorphous zirconium diboride powder obtained at 573 or 623 K consists of spherical particles 30–40 nm in diameter, which is in quite a good agreement with the equivalent particle diameter (∼35 nm) calculated from the specific surface area of ZrB₂. After annealing at 1273 K, the X-ray amorphous zirconium diboride powder crystallizes into a hexagonal lattice with the unit cell parameters a = 0.3159 nm and c = 0.3527 nm. The coherent scattering length D _hkl is ∼27 nm. The zirconium diboride film produced at 573 or 623 K crystallizes into a hexagonal lattice with the unit cell parameters a = 0.3163−0.3168 nm and c = 0.3524−0.3531 nm. The coherent scattering length D _hkl is ∼14 nm. The thickness of the ZrB₂ film on quartz, glass ceramics, and stainless steel is 5–7 μm. The microhardness of the film on a stainless steel substrate under a load of 20 g is 17.8 GPa.     

Orientation of water molecules by the diamond surface

The properties of water in suspensions of diamond powders with particle sizes from 125–160 μm to 2–10 nm were studied. The dielectric constant of water in these suspensions changed from 1.3 × 10³ to 2.6 × 10⁶. The particle sizes correlated with the dielectric constants. The sound velocity of “diamond” water exceeded the initial velocity by 15–20 m/s. The crystals isolated from “diamond” water after prolonged storage had specific diffraction patterns and IR spectra. Their composition was not determined.     

Simultaneous RP-LC Determination of Losartan Potassium, Ramipril, and Hydrochlorothiazide in Pharmaceutical Preparations

A simple, rapid, and precise reversed-phase high-performance liquid chromatographic method has been developed for simultaneous determination of losartan potassium, ramipril, and hydrochlorothiazide. The three drugs were separated on a 150 mm × 4.6 mm i.d., 5 μm particle, Cosmosil C₁₈ column. The mobile phase was 0.025 m sodium perchlorate–acetonitrile, 62:38 (v/v), containing 0.1% heptanesulphonic acid, pH adjusted to 2.85 with orthophosphoric acid, at a flow rate of 1.0 mL min⁻¹. UV detection was performed at 215 nm. The method was validated for linearity, accuracy, precision, and limit of quantitation. Linearity, accuracy, and precision were acceptable in the ranges 35–65 μg mL⁻¹ for losartan, 1.75–3.25 μg mL⁻¹ for ramipril, and 8.75–16.25 μg mL⁻¹ for hydrochlorothiazide.     

Isocratic Reversed-Phase HPLC for Simultaneous Separation and Determination of Seven Antiepileptic Drugs and Two of their Active Metabolites in Human Plasma

A simple reversed-phase high-performance liquid chromatographic (HPLC) method has been developed for the simultaneous determination of the antiepileptic drugs (AEDs) zonisamide (ZNS), primidone (PRI), lamotrigine (LTG), phenobarbital (PB), phenytoin (PHT), oxcarbazepine (OXC), and carbamazepine (CBZ) and two of their active metabolites, monohydroxycarbamazepine (MHD) and carbamazepine 10,11-epoxide (CBZE) in human plasma. Plasma (100 μL) was pretreated by deproteinization with 300 μL methanol containing 20 μg mL⁻¹ propranolol hydrochloride as internal standard. HPLC was performed on a C₈ column (4.6 mm × 250 mm; particle size 5 μm) with methanol–acetonitrile–0.1% trifluoroacetic acid, 235:120:645 (v/v), as mobile phase at a flow rate of 1.5 mL min⁻¹. ZNS, OXC, and CBZ were monitored by UV detection at 235 nm, and PRI, LTG, MHD, PB, PHT, and CBZE by UV detection at 215 nm. Relationships between response and concentration were linear over the concentration ranges 1–80 μg mL⁻¹ for ZNS, 5–50 μg mL⁻¹ for PRI, 1–25 μg mL⁻¹ for LTG, 1–50 μg mL⁻¹ for MHD, 5–100 μg mL⁻¹ for PB, 1–10 μg mL⁻¹ for CBZE, 0.5–25 μg mL⁻¹ for OXC, 1–50 μg mL⁻¹ for PHT, and 1–25 μg mL⁻¹ for CBZ. Intra-day and inter-day reproducibility were adequate (coefficients of variation were ≤11.6%) and absolute recovery ranged from 95.2 ± 6.13 to 107.7 ± 7.76% for all the analytes; for the IS recovery was 98.69 ± 1.12%. The method was proved to be accurate, reproducible, convenient, and suitable for therapeutic monitoring of the nine analytes.     

Determination of Pyrethroid Insecticide Deltamethrin by Micellar Liquid Chromatography with Spectrophotometric Detection

A simple micellar liquid chromatographic technique for deltamethrin determination was developed and validated. The method provided to be suitable for deltamethrin determination in pediculicide shampoo. Kromasil C18 column (150 mm×4.6 mm, 5 μm) and mobile phase −0.12 M sodium dodecyl sulfate with 9% (v/v) 1-butanol were used for deltamethrin separation. Detection wavelength was 265 nm. The retention time was about 15 min. Different validation parameters were evaluated. The specificity of the method was demonstrated. Linearity was established in the range 10–40 μg L⁻¹. The limits of detection and quantitation were 1.06 and 3.22 μg mL⁻¹, respectively. The method showed excellent accuracy (100.6%) and precision (repeatability) gave a relative standard deviation of less than 1%. The influence of the various method parameters (robustness study) was also studied.     

Simultaneous HPLC Analysis of Olmesartan and Hydrochlorothiazide in Combined Tablets and in vitro Dissolution Studies

A simple, rapid and reproducible HPLC method was developed and validated for the simultaneous determination of olmesartan (OLM) medoxomil and hydrochlorothiazide (HCT) in combined tablets. Chromatography was carried out on a 4.6 mm I.D × 200 mm, 5 μm cyano column with methanol–10 mM phosphoric acid containing 0.1% triethylamine (pH 2.5, 50:50 v/v) at a flow rate of 1.0 mL min⁻¹ and UV detector was set at 260 nm. Valsartan (VAL) was used as internal standard (IS). A linear response was observed in the range of 0.2–6 μg mL⁻¹ (r ² = 0.9998) for OLM and 0.1–4 μg mL⁻¹ (r ² = 0.9999) for HCT, respectively. The method showed good recoveries (99.56% for OLM and 99.48% for HCT) and the relative standard deviation (RSD) values for intra- and inter-day precision were 0.70–1.59 and 0.80–2.00% for OLM and 1.20–1.37 and 1.63–1.93% for HCT, respectively. The developed method was applied successfully for quality control assay of OLM and HCT in combined tablets and in vitro dissolution studies.     

Simultaneous determination of azelaic and benzoic acids in topical preparations by liquid chromatography

Summary An isocratic, reversed-phase liquid chromatographic (LC) method has been developed for the simultaneous determination of azelaic and benzoic acids in pharmaceutical creams. The compounds were separated on a C₁₈ column (4 μm particles); the mobile phase was methanolwater, 40∶60, containing 10mm ammonium acetate and with the pH adjusted to 5.0. Detection was performed at 220 nm. The method was validated for accuracy, linearity, precision, and selectivity. Recoveries at levels corresponding to 80% to 120% of the declared content of the creams ranged from 99.5 to 101.8% and from 100.4 to 102.1% for azelaic and benzoic acids, respectively. The calibration graphs were linear in the ranges 20–1400 μg mL⁻¹ for azelaic acid (correlation coefficient,r ₁>0.99999), and 0.1–7.0 μg mL⁻¹ for benzoic acid (r>0.99998).     

Absorption spectra of large colloidal silver particles in aqueous solution

Calculations of the optical absorption spectra of spherical particles of silver with a radius (r) of 10 to 80 nm in water were performed. The single intense absorption band for small particles (r=10 nm) with a maximum at about 395 nm is gradually broadened and shifted to the long-wave region with an increase in the particle size (to 435 nm atr=40 nm). In the case of large particles, the band splits into several components absorbing light in the visible spectral region. The results are in good agreement with the optical characteristics of colloidal solutions of silver obtained upon radiochemical reduction of Ag⁺ ions in aqueous solution. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 201–203, January, 1997.     

Gas chromatography on 10 um silica particles

Summary Porous silica microparticles designed for modern liquid chromatography have proven effective in gas chromatography. Columns of 35–50 cm gave plate heights as low as 3.3 particle diameters and speeds of 2400 theoretical plates per second or 500 effective theoretical plates per second. Inlet pressures up to 70 atmospheres were required using hydrogen as carrier gas. The particles as received were too retentive for fast chromatography and gave asymmetric peaks. A coating of fluorosilicone oil overcame both problems. Other coatings were less effective. Bonded phases proved less satisfactory on both counts and also gave substantially less efficient columns and greater flow resistance. Column efficiency and flow resistance were sharply dependent on physical properties of the particles. The most efficient packing was clearly spherical particles of 5–10 μm diameter with narrow size distribution, pore diamters about 50 nm, BET surface areas of 25–50 m²/g and surfaces modified with trifluoropropyl silicone. A six-component hydrocarbon sample was separated in 33 s with a resolution of 4 for the most difficult pair and in 2.6 s with a minimal resolution. Performance was limited by end effects and by available pressure so that much better performance can be expected from longer columns and higher pressures.     

Glucosamine-functionalized silver glyconanoparticles: characterization and antibacterial activity

We report the analytical and in vitro antibacterial activity of glucosamine-functionalized silver glyconanoparticles. Morphological characterization ensured the surface topography and particle size distribution of both silver and glucosamine–silver nanoparticles. Surface plasmon resonance of both types of nanoparticle was determined from UV–visible spectroscopy using four different sample concentrations (10–40 μL). The resulting functionalized glyconanoparticles show maximum absorbance with a red shift of 30 ± 5 nm (390–400 nm) from their initial absorbance (425–430 nm). FT-Raman and ¹H-NMR spectroscopic measurement confirmed the surface functionalization of glucosamine on the silver surface through the carbonyl group of a secondary amide linkage (–NH–CO–), elucidated by the conjugation of N-hydroxysuccinimide (NHS)-terminated silver nanoparticles and the amino group of glucosamine. Antimicrobial experiments with well-characterized silver nanoparticles (AgNPs) and glucosamine-functionalized silver nanoparticles (GlcN-AgNPs) demonstrate that GlcN-AgNPs have similar and enhanced minimum inhibitory concentration (MIC) against eight gram-negative and eight gram-positive bacteria compared with AgNPs. MIC data shows that Klebsiella pneumoniae (ATCC 700603) and Bacillus cereus isolate express high levels of inhibition, with the quantity and magnitude of inhibition being higher in the presence of GlcN-AgNPs.     

X-ray study of the thermolysis products of (NH4)2[OsCl6]x[PtCl6]1?x

Thermolysis of the complex salts (NH₄)₂[OsCl₆] _x [PtCl₆]_1−x (x = 0.25−0.9) formed nanocrystalline Os _x Pt_1−x phases. Pseudomorphism has been found: the habit of the single crystals of the starting salts is preserved during thermolysis, and the ∼10–20 nm metal particles are agglomerated into octahedral structures sized 5–10 μm.     

Determination of triadimenol based on the quenching effect on resonance light scattering from the triadimenol–deoxyribonucleic acid–hydrochloric acid system

Analysis of triadimenol was carried out using deoxyribonucleic acids (DNA) via the resonance light scattering (RLS) technique. After adding triadimenol into aqueous medium of pH 1.72, the RLS of DNA was remarkably quenched. A resonance light scattering peak at 310 nm was found, and the quenched intensity of RLS at this wavelength was proportional to the concentration of triadimenol. The linear range of the calibration curve was approximately 0–3 μg mL⁻¹ with a detection limit (S/N = 3) of 0.07 μg mL⁻¹. The triadimenol in samples of water, cucumber and human serum was determined. The results were satisfactory, and the recovery rates were in the range of 96.3–106.0%, 94.8–105.9% and 92.3–100.5%, respectively. The interaction mechanism was also studied.     

Microwave synthesis and characterization of europium complexes with cinnamic acid and phenanthroline

We report here the synthesis and characterization of a host of Eu(Phen)L₃ with cinnamic acid (C₆H₅CH = CHCOOH, HL) and phenanthroline (Phen), and employing microwave radiation, where the microwave radiation is used just for the uniform heating of the reaction mixture. Its IR absorption spectra, scanning electron microscopy (SEM), and fluorescence spectra were studied. The results show that the particles of Eu(Phen)L₃ phosphors are basically spherical in shape, with good dispersing. The mean particle size is 1–2 μm. The excitation spectrum is a broad band and the main peak is at 320.0 nm. Moreover, excitation peak at 396.0 nm was found in the excitation spectrum. The emission spectrum shows that Eu(Phen)L₃ has narrow emission peaks. The emission peaks are ascribed to Eu³⁺ ions transition from ⁵ D _J (J = 0) to ⁷ F _J (J = 1, 2, 4). However, the strongest main emission peak locates at 614.0 nm, which corresponds to the electric dipole transition of Eu³⁺(⁵ D ₀ → ⁷ F ₂) The article is published in the original.     

Recombination rate constant of free electrons and holes in thin CdSe films

The decay kinetics of electrons generated in thin CdSe films by laser pulse (wavelength 337 nm, pulse duration 8 ns) at 295 K was studied by the microwave photoconductivity method (36 GHz). Based on analysis of the photoresponse decay kinetics and the reactions of free and trapped electrons, holes, and ions, a model for the processes was proposed and the recombination rate constant of free electrons and holes in cadmium selenide was determined, being (4–6)· 10–11 cm³ s⁻¹. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 740–743, May, 2006. The samples were kindly presented by Yu. V. Meteleva.     

Synthesis of Nanocrystalline TiO<Subscript>2</Subscript> Particles and Their Structural Characteristics

Controlled nanosized TiO₂ particles of 4–10 nm were synthesized by a simple hydrolysis method followed by calcination at different temperatures. These particles were investigated using X-ray diffraction (XRD), Photoacoustic/Fourier transform infrared (PA/FTIR) spectroscopy, Raman spectroscopy and electron spin resonance (ESR) spectroscopy to understand their structural properties. X-ray diffraction studies confirmed the anatase phase of the particles where as the PA/FTIR revealed the bands around 1,500 and 3,300 cm⁻¹ due to –OH bands. ESR spectroscopic investigations carried out from 5 to 300 K indicated the presence of an ESR line at g = 2.00 emerging from radical species. It is significant to note that the intensity of the ESR line decreased as the particle size increased.     

Visual microscopic studies on hetero-aggregation and selective aggregation

 An optical video microscopic technique was used to study hetero-aggregation and selective aggregation phenomena among n-hexadecane oil drops (40–110 μm in diameter) and two types of polystyrene latex particles (6.76 and 30.2 μm, in diameter), suspended inside an aqueous medium with pH varying between 1.1 and 12.9. A single drop was produced in situ using a micropipette inside the aqueous phase-filled glass microcapillary (100–160 μm i.d.) containing the particles. Interactions between the drop and the solid particles and among the solid particles was achieved by movement of the aqueous medium in and out of a second micropipette. Drop–particle interactions were distinctly different from particle–particle interactions. It was observed that the latex particles aggregated irreversibly with the oil drop in all cases except two, viz. for 6.76 μm particles at around neutral pH whereas the irreversibility of aggregation in particle–particle interactions was only seen at the ends of the pH spectrum. At around neutral pH, the flocs or clusters of small particles were very weak. Visual observations at each pH are explained on the basis of the classical DLVO (Derjaguin–Landau–Verwey–Overbeek) theory. Partial wetting of particles surfaces by oil appears to be a key factor in the irreversibility of drop– particle hetero-aggregation. Results indicate that the display of reversible, irreversible or weak aggregation depends on the location and depth of the secondary minimum and that the long-range, attractive, London–van der Waals force is responsible for the initial formation of an aggregate. Received: 4 July 1996 Accepted: 5 December 1996     

HPLC assay method for ceftibuten in plasma and its application to pharmacokinetic study

The purpose of this study was to validate a reliable analytical method for pharmacokinetic study of ceftibuten in human plasma by high performance liquid chromatography (HPLC) system with UV detection. Ceftizoxime was used as the internal standard. After plasma sample was precipitated with acetonitrile and dichloromethane, the supernatant was directly injected into the HPLC system. Separation was performed on a Capcell Pak C₁₈ UG120 column (4.6 mm × 250 mm, 5 μm particles) with a mobile phase of acetonitrile/50 mM ammonium acetate (5: 95, v/v) and UV detection at a wavelength of 262 nm. The intra- and inter-day precision expressed as the relative standard deviation was less than 15%. The lower limit of quantification was 0.5 hg/mL of ceftibuten using 0.5 mL of plasma. The calibration curve was linear in concentration range of 0.5–30 μg/mL (r ² = 0.9998). The mean accuracy was 96–102%. The coefficient of variation (precision) in the intra- and inter-day validation was 0.9–3.9 and 0.9–2.4%, respectively. The pharmacokinetics of ceftibuten was evaluated after a single oral administration of 400 mg to healthy volunteers. The AUC_{0–9 h}, c _max, T _max, and T _1/2 were 86.6 ± 12.7 μg h/mL, 18.4 ± 1.5 μg/mL, 2.63 ± 0.83 and 2.65 ± 0.41 h, respectively. The method was demonstrated to be highly reproducible and feasible for pharmacokinetic studies of ceftibuten in eight volunteers after oral administration (400 mg as ceftibuten).