Driving the photoluminescent and structural properties of X2-Y2SiO5 by varying the dopant Dy3+ concentration towards cool WLED applications

Dy³⁺ doped Y₂SiO₅ nanophosphors were synthesized by solution combustion technique using Calotropis gigantean milk latex and NaCl as fuel and flux respectively. Powder X-ray diffraction (PXRD) confirmed the formation of monoclinic X₂-phase Y₂SiO₅ belonging to the phase group C₂/c. Fourier transform infrared spectroscopy (FTIR) shows characteristic metal–oxygen (Y–O) vibration band at 721 cm⁻¹. Transmission electron microscopic (TEM) and Scanning electron microscopic (SEM) morphological feature exhibits non-uniform almost spherical shaped nanosized particles. The photoluminescence (PL) emission peaks, recorded at 388 nm, showed radiative emissions at 483, 575 and 636 nm respectively. Judd–Ofelt (JO) analysis was carried out to estimate the radiative (A_R) properties, radiative life time (τ_R), branching ratio (β_R) and stimulated emission crossection (σλ_p). The CIE and CCT was estimated using McCamy empirical formula. In the beginning, the CIE co-ordinate values were lying in the light blue region. However, with increase in Dy³⁺ concentration the values shifted towards white region. CCT value was found to be ∼6984 K. Therefore, Y₂SiO₅:Dy³⁺ (9 mol%) can be used for cool day light and WLED applications.     

Applying green analytical chemistry for development and validation of RP-HPLC stability indicating assay method for estimation of fenoverine in bulk and dosage form using quality by design approach

A green and robust reverse-phase liquid chromatographic method has been developed for the determination of fenoverine (FEN), by applying combined principles of green analytical chemistry and quality by design approaches on a Spherisorb C18 column (150?×?4.6?mm, 3?µm) with UV detection at 262?nm. A two level fractional factorial design (2^^7-3) Res IV was used for screening of influential chromatographic factors. The critical method parameters actively affecting critical quality attributes (CQAs) were identified and further optimized using Box–Behnken design. The predicted optimum assay conditions comprised of methanol and ammonium acetate buffer 20?mM, in an extent of 81:19% v/v individually having a flow rate of 1.0?mL/min with a column oven temperature of 33°C. The drug was stressed in hydrolytic, oxidative, reductive, thermal, and photolytic conditions. The developed method was validated successfully. The detector response was linear in the concentration of 0.5–160?µg/mL with a limit of detection (LOD) and limit of quantitation (LOQ) as 0.1 and 0.3?µg/mL, respectively. The % recovery was found to be 99.7%. The analytical method volume intensity value for developed method was 45?mL and the environment assessment tool (EAT) score was 41.07. The method is simple, environmentally benign, rapid, and robust for the determination of FEN in bulk and in its dosage form.     

Development and validation of high-performance thin-layer chromatographic method for determination of amygdalin

ABSTRACT

A new method for the extraction and quantitative determination of amygdalin has been proposed. Accelerated solvent extraction was applied for the extraction, and reversed-phase high-performance thin-layer chromatography method was developed, validated, and applied for the determination of amygdalin in the extracts of apricot, plum, almond, and peach kernels. The chromatographic system used was RP-18 silica, as stationary phase and acetonitrile/water (50:50, v/v), as mobile phase. Densitometric scanning was performed at 210 nm. The method was validated with respect to specificity, linearity, precision, and accuracy. The results showed that the peak area responses were linear within the concentration range of 2.5–50.0 µg/spot (R² = 0.9984). The limit of quantification was 4.28 µg/spot, and the detection limit 1.28 µg/spot. The intra-day and inter-day reproducibility, in terms of %RSD, were in the range of 0.81–1.15 and 1.32–1.89, respectively. The accuracy data were in the range from 99.98 to 100.56%. The method is linear, quantitative and reproducible, and could be used as an efficient and economical green chromatographic procedure for the determination of amygdalin in the fruit kernel.     

Tracing (r)bST in cattle: Liquid-based options for extraction and separation

Growth hormone (GH) or somatotropin (ST) is a species-specific polypeptide hormone produced in the pituitary gland of vertebrates. When administered exogenously to dairy cattle, it has galactopoietic effects and is capable of increasing the milk yield. The beginning of the commercial production of recombinant variants of bovine somatotropin (rbST), by the end of the 20th century, had a major economic impact in the dairy industry. Recombinant bST enabled large-scale applications in farms, enhancing significantly milk production. While it is banned in the European Union (EU), several countries permit the trade and use of recombinant somatotropins in animal husbandry. Also, rbST-free dairy products can be frequently found in the market of those countries, even though these labels are not actually verified in a laboratory. In this context, effective analytical methods are needed for residue control to avoid an illegal use of rbST but also to prevent fraudulent labeling in some cases. The present review includes studies published in the last 5 years (from 2012 to 2017) to monitor rbST in bovine animals, using liquid-based applications. It is then intended to serve as a practical guide to help those laboratories interested in developing analytical methods to detect rbST use and abuse.     

Rasagiline-encapsulated chitosan-coated PLGA nanoparticles targeted to the brain in the treatment of parkinson's disease

The aim of this study was to investigate the brain targeting potential of rasagiline-encapsulated chitosan-coated PLGA nanoparticles (RSG-CS-PLGA-NPs) delivered intranasally into the brain. Chitosan-coated PLGA nanoparticles (RSG-CS-PLGA-NPs) were developed through double emulsification-solvent evaporation technique. RSG-CS-PLGA-NPs were characterized for particle size, zeta potential, size distribution, encapsulation efficiency, and in vitro drug release. The mean particle size, polydispersity index, and encapsulation efficiency were found to be 122.38?±?3.64, 0.212?±?0.009, and 75.83?±?3.76, respectively. High-performance liquid chromatography–mass spectroscopy and mass spectroscopy study showed a significantly high mucoadhesive potential of RSG-CS-PLGA-NPs and least for conventional and homogenized nanoformulation. Pharmacokinetic results of RSG-CS-PLGA-NPs in Wistar rat brain and plasma showed a significantly high (**p?<?0.005) AUC_0-24 and amplified C_max over intravenous treatment group. Finally, the investigation demonstrated that intranasal delivery of mucoadhesive nanocarrier showed significant enhancement of bioavailability in brain, after administration of the RSG-CS-PLGA-NPs which could be a substantial achievement of direct nose to brain targeting in Parkinson’s disease therapy and related brain disorders.     

Stability-indicating RP-HPLC method for simultaneous quantitation of tramadol and aceclofenac in presence of their major degradation products: Method development and validation

Primary objective of this study was to develop a stability-indicating reverse-phase high-performance liquid chromatography (HPLC) method for simultaneous quantitation of tramadol and aceclofenac in presence of their degradation products. The drugs were subjected to various International Conference on Harmonization recommended stress conditions, such as acid hydrolysis, alkaline hydrolysis, peroxide oxidation, thermolysis, and photolysis. The major degradation products got well resoluted from the analytes in HPLC analysis with a mobile phase composed of a mixture of 0.01?M ammonium acetate buffer (pH 6.5) and acetonitrile (65:35, v/v) through a Phenomenex Gemini C18 (250?mm?×?4.6?mm, 5?µm particle size) column. The method was linear over a range of 15–60?µg/mL for tramadol and 40–160?µg/mL for aceclofenac concentration. The analytes were detected at a wavelength of 270?nm. The method was validated and found to be specific, accurate, precise, stable, and robust for its intended use. The method can be recommended for its future use in routine quality control, accelerated and real-time stability analysis of the formulations containing tramadol and aceclofenac combination.     

One-step mild hydrothermal method to prepare low valent sodium vanadium(III) monohydrogenphosphate: NaV(HPO4)2

Green colored single crystals of a reduced sodium vanadium(III) monohydrogenphosphate, NaV(HPO₄)₂, were grown using a one-step mild hydrothermal method. The in situ reduction of V⁵⁺ to V³⁺ was performed using copper acetate as the reducing agent. The title compound crystalizes in the monoclinic space group Cc and exhibits a three-dimensional crystal structure that consists of distorted VO₆ octahedra connected to PO₃(OH) tetrahedra that are further connected via Na cations. The compound exhibits simple paramagnetic behavior at high temperatures and a discontinuity near 5 K is likely due to the onset of magnetic coupling. The compound was also characterized by TGA, IR and UV–vis spectroscopies.     

基于虚拟相位平面的相位展开方法

在基于相位分析的三维测量系统中,为了准确地得到物体的高度,相位展开扮演着很重要的角色。传统的相位展开方法常常需要额外的投影图,而傅里叶变换轮廓术只需要采集一幅或两幅变形条纹图就可以实现对物体轮廓的测量,其方法速度快,易于实现。针对傅里叶变换轮廓术方法计算得到的截断相位分布,本文提出了一种利用截断相位与参考平面相位差值2π的整数倍数获得截断相位的正确级次,辅助相位展开的方法。当被测物体较复杂,或者相位截断次数较多时,该方法在已有参考平面相位的基础上虚拟新的相位平面,依次比较截断相位和虚拟相位,进行多次分级相位展开,结合多个展开相位结果,最终得到正确的展开相位。该方法展开速度快,展开错误不会蔓延传递。仿真和实物实验结果证明了该方法的可行性,说明该方法可用于傅里叶变换轮廓术中进行截断相位的快速展开。     

Structural Elucidation of Trace Amounts of Volatile Compounds Using the Crystalline Sponge Method

Volatile organic compounds are widely present as scents and odors in our daily lives and are readily found in a variety of natural extracts. Because these compounds are highly volatile and usually available only in minute quantities, little attention has been paid to X‐ray diffraction as a technique for their structure determination. Here, we show that the structures of volatile organic compounds are easily elucidated using minute quantities of the compounds and the crystalline sponge method. The compound vapors can be directly absorbed into the sponge crystals, or alternatively, preparative gas chromatography can be used to separate the desired compound from a natural mixture.     

Gold‐Catalyzed Suzuki Coupling of ortho‐Substituted Hindered Aryl Substrates

A method that allows hindered ortho ‐substituted aryl iodides to be efficiently coupled to phenylboronic acid using a gold‐catalyzed C−C bond formation is presented. The use of a molecularly‐defined dinuclear gold chloride catalytic precursor that is stabilized by a new tetradentate (N ,N′ )‐diamino‐(P,P′ )‐diphosphino ferrocene hybrid ligand in a Suzuki‐type reaction is described for the first time. Electron‐rich isopropyl groups on phosphorus were found essential for a superior activity, while the performances of a set of analogous gold dinuclear complexes that were fully characterized by multinuclear NMR spectroscopy and XRD analysis, were investigated. Therefore, arylation of para and ortho ‐substituted iodoarenes bearing electron‐rich, electron‐poor functional groups, and even hindered polycyclic aromatic compounds is described.