Simultaneous dual-wavelength CW laser operation at 1064 and 930 nm in Nd<Superscript>3+</Superscript>:YAlO<Subscript>3</Subscript>

A dual-wavelength continuous-wave (CW) diode end-pumped Nd³⁺:YAlO₃ (Nd:YAP) laser that generates simultaneous laser action at the wavelengths 1064 and 930 nm is demonstrated. A total output power of 2.15 W (1.57 W at 1064 nm and 0.58 W at 930 nm) for the dual-wavelength was achieved at the incident pump power of 17.8 W with optical conversion efficiency of 12.1%. The M ² values for 930 and 1064 nm lights were found to be around 1.21 and 1.32, respectively.     

Identification of heparin samples that contain impurities or contaminants by chemometric pattern recognition analysis of proton NMR spectral data

Chemometric analysis of a set of one-dimensional (1D) (1)H nuclear magnetic resonance (NMR) spectral data for heparin sodium active pharmaceutical ingredient (API) samples was employed to distinguish USP-grade heparin samples from those containing oversulfated chondroitin sulfate (OSCS) contaminant and/or unacceptable levels of dermatan sulfate (DS) impurity. Three chemometric pattern recognition approaches were implemented: classification and regression tree (CART), artificial neural network (ANN), and support vector machine (SVM). Heparin sodium samples from various manufacturers were analyzed in 2008 and 2009 by 1D (1)H NMR, strong anion-exchange high-performance liquid chromatography, and percent galactosamine in total hexosamine tests. Based on these data, the samples were divided into three groups: Heparin, DS ≤ 1.0% and OSCS = 0%; DS, DS > 1.0% and OSCS = 0%; and OSCS, OSCS > 0% with any content of DS. Three data sets corresponding to different chemical shift regions (1.95-2.20, 3.10-5.70, and 1.95-5.70 ppm) were evaluated. While all three chemometric approaches were able to effectively model the data in the 1.95-2.20 ppm region, SVM was found to substantially outperform CART and ANN for data in the 3.10-5.70 ppm region in terms of classification success rate. A 100% prediction rate was frequently achieved for discrimination between heparin and OSCS samples. The majority of classification errors between heparin and DS involved cases where the DS content was close to the 1.0% DS borderline between the two classes. When these borderline samples were removed, nearly perfect classification results were attained. Satisfactory results were achieved when the resulting models were challenged by test samples containing blends of heparin APIs spiked with non-, partially, or fully oversulfated chondroitin sulfate A, heparan sulfate, or DS at the 1.0%, 5.0%, and 10.0% (w/w) levels. This study demonstrated that the combination of 1D (1)H NMR spectroscopy with multivariate chemometric methods is a nonsubjective, statistics-based approach for heparin quality control and purity assessment that, once standardized, minimizes the need for expert analysts.     

Determination of galactosamine impurities in heparin samples by multivariate regression analysis of their <Superscript>1</Superscript>H NMR spectra

Heparin, a widely used anticoagulant primarily extracted from animal sources, contains varying amounts of galactosamine impurities. Currently, the United States Pharmacopeia (USP) monograph for heparin purity specifies that the weight percent of galactosamine (%Gal) may not exceed 1%. In the present study, multivariate regression (MVR) analysis of ¹H NMR spectral data obtained from heparin samples was employed to build quantitative models for the prediction of %Gal. MVR analysis was conducted using four separate methods: multiple linear regression, ridge regression, partial least squares regression, and support vector regression (SVR). Genetic algorithms and stepwise selection methods were applied for variable selection. In each case, two separate prediction models were constructed: a global model based on dataset A which contained the full range (0–10%) of galactosamine in the samples and a local model based on the subset dataset B for which the galactosamine level (0–2%) spanned the 1% USP limit. All four regression methods performed equally well for dataset A with low prediction errors under optimal conditions, whereas SVR was clearly superior among the four methods for dataset B. The results from this study show that ¹H NMR spectroscopy, already a USP requirement for the screening of contaminants in heparin, may offer utility as a rapid method for quantitative determination of %Gal in heparin samples when used in conjunction with MVR approaches.     

Syntheses, structures and properties of silver-organic frameworks constructed with 1,2,3,4-benzenetetracarboxylic acid

The reactions of 1,2,3,4-benzenetetracarboxylic acid (H(4)mpda) and different silver(I) salts under hydrothermal or solvent evaporation conditions yielded four unusual coordination complexes with interesting frameworks: [Ag(4)(mpda)](n) (1), {[Ag(2.5)(mpda)(bpy)(2)]·[Ag(bpy)]·[Ag(bpy)(H(2)O)]·(NO(3))(0.5)·(H(2)O)(9)}(n) (2), {[Ag(5)(mpda)(2)(bpy)(4)]·[Ag(bpy)]·[Ag(bpy)(H(2)O)]·[Ag(bpy)(H(2)O)]·(H(2)O)(16)}(n) (3), {[Ag(2)(mpda)(H(2)O)]·[Ag(bpy)]·[Ag(bpy)]}(n) (4) (bpy = 4,4'-bipyridine). Complex 1 displays a novel (3,4,7)-connected {4.6(2)}{4.6(5)}{4(2).6(13).8(5).10} topology, in which the carboxylic groups of the mpda(4-) ligand adopt variable coordination modes. In 1, besides Ag-O coordination bonding, AgAg and Agaromatic intermolecular interactions also make their appearance. In complexes 2-4, rare architectures comprising three or four isolated coordination polymers within the same crystalline structure have been obtained, respectively. In 2 and 3, neighboring layers are linked together through water tapes into a three-dimensional supramolecular architecture, which is also consolidated by π···π stacking, while independent infinite rod-like polymer chains fill the void space between layers. Interestingly, an anionic (H(2)O-NO(3)(-))(n) layer, built from water tapes and nitrate anions as well as consolidated by the mpda(4-) ligands, has been structurally identified in compound 2. A new water tape constructed from alternating tetramers and decamers has been obtained in compound 3. In compound 4, a right-handed helical chain and two rod-like polymeric chains are interconnected through host-guest molecular recognition to generate a three-dimensional chiral supramolecular architecture. Bulk materials for 1 and 4 have second-harmonic generation activity, being approximately 0.6 and 0.4 times that of urea. The IR spectra, thermogravimetric analysis and luminescent properties of all compounds were also investigated.     

Study of proton resonances in 18Ne via resonant elastic scattering of 17F+p and its astrophysical implication

The proton resonant properties in ¹⁸Ne, which determine the reaction rate of the key stellar ¹⁴O(α,p)¹⁷F reaction, have been studied by using a technique of proton resonant elastic scattering of ¹⁷F+p. A 4.22 MeV/nucleon ¹⁷F radioactive ion (RI) beam was produced via a projectile-fragmentation reaction, and separated by a Radioactive Ion Beam Line in Lanzhou (RIBLL). By bombarding a thick (C_H2) _n target, the energy spectra of the recoiled protons were measured by two ΔE-E silicon telescopes at the center-of-mass scattering angles of θ _c.m.≈175°±5°, θ _c.m.≈152°±8°, respectively. Several proton resonances in ¹⁸Ne were observed clearly. A further R-matrix analysis of the experimental data is under way to determine the resonant parameters. The present work reports the preliminary results briefly.     

A series of POM-based entangled frameworks with the rigid ligand 1,4-bis(1-imidazolyl)benzene and different isomers of octamolybdate

With BIMB ligand, we have successfully obtained and characterized three novel entangled inorganic-organic hybrid compounds by choosing different metal ions, that is, [Ni(BIMB)₂(γ-Mo₈O₂₆)_0.5]·3H₂O (1), [Zn(BIMB)₂(γ-Mo₈O₂₆)_0.5] (2), and [Cu₃(BIMB)₄(H₂O)(δ-Mo₈O₂₆)Cl₂]·3H₂O (3) (where BIMB=1,4-bis(1-imidazolyl)benzene). Compound 1 is a 2-fold interpenetration 4-connected 3D framework with the short Schläfli symbol of (4×6⁴×8)₂(4²×6²×8²), in which octamolybdate anion shows γ-isomer; 2 exhibits a (5,6)-connected 3D self-penetrating topological motif with the short Schläfli symbol of (4×5⁷×6²)₂(4²×5¹¹×7²), and 3 shows a (4,6)-connected self-penetrating 3D framework with the short Schläfli symbol of (4²·5²·6·7) (4⁴·5·6⁹·8) (5⁴·6²) whose octamolybdate has δ-isomer. In addition, the optical band gaps of these three compounds have been measured, which are 2.98 eV for 1, 3.42 eV for 2, and 2.88 eV for 3. Moreover, 2 has photoluminescent property, which can be attributed to ligand-to-metal charge-transfer (LMCT) band.     

Antifungal evaluation of cholic acid and its derivatives on Candida albicans by microcalorimetry and chemometrics

Multi-hydroxyl amines including tris(hydroxymethyl)aminomethane (Tris), serinol and ethanolamine were selected as weak affinity ligands using a rapid screening by quartz crystal microbalance (QCM) biosensor. Based on the specific recognition between the ligands and two proteins, lysozyme (LZM) and cytochrome c (Cyt c), a weak affinity chromatography method was developed for specific separation of the two proteins. The frontal analysis results showed that the apparent dissociation constants (K_D) of ligand–protein complexes were all in the order of weak affinity (10⁻⁴ M). By weak affinity columns modified with the three multi-hydroxyl amines individually, LZM and Cyt c were baseline separated as retarded peaks from non-specific protein and each other in a single cycle of loading and eluting. Moreover, the Tris-modified column typically showed the satisfactory repeatability and stability as a new type of weak affinity columns. The present strategy composed of QCM selecting and affinity chromatography separating was promising to extend the variety of weak affinity ligands and develop inexpensive specific affinity methods for separation and purification of multiple proteins on one single column.     

Development of ultrasound-assisted emulsification microextraction for the determination of triazine herbicides in environmental water samples by high-performance liquid chromatography

A simple, rapid, efficient, and environmentally friendly method for the determination of some triazine herbicides (simazine, atrazine, prometone, ametryn and prometryne) in water samples was developed by ultrasound-assisted emulsification microextraction (USAEME) coupled with high-performance liquid chromatography-diode array detection (HPLC-DAD). The main parameters that affect the extraction efficiencies, such as the kind and volume of the extraction solvent, ultrasound emulsification time and salt addition, were investigated and optimized. Under the optimum conditions, the method was sensitive and showed a good linearity within a range of 0.5 to 200?ngm?L^?1 for simazine, atrazine, prometone, ametryn and prometryne, with the correlation coefficients (r) varying from 0.9993 to 0.9998. High enrichment factors were obtained ranging from 148 to 225. The limits of detection (LODs) were in the range between 0.06 and 0.1?ngm?L^?1 and the limits of quantification (LOQs) were in the range between 0.2 and 0.3?ngm?L^?1. The recoveries of the analytes from water samples at spiking levels of 5.0 and 50.0?ngm?L^?1 were ranged from 82.4% to 107.0%. The relative standard deviations (RSDs) varied from 3.0% to 4.6%. The results demonstrated that the USAEME-HPLC-DAD method was an ef?cient pretreatment and enrichment procedure for the determination of triazine pesticides in real water samples.     

The use of silica‐coated magnetic graphene microspheres as the adsorbent for the extraction of pyrethroid pesticides from orange and lettuce samples followed by GC–MS analysis

Graphene‐grafted ferroferric oxide microspheres were used as the adsorbent to extract some pyrethroid pesticides (bifenthrin, λ‐cyhalothrin, cyfluthrin, cypermethrin, fenvalerate, and deltamethrin) from orange and lettuce samples prior to their determination by GC–MS. The main variables that could affect the extraction, including the amount of the adsorbent, pH of the sample solution, extraction time, concentration of salt, and desorption conditions, were investigated and optimized. Under the optimized conditions, a linear response was obtained in the concentration range of 0.3–100.0 ng/g for the analytes with the coefficients of determination ranging from 0.9877 to 0.9925. The LODs for the pyrethroids ranged from 0.01 to 0.02 ng/g. The method provided a good repeatability with RSDs < 10.6%. The recoveries for the six pyrethroid pesticides were in the range from 90.0 to 103.7%. The method was applied to the determination of the pesticides in orange and lettuce samples with a satisfactory result.     

基于分形理论的飞机雷击初始附着点的数值模拟

飞机雷击附着点的确定能够为飞机防雷设计提供依据,是飞机雷击区域划分和飞机各部件进行雷电试验鉴定的先决条件.本文提出了一种基于分形理论的飞机雷击初始附着点数值模拟的新方法.该方法首先依据标准SAE-ARP5416中有关飞机雷击附着点试验的规定,确定放电间隙、雷电起始坐标、飞机姿态和放电次数等参数,然后根据分形理论,使用电介质击穿模型模拟符合自然界雷电物理机理和几何特征的雷电先导分形发展过程,同时考虑飞机自身触发双向先导的情况,最终得到飞机的雷击附着点分布.通过本文方法仿真模拟得到飞机F-4雷击附着点的分布概率,并分别与该飞机飞行实验和实验室高压放电实验测试得到的真实雷击附着点的概率分布情况比较,结果基本吻合,验证了该方法的有效性.研究结果为飞机雷击附着点仿真模拟提供了一个有潜力的方法,可作为飞机防雷设计和今后开展相关研究工作的基础.