Synthesis,characterization, and molecular structures of Ni(II) and Cd(II) complexes derived from dithiophosphonate

Two novel dithiophosphonate ligands, HS₂P(p‐C₆H₄OMe)(OCH₂CH₂CH(CH₃)₂) ( 1 ) and HS₂P(p‐C₆H₄OMe)(OCH(CH₃)₂) ( 2 ), were synthesized and characterized by multinuclear (¹H, ³¹P, and ¹³C) NMR, infrared spectroscopy as well as elemental analysis. The reactions of 1 and 2 with NiCl₂·6H₂O and Cd(NO₃)₂·4H₂O in methanol led to novel complexes 3 and 4 . The single crystal X‐ray structures of 3 and 4 showed tetracoordinated structure with square planar geometry for the nickel complex, while it showed pentacoordinated structure with distorted square‐pyramid environment for the cadmium complex.     

Per Aqueous Liquid Chromatography (PALC) as a Simple Method for Native Separation of Protein A

Staphylococcal protein A (protein A) is an important protein frequently used in research studies within the fields of biomedicine and biotechnology. Due to some limitations in available protein purification methods which can hold the native structure of the protein A without changing the folding or adding histidine to structure of this protein, its separation in the native form is difficult. In this study, a new cost-effective and powerful technique was introduced for separation of the full-length and truncated forms of recombinant protein A, without any alteration in their 3D structures. Per aqueous liquid chromatography with bare silica gel stationary phase and water:acetonitrile as the mobile phase was proved to be an attractive choice among the range of separation methods. Similar to hydrophilic liquid chromatography, this method employs high percentage of water in mobile phase. The effects of mobile phase composition, pH, and salt concentration on the retention behavior of protein A on bare silica gel stationary phases were investigated. In this method, applying high amounts of aqueous solvent accompanied by a minimum percentage of organic solvent could successfully separate protein A with preservation of folding, and any affinity-tagged group such as histidine has not occurred on its structure. Purity of the fractions obtained by the proposed method was confirmed using SDS-PAGE, western blotting, and matrix-assisted laser desorption ionization time-of-flight mass spectrometry. According to the results of ELISA, separated proteins retained their ability of binding to antibody.     

纳米尺度氧化石墨烯层作为高效碳催化剂用于苄醇与芳香醛的绿色氧化

合成了纳米尺度氧化石墨烯(NGO)层,用作碳催化剂高效催化苄醇与芳香醛的氧化反应.对于醇氧化反应,当80℃时H2O2存在下,NGOs(20 wt％)可高效催化醇选择性生成醛,其反应速率和产率取决于醇上取代基的性质.对于4-硝基苄醇,反应24 h后,只有10％可转换为相应羧酸.相反,4-甲氧基苄醇和二苯基甲醇分别反应仅9和3h则可完全转化为对应的羧酸和酮.NGO碳催化剂上芳香醛氧化速率高于醇氧化速率.对于所有的醛,采用7 wt％ NGO作催化剂,在70℃反应2-3 h后,就可完全转化为相应羧酸.我们讨论了NGO催化剂结构对苄醇和芳香醛氧化反应影响的可能机理.     

Synthesis and in vitro antibacterial evaluation of 6-substituted 4-amino-pyrazolo[3,4-<Emphasis Type="Italic">d</Emphasis>]pyrimidines

Pyrazolo[3,4-d]pyrimidines are one of the most important classes of fused heterocyclic compounds which exhibit a broad range of biological and medicinal properties. They are known as anticancer, antifungal, antibacterial, antiviral and anti-inflammatory agents. In this study, some new 6-substituted 4-amino-pyrazolo[3,4-d]pyrimidine derivatives were prepared via reaction of 5-amino-3-methyl-1-phenyl-1H-pyrazole-4-carbonitrile with various nitriles in the presence of sodium ethoxide as catalyst. The inhibitory properties of synthesized compounds were studied according to CLSI guidelines against some pathogenic bacteria including four gram-positive strains (Streptococcus pyogenes, Staphylococcus aureus, Bacillus cereus and Bacillus subtilis subsp. spizizenii) and three gram-negative strains (Pseudomonas aeruginosa, Shigella flexneri and Salmonella enterica subsp. enterica). The antibacterial effects of all derivatives were compared with those of antibiotics belonging to different classes. The values were reported as inhibition zone diameter (IZD), minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC). The effect of substituents on the biological activity of derivatives was discussed as well. The inhibitory effect of compound 6a, was shown to be the most, with MIC values in the range of 32–4096 μg/mL. Since most of the synthesized compounds were effective against Streptococcus pyogenes and Pseudomonas aeruginosa, they can be considered as inhibitors of these two bacteria.     

Application of N,N'-Diiodo-N,N'-1,2-ethandiylbis(p-toluene sulfonamide)as a New Reagent for Synthesis of2-Arylbenzimidazoles and 2-Arylbenzothiazoles under Solvent-free Conditions

N,N′‐Diiodo‐N,N′‐1,2‐ethandiylbis(p‐toluene sulfonamide) (NIBTS) is a good and new reagent for synthesis of 2‐arylbenzimidazoles and 2‐arylbenzothiazoles at room temperature under solvent‐free condition with good to high yield. Absence of solvent, short reaction times, non‐corrosive, operational simplicity and environmentally friendliness are the main advantages of this procedure.     

Selective and mild oxidation of sulfides to sulfoxides by H_2O_2 using DBUH-Br_3 as catalyst

<正>DBUH-Br_3 catalyzed selective conversion of sulfides to sulfoxides in the presence of H_2O_2 as oxidizing agent is described.The reaction was performed selectively at room temperature and relatively short reaction times.     

Prediction of sound velocity and compressibility via molecular simulation at fixed entropy

A molecular-level simulation route is proposed to compute the isentropic thermodynamic properties in a fluid system by Monte Carlo simulation at fixed entropy. The method involves computation of the pressure response of a system to an infinitesimal change in system density by introduction of a single molecule, while retaining the system volume as well as the absolute molar entropy. The probability for accepting a change in temperature during the Monte Carlo moves was weighted against the argument proposed by Smith et al. [W.R. Smith, M. Lísal, I. Nezbeda, Chem. Phys. Lett. 426 (2006) 436–440]. Application to fluid argon has confirmed superior accuracy for the technique within the gas state to yield results within 1.2% of the measured values for the range of thermodynamic conditions investigated.     

Trace amounts determination of lead,zinc and copper by adsorptive stripping voltammetry in the presence of dopamine

A selective and sensitive method for simultaneous determination of lead, zinc and copper by adsorptive differential pulse cathodic stripping voltammetry is presented. The method is based on adsorptive accumulation of the complexes of Pb(II), Zn(II), and Cu(II) ions with dopamine onto hanging mercury drop electrode (HMDE), followed by reduction of adsorbed species by differential pulse cathodic stripping voltammetry. The effect of experimental parameters such as pH, dopamine concentration, accumulation time and potential and scan rate were examined. Under the optimized conditions, linear calibration curves were established for the concentration of Pb, Zn, and Cu in the ranges of 5–150, 5–250, and 1–150 ng/mL, respectively. Detection limits of 0.06, 0.25, and 0.04 ng/mL for Pb, Zn, and Cu were obtained. An application of the proposed method is reported for the determination of these elements in some real samples such as natural waters and alloys.     

Preparation and utilization of a molecularly imprinted polymer for solid phase extraction of tramadol

In this paper, a highly selective molecularly imprinted polymer (MIP) for tramadol hydrochloride, a drug used to treat moderate to severe pain, was prepared and its use as solid-phase extraction (SPE) sorbent was demonstrated. The molecularly imprinted solid-phase extraction procedure followed by high performance liquid chromatography with ultraviolet detector (MISPE-HPLC) was developed for selective extraction and determination of tramadol in human plasma and urine. The optimal conditions for molecularly imprinted solid-phase extraction (MISPE) consisted of conditioning with 1 mL methanol and 1 mL of deionized water at neutral pH, loading of tramadol sample (50 μg L⁻¹) at pH 7.5, washing using 1 mL acetone and elution with 3 × 1 mL of 10% (v/v) acetic acid in methanol. The MIP selectivity was evaluated by checking several substances with similar molecular structures to that of tramadol. Results from the HPLC analyses showed that the calibration curve of tramadol (using MIP from human plasma and urine) is linear in the ranges of 6–100 and 3–120 μg L⁻¹ with good precisions (1.9% and 2.9% for 5.0 μg L⁻¹), respectively. The recoveries for plasma and urine samples were higher than 81%.