Visible light-promoted metal-free aerobic oxyphosphorylation of olefins: A facile approach to β-ketophosphine oxides

A metal-free direct aerobic oxyphosphorylation of alkenes with H-phosphine oxides has been developed utilizing visible light photoredox catalysis. A variety of β-ketophosphine oxides have been obtained in good yields from simple olefins under air with inexpensive rhodamine B as the non-metallic photocatalyst. This method provides a mild, green, and practical synthetic approach to valuable β-ketophosphine oxides.     

Boron-Cluster Embedded Necklace-Shaped Nanohoops

The combination of carbon-based nanohoops with other functional organic molecular structures should lead to the design of new molecular configurations with interesting properties. Here, necklace-like nanohoops embedded with carborane were synthesized for the first time. The unique deboronization of o-carborane has led to the facile preparation of ionic nanohoop compounds. Nanohoops functionalized by nido-o-carborane show excellent fluorescence emission, with a solution quantum yield of up to 90.0 % in THF and a solid-state quantum efficiency of 87.3 %, which opens an avenue for the applications of the nanohoops in OLEDs and bioimaging.     

Sonochemical synthesis and characterization of three nano zinc(II) coordination polymers; Precursors for preparation of zinc(II) oxide nanoparticles

Nanostructures of three Zinc(II) coordination polymers, [Zn(NNO)₂(H₂O)₄]_n (1), [Zn(PNNO)₂(H₂O)₂]_n (2) and [Zn(H₂O)₆]·(INNO)₂ (3) {NNO: Nicotinic acid N-oxide, PNNO: Picolinic acid N-oxide and INNO: Isonicotinic acid N-oxide}, have been synthesized by a sonochemical process and reaction of ligands with Zn(CH₃COO)₂. The Zinc(II) oxide nano-particles have been synthesized from thermolysis of [Zn(NNO)₂(H₂O)₄]_n (1), [Zn(PNNO)₂(H₂O)₂]_n (2) and [Zn(H₂O)₆]·(INNO)₂ (3) at two different methods (with surfactant and without surfactant) and two temperatures (200 and 600 °C). The ZnO nanoparticles were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Comparison of the SEM images of ZnO nano-particles at two different methods and temperatures shows that higher temperature results in an increasing of agglomeration and thus small and spherical ZnO particles with good separation were produced by thermolysis of compounds at 200 °C and by use of surfactant.     

The disinfection effect of a novel continuous-flow water sterilizing system coupling dual-frequency ultrasound with sodium hypochlorite in pilot scale

In this paper, a self-designed novel continuous-flow water disinfection system coupling dual-frequency ultrasound (US) with chemical disinfectant sodium hypochlorite (NaClO) was tested in a pilot scale using a simulated effluent containing Bacillus subtilis (B. subtilis), one of the indicators of water treatment efficiency. A suspension having a B. subtilis concentration of approximately 10⁴ CFU/mL was introduced into the system to (1) investigate disinfection efficiency of US pretreatment with NaClO (US + NaClO) and simultaneous US and NaClO (US/NaClO) disinfection under different single frequencies; (2) further examine the disinfection efficiency of these two processes with dual-frequency US; and (3) identify dosage reduction of chlorine in this disinfection system. The results demonstrated that lower dual-frequency (17 kHz + 33 kHz) US pretreatment with NaClO disinfection and simultaneous higher dual-frequency (70 kHz + 100 kHz) US and NaClO were beneficial to bacterial inactivation in terms of sterilizing efficiency. It has also been observed that US pretreatment with lower combination of 17 + 33 kHz frequencies showed better enhancement in which log reduction reached to 3.82 after 10 min chlorine reaction (chlorine alone was 0.22 log reduction), nearly 1 log reduction higher than single frequencies at the same constant power. Consequently, at equivalent power dissipation levels, US of lower frequencies combination pretreatment with NaClO disinfection performed such a promising process that one-thirds (from 12 mg/L NaClO reduced to 8 mg/L NaClO) of the required NaClO dosage was reduced for the ideal disinfection efficiency of 4 log reduction, namely 100% disinfection. And the utilization efficiency of NaClO was increased from 37.67% to 85.25% in 30 min of treatment time using an optimized combination of pretreatment and chlorination.     

Determination of Prometryne in water and soil by HPLC-UV using cloud-point extraction

A CPE-HPLC (UV) method has been developed for the determination of Prometryne. In this method, non-ionic surfactant Triton X-114 was first used to extract and pre-concentrate Prometryne from water and soil samples. The separation and determination of Prometryne were then carried out in an HPLC-UV system with isocratic elution using a detector set at 254 nm wavelength. The parameters and variables that affected the extraction were also investigated and the optimal conditions were found to be 0.5% of Triton X-114 (w/v), 3% of NaCl (w/v) and heat-assisted at 50 °C for 30 min. Using these conditions, the recovery rates of Prometryne ranged from 92.84% to 99.23% in water and 85.48% to 93.67% in soil, respectively, with all the relative standard deviations less than 3.05%. Limit of detection (LOD) and limit of quantification (LOQ) were 3.5 μg L⁻¹ and 11.0 μg L⁻¹ in water and 4.0 μg kg⁻¹ and 13.0 μg kg⁻¹ in soil, respectively. Thus, we developed a method that has proven to be an efficient, green, rapid and inexpensive approach for extraction and determination of Prometryne from soil samples.     

Microwave‐promoted Synthesis of Novel Fused Osthole Analogues

Osthole is a natural coumarin derivative and has a broad scope of biological activities. Two series of novel fused osthole analogues were designed, and synthesized through a highly efficient microwave‐promoted synthetic protocol via the reaction of 4‐hydroxycoumarins and β‐ketoesters. The reaction conditions including solvent, catalyst, microwave power and irradiation time were also optimized. The pyrano[3,2‐c]chromene‐2,5‐diones and furo[3,2‐c]coumarins were obtained through two distinct intramolecular cyclization processes, and the proposed mechanism was also discussed.     

菠菜和苏州青类囊体溶液的光谱特性

通过分析不同波长光激发下菠菜(Spinach)和苏州青(Suzhou Green)类囊体溶液的发射光谱和荧光光谱,以及同一波长下磁场处理前后类囊体溶液的光谱变化,探讨了低强度稳恒磁场对类囊体溶液的作用机理.结果表明,类囊体溶液中形成了大量的氢键,磁场处理前菠菜和苏州青的氢键喇曼散射峰为531 nm和533.2 nm,两者光系统II(PSII)荧光分别在689.8 nm和686 nm;磁场处理后两者的喇曼散射峰变为532.8 nm和532.4 nm,PSII荧光变为686.8 nm和685.4 nm.磁场改变了两样品中氢键键能,使其趋于相等.     

Comparison of oil-in-water emulsions prepared by ultrasound,high-pressure homogenization and high-speed homogenization

This study was designed to compare the properties of myofibrillar protein (MP) stabilized soybean oil-in-water emulsions fabricated by ultrasound-assisted emulsification (UAE), high-pressure homogenization (HPH) and high-speed homogenization (HSH). The emulsion properties, droplet characteristics, interfacial proteins, protein exposure extent, microrheological properties, multiple light scattering results, and 7 d storage stabilities of the three emulsions were specifically investigated. Our results indicate that UAE and HPH were better emulsification methods than HSH to obtain high-quality emulsions with higher emulsifying activity index (UAE 20.73 m²·g⁻¹, HPH 11.76 m²·g⁻¹ and HSH 6.80 m²·g⁻¹), whiteness (UAE 81.05, HPH 80.67 and HSH 74.09), viscosity coefficient (UAE 0.44 Pa·sⁿ, HPH 0.49 Pa·sⁿ and HSH 0.22 Pa·sⁿ), macroscopic viscosity index (UAE 2.31 nm⁻²·s, HPH 0.38 nm⁻²·s and HSH 0.34 nm⁻²·s), and storage stability, especially for the UAE. Furthermore, UAE was a more efficient emulsification method than HPH to prepare the fine MP-soybean oil emulsion. The protein-coated oil droplets were observed in the three emulsions. The emulsion droplet size of the UAE-fabricated emulsion was the lowest (0.15 μm) while the interfacial protein concentration (93.37%) and the protein exposure extent were the highest among the three emulsions. During the 7 d storage, no separation was observed for the UAE-fabricated emulsion, while the emulsions fabricated by HPH and HSH were separated after storage for 5 d and 2 h. Therefore, this work suggests that UAE could be a better method than HPH and HSH to fabricate MP-soybean oil emulsion.     

Synthesis and bioactivity of novel 3-(1-hydroxyethylidene)-5-substituted-pyrrolidine-2,4-dione derivatives

Ten novel 5-substituted derivatives of 3-(l-hydroxyethylidene)pyrrolidine-2,4-dione were synthesized.The compounds were confirmed by IR,:H NMR,MS and elemental analysis.The bioassay indicated that these compounds showed noticeable herbicidal activities,and compounds 6f and 6j exhibited excellent inhibitory activities against the stalk of Echinochloa crusgalli,with EC50 values of 94.4 and 72.7 mg/L,respectively.     

S,S-氰戊菊酯间接竞争酶联免疫吸附分析方法研究

合成了S,S-氰戊菊酯的半抗原S-2-(4-氯苯基)-3-甲基丁酸-α-S-(N-丁酸基)-甲酰氨-(3-苯氧基)苄酯(Efvb).半抗原通过混合酸酐法与卵清蛋白(OVA)偶联作为包被抗原,活泼酯法与牛血清蛋白(BSA)偶联作为免疫抗原.用免疫抗原免疫新西兰大白兔,得到抗S,S-氰戊菊酯多克隆抗体.通过异源分析及检测条件优化,确立了间接竞争酶联免疫分析方法的最佳检测条件为pH 7.4,0.4 mol/L Na+、40％甲醇-PBS溶液,建立了S,S-氰戊菊酯酶联免疫分析方法.方法的抑制中浓度(IC50)值为(3.16±0.01)mg/L;检出限(IC10)为(0.0053±0.0012) mg/L.对甲氰菊酯、溴氰菊酯、氯氰菊酯、三氟氯氰菊酯及其代谢物戊菊酸没有明显交叉反应.在自来水、河水和土壤样品中添加S,S-氰戊菊酯,其回收率分别为82.3％～108.2％,83.1％～109.2％和72.0％～91.2％.