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1.
This study reports a deep eutectic solvent based dispersive liquid-liquid microextraction (DES-DLLME) to extract aromatic amines (4-chloroaniline, 3-nitroaniline, 2-naphtylamine) in environmental water samples before their HPLC-UV determination. The hydrophobic deep eutectic solvent (DES) was prepared by mixing bis(2-ethylhexyl) phosphate (BEHP) as a hydrogen bond acceptor and phenol as a hydrogen bond donor. Affecting factors on the extraction of the aromatic amines were investigated and optimized. Optimum conditions were: DES type: BHHP-Ph ratio: 1 to 2; pH of solution: 8.0; DES volume: 80 µL, salt amount: 10% (w/v). Under optimum conditions, the developed method showed a wide linear range of 0.2–200 µg L?1 (R2 ≥ 0.99) with satisfactory recoveries (≥90.0%). The limit of detections (LODs) and limit of quantifications (LOQs) were in the range of 0.07–0.17 µg L?1 and 0.2–0.5 µg L?1, respectively. The enrichment factors were 170, 180 and 190 for 4-chloroaninile, 3-nitroaniline, 2-naphtylamine, respectively. Based on obtained results, the proposed method is straightforward, efficient, sensitive, and eco-friendly for the extracting and determining of the aromatic amines in environmental water samples.  相似文献   
2.
采用铜/锌复合金属磷酸盐晶体和海藻酸钙凝胶双重包覆技术对漆酶进行固定化, 制得石榴状Alg@Cu3/Zn3(PO4)2@Lac的凝胶微球. SEM, EDX和FTIR表征结果表明, 在凝胶微球内部, 漆酶被成功固定于由海藻酸钙凝胶包覆的铜/锌复合金属磷酸盐晶体内, 铜/锌复合金属磷酸盐晶体镶嵌于海藻酸钙凝胶网格的孔隙中而呈石榴状. 以2,2′-联氮双(3-乙基苯并噻唑啉-6-磺酸)(ABTS)为底物, 经酶学性质研究表明, 在无机盐晶体和海藻酸钙凝胶的双重保护下, Alg@Cu3/Zn3(PO4)2@Lac的耐热性、 耐酸性以及储存稳定性比游离漆酶均有不同程度增强. 将Alg@Cu3/Zn3(PO4)2@Lac应用于双酚A(BPA)的降解, 采用孔径约1 mm滤网实现快速回收, 经6次循环利用, 对BPA的降解率下降约14%, 显示出比较稳定的重复利用性和便捷的可操作性, 这主要得益于海藻酸钙和铜/锌无机盐晶体对漆酶蛋白分子的双重保护.  相似文献   
3.
A novel solid-phase microextraction coating of phosphorous-containing titanium oxide composite was developed using titanium fiber as a support and a titanium source by hydrothermal oxidation in a phosphoric acid solution containing hydrogen peroxide. The morphology of the fiber coatings was controlled by the conditions of the hydrothermal oxidation reaction. The oriented nanofiber coating was employed to extract several types of representative aromatic analytes. The experimental results demonstrated that the as-prepared fiber exhibited excellent extraction efficiency toward polycyclic aromatic hydrocarbons. Combined with high-performance liquid chromatography with ultraviolet detection, main extraction conditions were optimized, including pH, ionic strength, extraction temperature, stirring rate, extraction time and desorption time. The established method presented good linearity from 0.05 to 200 μg/L with limit of detection ranging from 0.012 to 0.126 μg/L. This convenient and green procedure was suitable for the selective extraction and determination of typical polycyclic aromatic hydrocarbons in environmental water samples. The relative recoveries of 85.8–112% were obtained for the determination of target polycyclic aromatic hydrocarbons in water samples spiked with 5.0 and 15.0 μg/L. Moreover, the as-prepared fiber showed at least 210 extraction/desorption cycles due to its high mechanical and chemical stability.  相似文献   
4.
Although recent decades have witnessed the synthesis of 1,3,4-thiadiazoles via phosphorus POCl3-promoted cyclization reaction, simultaneous access to 2-amino-1,3,4-thiadiazole and 2-amino-1,3,4-oxadiazole analogs remains unexpected and elusive. Herein, a detailed regiocontrolled synthesis of 2-amino-1,3,4-thiadiazoles in good to high yields with good regioselectivities from readily available thiosemicarbazides using POCl3 was disclosed. Meantime, to establish a comprehensive structure–activity relationship, 2-amino-1,3,4-oxadiazole derivatives as single regioisomers were prepared via EDCI·HCl-triggered cyclization of the thiosemicarbazide intermediates. The in vitro anti-influenza assays proved that the selected compounds with the pyrazine/pyridine ring exhibited certain inhibitory activities against influenza A virus strains A/HK/68 (H3N2) and A/PR/8/34 (H1N1) in MDCK cells. Among them, N-(adamantan-1-yl)-5-(5-(azepan-1-yl)pyrazin-2-yl)-1,3,4-thiadiazol-2-amine (4j) was the most active compound, and exhibited favorable activity with EC50 values of 3.5 μM and 7.5 μM, respectively. In addition, the molecular docking results explained the reason why compound 4j had dual inhibitory activity and revealed the reasonable binding mode of this compound with the M2-S31N and M2-WT ion channels. This compound had the potential to be further developed as an anti-influenza drug.  相似文献   
5.
An ion chromatography system employing a low-cost three-dimensional printed absorbance detector for indirect ultraviolet detection towards portable phosphate analysis of environmental and industrial waters has been developed. The optical detection cell was fabricated using stereolithography three-dimensional printing of nanocomposite material. Chromatographic analysis and detection of phosphate were carried out using a CS5A 4 × 250 mm analytical column with indirect ultraviolet detection using a 255 nm light-emitting diode. Isocratic elution using a 0.6 mM potassium phthalate eluent combined with 1.44 mM sodium bicarbonate was employed at a flow rate of 0.75 mL/min. A linear calibration range of 0.5 to 30 mg/L PO43− applicable to environmental and wastewater analysis was achieved. For retention time and peak area repeatability, relative standard deviation values were 0.68 and 4.09%, respectively. Environmental and wastewater samples were analyzed with the optimized ion chromatography platform and the results were compared to values obtained by an accredited ion chromatograph. For the analysis of environmental samples, relative errors of <14 % were achieved. Recovery analysis was also carried out on both freshwater and wastewater samples and recovery results were within the acceptable range for water analysis using standard ion chromatography methods.  相似文献   
6.
Gaseous CePO2 has been identified by Knudsen effusion mass spectrometry during vaporization of CeO2 and magnesium diphosphate from tungsten double, two‐temperature effusion cell. Structure and molecular parameters of gaseous cerium phosphate under study were determined using quantum chemical calculations. On the basis of equilibrium constants measured for gas‐phase reaction, standard formation enthalpy of CePO2 was determined to be ?508 ± 41 kJ ? mol?1 at the temperature 298 K.  相似文献   
7.
Two organic fluorophores, fluorescein (F) and rhodamine B (Rd), were entrapped in calcium phosphate nanoparticles. The as-obtained nanoparticles can be used for biological release applications. For this aim, calcium phosphate nanoparticles were synthesized using the precipitation method. Structural analysis of these nanoparticles was performed using XRD, FTIR, and Raman spectroscopy, confirming that the synthesized nanoparticles were hydroxyapatite. TEM and SEM analyses demonstrated that these nanoparticles had a size of 20 nm and a well-defined morphology. F and Rd (about 0.5 wt.%) were entrapped in these nanoparticles and their release, as a function of time, was studied via UV-Vis spectroscopy. The obtained results showed that the release of both fluorophores was progressive over time. The trapping efficiencies of the fluorophores were 67.15% and 90.76% for F and Rd, respectively.  相似文献   
8.
The combination of bioactive components such as calcium phosphates and fibrous structures are encouraging niche‐mimetic keys for restoring bone defects. However, the importance of hemocompatibility of the membranes is widely ignored. Heparin‐loaded nanocomposite poly(ε‐caprolactone) (PCL)‐α‐tricalcium phosphate (α‐TCP) fibrous membranes are developed to provide bioactive and hemocompatible constructs for bone tissue engineering. Nanocomposite membranes are optimized based on bioactivity, mechanical properties, and cell interaction. Consequently, various concentrations of heparin molecules are loaded within nanocomposite fibrous membranes. In vitro heparin release profiles reveal a sustained release of heparin over the period of 14 days without an initial burst. Moreover, heparin encapsulation enhances mesenchymal stem cell (MSC) attachment and proliferation, depending on the heparin content. It is concluded that the incorporation of heparin within TCP–PCL fibrous membranes provides the most effective cellular interactions through synergistic physical and chemical cues.  相似文献   
9.
Nickel zirconium phosphate nanoparticles were found to function as efficient catalysts for the selec-tive oxidation of a wide range of alcohols to their corresponding ketones and aldehydes using H2O2 as an oxidizing agent and without any organic solvents, phase transfer catalysts, or additives. The steric and electronic properties of various substrates had significant influence on the reaction con-ditions required to achieve acetylation. The results showed that this method can be applied for the chemoselective oxidation of benzyl alcohols in the presence of aliphatic alcohols. The catalyst used in the current study was characterized by ICP-OES, XRD, NH3-TPD, Py-FTIR, N2 adsorp-tion-desorption, SEM and TEM. These analyses revealed that the interlayer distance in the catalyst increased from 0.75 to 0.98 nm when Ni2+ was intercalated between the layers, whereas the crystal-linity of the material was reduced. The nanocatalyst could also be recovered and reused at least seven times without any discernible decrease in its catalytic activity. This new method for the oxi-dation of alcohols has several key advantages, including mild and environmentally friendly reaction conditions, short reaction time, excellent yields and a facile work-up.  相似文献   
10.
以2,4-二叔丁基苯酚为原料分别合成2,2'-亚甲基双(4,6-二叔丁基苯基)磷酸钠(NA-1)和2,2'-亚甲基双(4-叔丁基苯基)磷酸钠(NA-2),并将其应用于等规聚丙烯(i PP),研究该类芳基杂环磷酸盐成核剂邻位取代基对其成核有效性的影响.通过红外吸收光谱(FTIR)、核磁共振谱(NMR)、X-Ray多晶粉末衍射(XRD)、扫描电镜分析(SEM)和热分析对其化学结构、凝聚态结构、颗粒形貌和物性特征进行了表征,确定了NA-1和NA-2的分子结构和凝聚态颗粒的结构、形貌和物性特征.利用偏光显微观察(POM)、扫描电镜(SEM)断口分析、示差式扫描量热分析(DSC)和雾度测试分析对其与i PP的复合材料的晶粒结构、结晶行为及宏观光学性能进行测试表征.结果表明,添加量0.2%时,邻位叔丁基(NA-1)的存在可使复合材料球晶尺度更加细密,结晶温度比无邻位叔丁基(NA-2)增加5.1 K,等温结晶速率提高至0.56 w/g是NA-2的7倍,半结晶时间由NA-2的11.55 min下降至2.36 min,邻位叔丁基存在对材料透光率和雾度值的影响分别达到4.3%,7.4%.SEM断口分析表明二者在i PP基体中分散均匀,平均粒径相近分别为0.79μm和0.82μm,粒径分布曲线相近,二者分散分布的差异性不显著.  相似文献   
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