锰-二茂铁基配位聚合物微球的制备与表征

采用溶剂热法制得了一系列锰-二茂铁基配位聚合物微球,系统研究了反应时间、反应物浓度等因素对配位聚合物微球的形貌和尺寸的影响规律,采用SEM、TEM、PXRD、EDX和FTIR等方法研究了微球的形貌、尺寸和结构等.发现通过调节反应时间,可使微球的尺寸约在4 ～9 μm范围内变化,提高反应物浓度可使微球从光滑的球形结构向核...     

动物源性食品中地西泮残留量的检测方法研究

采用高效液相色谱法（HPLC）、气相色谱质谱联用法(GC-MS/MS)以及液相色谱质谱联用法(HPLC-MS/MS)测定动物源性食品中镇静剂类药物地西泮的残留量。将样品均质粉碎后,经乙腈提取,固相萃取小柱净化后上机检测,外标法定量。实验证明,当固相萃取的洗脱液中甲醇与乙酸溶液的体积比为70：30时,洗脱效率最高。在不同仪器条件下,地西泮在各自浓度范围内的线性关系良好,相关系数（r²）均大于0.999,回收率在84.6%~ 101.7%,相对标准偏差（RSD）在0.52%~9.44%（n=3）,检出限为0.5 μg·kg^-1（S/N=3,气相色谱质谱联用法以及液相色谱质谱联用法）和10.0 μg·kg^-1（S/N=3,高效液相色谱法）,定量限按照3倍检出限计算; 3种方法均可分析动物源性食品中的地西泮残留量。对比可知,质谱法灵敏度和准确率高,但有一定的基质效应;液相色谱法操作简单,几乎不受基质效应的影响,但灵敏度和准确率不如质谱法。     

Synthesis and Characterization of Copper(II)–Phosphonate Coordination Chain Array of Metallocages

Reaction of CuCl₂ ·2H₂O and 2,4,6‐tris(phosphorylmethyl)mesitylene (H₆tpmm) in H₂O?DMF solution at room temperature afforded green crystals of [Cu₆(H₂tpmm)₃(H₂O)₉]·3H₂O ( 1 ), which were characterized by Fourier transform infrared (FT‐IR), thermogravimetric (TG) analysis, and powder X‐ray diffraction (PXRD). The solid‐state structure of 1 reveals a one‐dimensional chain array of M₄L₂ ‐metallocages constituted by the connection of two kinds of metallocage units, namely MC‐A (phosphonate/water‐bridged) and MC‐B (phosphonate‐bridged only), via μ₂‐O(phosphonate)? Cu bonds in ABAABA order. The tris‐phosphonate ligand H₆tpmm is partially deprotonated to form H₂tpmm^4?, which displays a cis,cis,cis conformation to bridge six Cu(II) centers via two monodentate phosphonate groups in a η ⁰:η ⁰:η ¹‐bonding mode and one tridentate phosphonate group in a μ₄, η ¹:η ¹:η ²‐bondingng mode.     

Eosin Y as a Direct Hydrogen‐Atom Transfer Photocatalyst for the Functionalization of C−H Bonds

Eosin Y, a well‐known economical alternative to metal catalysts in visible‐light‐driven single‐electron transfer‐based organic transformations, can behave as an effective direct hydrogen‐atom transfer catalyst for C?H activation. Using the alkylation of C?H bonds with electron‐deficient alkenes as a model study revealed an extremely broad substrate scope, enabling easy access to a variety of important synthons. This eosin Y‐based photocatalytic hydrogen‐atom transfer strategy is promising for diverse functionalization of a wide range of native C?H bonds in a green and sustainable manner.     

Determination and removal of sulfonamides and quinolones from environmental water samples using magnetic adsorbents

In this study, the magnetic materials known as polymerized ionic liquid@3‐(trimethoxysilyl)propyl methacrylate@Fe₃O₄ nanoparticles were synthesized and utilized as potential adsorbents. First, these nanoparticles were applied to the analysis of sulfonamides and quinolones present in different water samples using magnetic solid phase extraction and high‐performance liquid chromatography. Under optimized conditions, the developed method showed excellent detection sensitivity, with limits of detection (S/N = 3) and quantification limits (S/N = 10) within 0.2–1.0 and 0.8–3.4 μg/L, respectively. The spiked recoveries of the SAs and QNs in environmental water samples ranged from 83.5 to 103.0%, with RSDs of less than 4.5%. In addition, the adsorbents effectively removed sulfamethoxazole and ofloxacin present in existing aquatic environments. The adsorption kinetics and isotherms of sulfamethoxazole and ofloxacin on the magnetic adsorbents were studied to assess removal performance. The results indicate that the adsorption process follows a pseudo‐second‐order mechanism, which reveals that the sorption mechanism is the rate‐limiting step and produces high q_max values (sulfamethoxazole = 70.35 mg/g and ofloxacin = 48.95 mg/g), thus demonstrating the enormous adsorption capacity of these magnetic adsorbents.     

Silver(I) ion induced formation of 2-D ternary lead(II)-silver(I)-4-tolythiolate [PbAg2(μ-Stol)2(μ4-Stol)2]n from 1-D binary lead(II)-4-tolythiolate [(μ-Cl)Pb2(Stol)(μ-Stol)2]n (tol = 4-tolyl)

Treatment of [Pb(Stol)₂]_n with an equiv of [Et₄N]Cl in DMF afforded a new 1-D polymeric complex, [(μ-Cl)Pb₂(Stol)(μ-Stol)₂]_n (1), with Pb–Cl–Pb links. Interaction of 1 with a suspension of [Ag(Stol)] in DMF resulted in formation of a 2-D polymeric complex, [PbAg₂(μ-Stol)₂(μ₄-Stol)₂]_n (2), with the planar four-membered Ag₂S₂ and PbAgS₂ rings bridged by μ-Stol and μ₄-Stol ligands. Both polymeric complexes were structurally characterized by single-crystal X-ray diffraction analysis.     

Dependence of Colloidal Forces Between Bitumen and Silica on the Chain Lengths of Ammonium Surfactants

Effects of ammonium surfactants with different hydrocarbon chain lengths (C8, C12, C16, and C18) on the colloidal forces between bitumen and silica were studied by atomic force microscopy. The results showed that the chain length of the ammonium surfactants had a significant impact on both the long-range interaction and adhesion forces. With the addition of surfactants with relative short chains of C8 and C12 in the solutions, the long-range repulsive force decreased or even became strong attractive force, while it became repulsive again in solutions of surfactants with long chains of C16 and C18. It was further observed that addition of Ca²⁺ in various surfactants solutions would either depress or enhance the colloidal interactions based on the surfactant chain lengths. It was believed that variation of the interaction behaviors resulted from the mono-layer or bilayer adsorption of various surfactant molecules on the negatively charged surfaces of bitumen and silica, which affected the surface wettability and the surface charge characteristics and then greatly changed the colloidal interactions. The findings indicated that, to have a high bitumen recovery and good froth quality, the surfactant type and concentration of the di-valent metal ions in the oil sand processing slurry must be well considered.     

TiO_2/EDTA-rich carbon composites:Synthesis,characterization and visible-light-driven photocatalytic reduction of Cr(Ⅵ)

Ti02/EDTA-rich carbon composites(TiO_2/EDTA-RC) have been successfully synthesized via a low temperature carbonization process. TiO_2/EDTA-RC exhibits marked absorption of visible light and excellent photoreduction of Cr(Ⅵ) activity under visible light irradiation(λ420 nm). Due to the high carboxyl group content and strong coordination ability of EDTA, TiO_2-EDTA complex can be easily fabricated between EDTA incorporated in carbon sheet and titanol group on the surface of TiO_2. TiO_2-EDTA complexes on the surface of TiO_2/EDTA-RC, the LMCT complex, are responsible for the prominent photoreduction of Cr(Ⅵ) properties of Ti02/EDTA-RC under visible light irradiation. In addition, the unique structure ofTiO_2/EDTA-RC is also propitious to the visible-light photocatalytic reduction of Cr(Ⅵ).Carbon sheet of TiO_2/EDTA-RC acts as a supporter. TiO_2 nanoparticles and EDTA homogeneously disperse into the carbon sheet supporter and form the TiO_2-EDTA complexes, which can avoid the aggregation of TiO_2 nanoparticles in the aqueous solution and provide more photocatalytic reaction points for the reduction of Cr(Ⅵ).     

Mechanistic and kinetic investigations of N2H4 + OH reaction

The reaction of N₂H₄ with OH has been investigated by quantum chemical methods. The results show that hydrogen abstraction mechanism is more feasible than substitution mechanism thermodynamically. The calculated rate constants agree with the available experimental data. The calculated results show that the variational effect is small at lower temperature region, while it becomes significant at higher temperature region. On the other hand, the small‐curvature tunneling effect may play an important role in the temperature range 220?3000 K. Moreover, the calculated rate constants show negative temperature dependence at the temperatures below 500 K, which is in accordance with Vaghjiani's report that slightly negative temperature dependence is found over the temperature range of 258?637 K. The mechanism of the major product (N₂H₃) with OH has also been investigated theoretically to understand the title reaction thoroughly. © 2009 Wiley Periodicals, Inc. J Comput Chem, 2010     

Two new coumarin biosides from Angelica dahurica

Two new coumarin biosides, tert-O-β-D-apiofuranosyl-(1→6)-O-β-D-glucopyranosyl-byakangelicin (1) and 2′-O-β-D-apiofuranosyl-(1→6)-β-D-glucopyranosyl-peucedanol (2), were isolated from the fresh roots of Angelica dahurica. The structures of the new compounds were elucidated on the basis of spectral analysis. Published in Khimiya Prirodnykh Soedinenii, No. 6, pp. 561–563, November–December, 2008.