UHPLC-ESI-MS/MS法测定动物源食物提取物中肌肽与鹅肌肽的含量

建立了一种同时测定动物源提取物中肌肽(Carnosine)和鹅肌肽(Anserine)含量的超高效液相色谱-电喷雾串联三重四极杆质谱(UHPLC-ESI-MS/MS)分析方法。采用超高效液相分离系统,借助Inertsil Amide HP色谱柱(2. 1 mm×100 mm,3μm)以0. 1%乙酸水溶液-乙腈为流动相,梯度洗脱分离,利用峰面积外标法定量。经过优化,肌肽和鹅肌肽在1. 95～500μg/L质量浓度范围内与峰面积呈良好的线性关系,相关系数(r)均大于0. 998。肌肽和鹅肌肽的检出限分别为0. 12、0. 47μg/L。以低浓度低聚肽原料为基质,在低、中、高3个加标浓度下,肌肽的回收率为99. 3%～109%,相对标准偏差(RSD,n=6)为0. 98%～1. 1%;鹅肌肽的回收率为100%～113%,RSD为1. 0%～1. 1%。该法前处理简单、快速,重现性好,准确度高,适用于动物源食物提取物中肌肽和鹅肌肽的同时快速检测。     

Electrochemical Synthesis of Imidazo‐Fused N‐Heteroaromatic Compounds through a C−N Bond‐Forming Radical Cascade

We have developed a unified strategy for preparing a variety of imidazo‐fused N‐heteroaromatic compounds through regiospecific electrochemical (3+2) annulation reaction of heteroarylamines with tethered internal alkynes. The electrosynthesis employs a novel tetraarylhydrazine as the catalyst, has a broad substrate scope, and obviates the need for transition‐metal catalysts and oxidizing reagents.     

FeP nanoparticles derived from metal-organic frameworks/GO as high-performance anode material for lithium ion batteries

Double carbon coated Fe P composite(Fe P@NC@r GO)was in situ fabricated via the phosphorization process of the as-prepared Prussian blue@graphene oxide(PB@GO)precursor.The Fe P nanocrystals were successfully embedded in the nitrogen-doped porous carbon matrix.When used as the anode for lithium ion batteries(LIBs),the Fe P@NC@r GO anode shows superior lithium storage properties,delivering a high specific capacity of 830 m A h g~(-1)after 100 cycles at 100 m A g~(-1)and excellent rate capability of 359 m A h g~(-1)at 5 A g~(-1).The outstanding performance mainly ascribes to the synergistic effect of the double carbon coating and porous structure design.The introduction of porous carbon and graphene coating on Fe P nanoparticles greatly enhance the electronic conductivity of the active material and well accommodates the large volume variation of Fe P during the cycling process.     

双(1,4-二酰基氨基硫脲)化合物的合成

酰氨基硫脲及其相关化合物通常具有广泛的生物活性 ,如抗菌[1～ 3] ,抑制神经紧张[4] ,治疗血糖过低[5] ,植物生长调节[6～ 9] 等。迄今为止 ,鲜有关于双 (1 ,4 二酰基氨基硫脲 )合成的报道。为了考查该类化合物的生物活性 ,我们设计合成了一系列双 (1 ,4 二酰基氨基硫脲 )化合物 ,以下图所示的两条合成路线合成了该类化合物 :二酰氯 (1 )、异硫腈酸酰酯 (2 )等中间体可不经进一步纯化直接用于下一步反应。所生成的产物 3ａ 3ｆ、3′ｄ 3′ｇ经ＤＭＦ Ｈ2 Ｏ ＥｔＯＨ重结晶 ,产率达 81 %～ 98%。在合成化合物 (1 )时 ,对于一些用ＳＯＣｌ2 …     

Stability studies on 1:1 or 1:3 stoichiometry complexes of hexaza tripods with zinc(II), copper(II), nickel(II) and cobalt(II)

The coordination properties of two C₃-symmetry hexaza tripods, 1,3,5-tri(2,5-diazahexyl)benzene (L1) and 1,3,5-tri(2,5-diazaheptyl)benzene (L2), towards Zn²⁺, Cu²⁺, Ni²⁺ and Co²⁺ ions, studied by potentiometric techniques, are reported. Both ligands form quite stable complexes either in a 1:1 or 1:3 M:L stoichiometry, presenting a preferential coordination order: Zn²⁺ < Cu²⁺ > Ni²⁺ > Co²⁺. It is observed that the different configurations of metal complexes are achieved due to the fact that tripodal ligands are flexible and not constrained into a rigid geometry.     

AMT在青铜电极表面上吸附的SERS研究

对AMT在青铜上的吸附行为进行激光拉曼电化学研究，通过改变青铜电极的电极电位对在有无Cl－存在条件下各主要拉曼振动峰进行观察.结果表明, AMT垂直吸附在青铜表面，有Cl－存在下， Cl－与AMT分子共吸附在青铜表面上.外加阳极极化电流、加入Cl－将增加AMT在青铜表面上的吸附.     

聚炔烃电子吸收光谱的理论研究

应用DFT/B3LYP方法,在6-31G水平上计算了HC2nH(n=1～13)的基态平衡几何构型和振动频率.在基态平衡构型下,通过TD-B3LYP/cc-PVTZ计算,确定了HC2nH(n=1～5)体系电子跃迁的能量和对应的振子强度.根据计算结果并结合先前的价键研究导出了HC2nH聚炔烃体系电子跃迁能与体系大小n有关的解析表达式.     

{[Zn2(Bim)3(OH)(H2O)]·(DMF)(H2O)3}∞: A Two Dimensional Coordination Polymer with Layer Silicate‐like Structure

A layer silicate‐like zinc(II) benzimidazolate polymer {[Zn₂(Bim)₃(OH)(H₂O)]·(DMF)(H₂O)₃}_∞ ( 1 ) was synthesized at room temperature and characterized with X‐ray single‐crystallography: Monoclinic, space group C2/m (No.12), a = 10.423(3) Å, b = 17.416(6) Å, c = 16.583(5) Å, β = 92.698(4), V = 3006.8(17) ų.     

Syntheses,Crystal Structures,and Cytotoxicity Evaluation of two Chain‐like and Diamond‐like Silver(I) Complexes

Two coordination polymers [Ag(dach)]_n(NO₃)_n ( 1 ) and [Ag(teda)(F₃CSO₃)]_n ( 2 ) (dach = 1, 2‐diaminocyclohexane, teda = 1, 4‐diazabicyclo[2.2.2]octane) have been synthesized and characterized by X‐ray single crystal analysis and cytotoxicity investigation. Compound 1 has a one‐dimensional chain‐like structure which is extended by ligand unsupported Ag···Ag interactions, hydrophobic interaction and hydrogen bonds into a three‐dimensional supramolecular array while compound 2 shows three‐dimensional diamond‐like framework constructed by coordination bonds. The high cytotoxities of these two compounds imply that they are potential candidates for antitumor agents.