基于一维锌(Ⅱ)配位聚合物的水中2,4,6-三硝基苯酚和氟啶胺的选择性检测（英文）

以1,1’∶4’,1’’∶4’’,1’’’-四联苯-2,4,2’’’,4’’’-四羧酸(H₄L)和4,4’-联吡啶(4,4’-bpy)为配体,采用水热法合成了一维锌配位聚合物[Zn₂(H₂L)₂(4,4’-bpy)₂(H₂O)]_n(1),并通过单晶X射线衍射分析、元素分析、红外光谱分析和热重分析等方法对其结构进行了表征。单晶结构分析表明1属于三斜晶系,空间群为■。配合物1含有2种配位构型不同的锌离子,分别处于扭曲的三角双锥{ZnNO₄}和八面体{ZnNO₅}几何构型中。配合物中2个H₂L^2-配体之间通过锌离子相互连接,构成了无限的一维zigzag平面结构。荧光传感实验表明配合物1的荧光能够被2,4,6-三硝基苯酚和氟啶胺猝灭,且具有较高的灵敏度和选择性,抗干扰性也非常好。     

含长碳烷基核苷氢亚磷酸酯衍生物的合成与表征

通过将抗病毒药物核苷(3'-叠氮-2',3'-二脱氧胸苷AZT或2',3'-二脱氢-2',3'-二脱氧胸苷d4T)与三氯化磷反应, 然后在不同的醇解试剂作用下, 一锅法合成得到6个含长链烷基的核苷氢亚磷酸二酯衍生物, 并采用³¹P NMR, ¹H NMR, ¹³C NMR和ESI-MS对其结构进行了表征.     

选择性合成手性八氢NOBIN和四氢NOBIN

通过部分氢化手性的(S)-NOBIN [(S)-2-氨基-2’-羟基-1,1’-联萘]选择性地合成了(S)-H8-NOBIN和(S)- -NOBIN. 弱极性溶剂(环己烷)和强极性溶剂(2,2,2-三氟乙醇和含乙酸的乙醇)几乎专一地得到(S)-H8-NOBIN (92%). 而中等极性溶剂(甲醇, 乙醇和异丙醇)以中等产率得到(S)- -NOBIN (66%).     

A Luminescent Tb(Ⅲ)-4,4’,4’’-nitrilotribenzoate Compound with a Three-dimensional Structure

A coordination polymer of [Tb(ntb)]n(1) based on 4,4’,4’’-nitrilotribenzoate ligand(ntb3–) was synthesized. Compound 1 crystallizes in monoclinic system, space group C2/c with a = 13.7318(4), b = 27.5628(9), c = 5.4046(2) ?, β = 111.142(3)°, V = 1907.88(12) ?3, Z = 4, C21H12NO6Tb, Mr = 533.24, Dc = 1.856 g/cm3, μ = 3.745 mm–1, F(000) = 1032, the final R = 0.0184 and wR = 0.0456 for 1883 observed reflections with Ⅰ > 2s(Ⅰ). In compound 1, the eight-coordinated Tb(III) atoms are bridged by carboxylate groups of ntb3– ligands to generate a one-dimensional Tb-carboxylate chain, which is further linked by the ntb3– ligands to form a three-dimensional structure. Compound 1 exhibits characteristic Tb(Ⅲ) luminescent emissions in the solid state.     

3-(3＇-乙酰基-5＇-芳基-1＇,3＇,4＇-二氢噁二唑-2＇-)色酮的微波促进合成

杂环取代色酮;3-(3＇-乙酰基-5＇-芳基-1＇;3＇;4＇-二氢噁二唑-2＇-)色酮的微波促进合成     

Two Cd(Ⅱ)-biphenyl-3,3’-disulfonyl-4,4’-dicarboxylate-2,2’-bipyridine Compounds: Structures and Luminescence

Two coordination polymers based on the mixed ligands of biphenyl-3,3?-disul-fonyl-4,4?-dicarboxylate(BPDSDC4–)and 2,2?-bipyridine(2,2?-bpy),{[Cd(BPDSDC)0.5(2,2?-bpy)(H2O)]·(H2O)}n(1)and{[Cd(BPDSDC)0.5(2,2?-bpy)2]·(H2O)}n(2)were synthesized.Both compounds crystallize in the monoclinic system,space group P21/n.For 1,a=7.5737(2),b=17.4284(5),c=13.5982(5)?,β=90.788(3)°,V=1794.76(10)?^3,Z=4,C17H15N2O7SCd,Mr=503.77,Dc=1.864 g/cm^3,μ=1.378 mm^?1,F(000)=1004,the final R=0.0299 and wR=0.0644 for 3137 observed reflections with I>2s(I).For 2,a=13.3097(2),b=10.66240(10),c=17.6583(3)?,β=91.779(2)°,V=2504.74(6)?^3,Z=4,C27H21N4O6SCd,Mr=641.94,Dc=1.702 g/cm^3,μ=1.008 mm^?1,F(000)=1292,the final R=0.0244 and wR=0.0583 for 4594 observed reflections with I>2s(I).The Cd(II)atoms in both compounds are six-coordinated.In 1,the Cd(2,2?-bpy)units are connected by BPDSDC4–ligands to generate a one-dimensional(1D)ribbon structure.The 1D ribbons are linked by the hydrogen bonds and π···π interactions to give a three-dimensional(3D)structure.In compound 2,the Cd(2,2?-bpy)2 units are linked by the BPDSDC^4–ligands to form a 1D chain.Compounds 1 and 2 show luminescent emissions.     

食品中残留过氧化氢的测定

利用猪血红蛋白(pHb)的催化特性,以3,3’,5,5’-四甲基联苯胺(TMB)为底物,建立了一种催化光度终止法测定食品中残留过氧化氢(H2O2)的方法。实验考察了终止剂的类型和浓度、反应时间、pH、温度、TMB浓度对H2O2检测的影响。在选定的反应条件下,体系吸光值与H2O2浓度在1.46×10-6～2.91×10-5mol/L范围内呈良好的线性关系,线性相关系数为0.9958,方法对H2O2的检出限为5×10-7mol/L,测定标准偏差为4.9%,样品的加标回收率为92.9%～103%,利用该方法进行了实际样品中的H2O2分析,结果与国标法无显著性差异。     

Synthesis and antioxidant activities of flavonoids derivatives, troxerutin and 3’, 4’, 7-triacetoxyethoxyquercetin

Syntheses of two very important derivatives of quercetin,troxerutin and 3’,4’,7-triacetoxyethoxyquercetin were described.The latter was synthesized by highly selective esterification reaction in first time.The compounds were characterized by NMR,IR and Mass spectroscopy.Additionally,the antioxidant activities of the compounds were tested by means of improved pyrogallol autoxidation method.This was the first in using this method to test the antioxidant activities of these two compounds in vitro.The optimum system of pyorgallol autoxidation spectrophotometry was investigated and established according to the reaction rules.The assay indicated that these compounds showed noticeable antioxidant activities,and compound 2 was much more effective as a free radical scavenger than the compound 1 vitamin C was used as a reference material.     

TMB目视比色法检测水中余氯的改进

为解决GB/T 5750.11-2006生活饮用水标准检验方法中的3,3',5,5'-四甲基联苯胺(TMB)目视比色法检测余氯时出现的评价方法准确性欠佳、TMB显色剂发黄、显色体系偏绿等问题,对TMB目视比色法的评价方法、TMB显色剂的配制条件和水样的检测条件进行了研究。结果表明,次氯酸钠不宜作为余氯标准物质来评价TMB目视比色法的改进效果,而通过检测显色体系的A450和目视比色值相结合的方法来判断方法改进效果更为准确。采用优级纯浓盐酸和无氯纯水室温搅拌溶解,可使显色剂无色透明,从而解决TMB显色剂发黄的问题,符合国标要求。将显色剂配制用酸(盐酸)的浓度由国标中0.1mol/L变更为0.6 mol/L,可解决余氯显色体系偏绿的问题。显色体系pH变化后,显色时间、显色温度、显色剂用量可仍按照国标方法的要求进行操作。通过以上改进措施,进一步提高了余氯检测结果的准确度。     

Comparison of the boundary theory with the contact rule of phase regions and Gupta’s method

1Introduction J.W.Gibbs’phase equilibrium theory,especially the phase rule,laid the foundation for the phase theory,but the phase rule cannot solve the problems regarding the relation between neighboring phase regions(ab-breviated to NPRs)and their bound…     

A Novel Energetic Ionic Salt: Hydroxylammonium Potassium 3,3’-Dinitro-5,5’-bis-1,2,4-triazole-1,1’-diolate Dihydrate

A novel energetic ionic salt,hydroxylammonium potassium 3,3?-dinitro-5,5?-bis-1,2,4-triazole-1,1?-diolate dihydrate[(NH3OH)2K(DNOBT)1.5?2H2O],was synthesized and structurally characterized by elemental analysis,IR spectra,13C NMR and single-crystal X-ray diffraction.(NH3OH)2K(DNOBT)1.5?2H2O crystallizes in triclinic system,space group P with a=7.9212(6),b=9.1924(7),c=14.2549(15)?,a=103.917(2)°,β=99.736(2)°,g=104.8110(10)°,V=944.16(14)?^3,Z=2,Dc=1.855 g/cm^3,F(000)=538,μ=0.386 mm^-1,S=1.070,the final R=0.0525 and wR(I>2s(I))=0.1593.Thermal decomposition of(NH3OH)2K(DNOBT)1.5?2H2O and its intermediate potassium 1?-hydroxy-3,3?-dinitro-5,5?-bis-1,2,4-triazole-1-olate monohydrate[K(HDNOBT)?H2O]was studied by using DSC and TG-DTG.It was found that(NH3OH)2K(DNOBT)1.5?2H2O,which has primarily one exothermic decomposition process at 248.2℃,has better thermal stability than K(HDNOBT)?H2O which is decomposed at 210.9℃.     

Evaluation of Transient Absorption Spectra of N,N,N’,N’—Tetra—（p—methylphenyl）

Photoinduced electron transfer processes between fullerenes(C60/C70)and N,N,N’,N’-tetra-(p-methylphenyl-4,4’-diamino-1,1’-diphenyl ether(TPDAE)have been studied by nanosecond laser flash photolysis.Quantum yields and rate constants of electron trasfer from TPDAE to excited triplet state of fullerenes(C60/C70)in benzonitrile have been evaluated by observing the trasient absorption bands in the near-IR region where the excited triplet state.radical anion of fullerenes(C60/C70)and radical cations of TPDAE appear.     

姜瘟病原菌的分离及其抑制物的筛选

从病姜上用梯度稀释法分离出病原菌 ,经鉴定为青枯假单胞菌 (P) (P .solanacearum) ,通过反复筛选 ,得到两种P的抑制物——— 2 ,4 ,4 三氯 2 羟基 联苯醚 (俗称三氯新 )和 2 ,4 ,4 三氯 5 溴 2 羟基 联苯醚 ,其最小抑菌浓度可达 1× 10 7g/ml。通过对其作用时间、杀灭浓度的研究和电镜结果 ,初步探明了该化合物能引起细菌染色质固缩 ,破坏细菌细胞壁 ,使细胞形态发生变化 ,最后崩解死亡。     

新型显色剂3,3,5,5''''-四甲基联苯胺分光光度法测定余氯的研究

本文报道了采用新型氧化还原剂3,3’,5,5’-四甲基联苯胺(TMB)测定水中总余氯的分光光度法,并对其灵敏度、稳定性、准确性作了较为详细的研究,探讨了分析条件,提出了分析方法。在pH≤2时,最大吸收峰为450 nm,表观摩尔吸光系数为6.89×10~4L·mol~(-1)·cm~(-1),可测范围为0.01～2.5 mg/L。与目前使用的传统显色剂邻联甲苯胺(DMB)相比较,具有灵敏度高,显色稳定,重现性好及使用安全等优点。     

沙田柚果肉汁中呋喃香豆素类化合物的液相色谱-质谱联用研究

采用反相高效液相色谱-质谱(HPLC-MS)联用技术分析了沙田柚果肉汁提取液中呋喃香豆素类化合物.沙田柚果肉汁用乙酸乙酯和正己烷的混合液(体积比5:3)萃取,有机层经硅胶柱色谱分离后得若干个组分,用HPLC-MS对各组分进行定性鉴定.结果表明沙田柚果肉汁中含有6',7'-二羟基香柠檬素(6',7'-dihydroxybergamottin,6',7'-DHB)、香柠檬素(bergamottin)、5-甲氧基呋喃香豆素(bergapten)、5-甲氧基-8-异戊烯氧基呋喃香豆素(phellopterin)、6',7'-环氧香柠檬素(6',7'-epoxybergamottin)及二聚体对氧呋喃香豆素-6',7'-二羟基香柠檬素(简称FC574)6种呋喃香豆素类化合物.并经HPLC-MS/MS进一步验证了其化合物结构.     

两个基于2,2’-联吡啶-3,3’-二羧酸的稀土配合物的晶体结构和荧光性质

采用水热法合成了2个具有二维结构的吡啶羧酸类稀土配位聚合物{[Ln₂（bpdc）₃（H₂O）₂]·5H₂O}_n,（Ln=Nd（1）,Eu（2）,2,2’-Bipyridyl-3,3’-dicarboxylicacid）。单晶衍射分析显示1、2结构相似,均属于单斜晶系,P2/c空间群。1、2的晶胞参数分别为a=1.24100（19）nm,b=0.74835（59）nm,c=2.06050（20）nm,β=94.84（1）°;a=1.24100（19）nm,b=0.74301（20）nm,c=2.05250（30）nm,β=94.95（2）°。配合物是由之字形一维链构成的二维网络结构,其拓扑符号为{3^9;4^18;5}。热重测试结果表明1、2热稳定性较好。配合物2显示出很好的荧光性能。     

主客体包结法选择分离白花前胡的化学成分

以1,1,6,6-四苯基-2,4-己二炔-1,6-二醇为主体分子, 可简单、迅速地从白花前胡粗提物中选择分离有效成分3'-乙酰氧基-4'-β-羟基丙酰氧基-3',4'-二氢邪蒿内酯, 收率为0.17%. IR, ¹H NMR, ¹³C NMR光谱和单晶衍射证实了包结化合物的形成及其晶体结构, 并且用气相色谱方法(GC)评价了选择分离效果.     

Synthesis and Crystal Structure of Palladium(Ⅱ) Complex with 2,2’-Bipyridine-3,3’-dicarboxylic Acid

1 INTRODUCTION As the first inorganic antitumor complex[1], cis- platin (cis-DDP) possesses prominent therapeutic ef- fect for encephaloma, lung cancer and several kinds of genital system tumors[2]. However, cis-DDP has toxic side-effect to a larger extent. Especially due to its damage to kidney, the dose is strictly limited[3]. Therefore, other Pt(II) complexes including carbon- platin were developed[4]. Pd(II) complex is struc- turally similar to Pt(II) complex, so the antitumor …     

首次合成来源于鼠李属植物中的两个新颖的蒽环鼠李糖苷，2’, 3’-Di-O-acetylfrangulin A 和 Prinoidin

首次全合成来源于鼠李属植物中的两个天然产物2’, 3’-di-O-acetylfrangulin A (1) 和 prinoidin (2),它们对KB细胞表现出较好的细胞毒活性。通过1H NMR, 13C NMR, 1H-1H COSY, HMQC 和 HMBC确证了两个化合物的结构。     

3",3"-二甲基吡喃[3',4']2,4,2'-三羟基查尔酮的首次全合成

以2,4---羟基苯乙酮和2,4-二羟基苯甲醛为起始原料,经过C-异戊烯基化、保护酚羟基、羟醛缩合、去保护基反应首次成功地完成了天然产物3",3"-二甲基吡喃[3’,4’]2,4,2’-三羟基查尔酮的全合成,总产率18.4％,其结构经1H NMR,IR和MS表征.中间体8未见文献报道.