山芝麻中的新三萜化合物

山芝麻 (Helicteresangustifolia L inn.)是梧桐科 (Sterculiaceae)山芝麻属植物 ,主要分布在广东、广西、云南及长江以南各省 ,用以治疗感冒发热、麻疹、疟疾和疔疮等症 [1] .王明时等 [2 ,3]曾从该植物中分离出 3个三萜类化合物和 1个萘醌化合物 .为进一步寻找有效成分 ,我们从山芝麻中又分离到 2个新的三萜化合物 1和 2 ,用波谱方法测定了其化学结构 .1　实验部分1 .1　仪器与材料　北京泰克仪器公司的双目镜 X-6型显微熔点仪 ;EQUINOX-55(Bruker)红外光谱仪 ;Varian Unity INOVA 50 0型核磁共振仪 (TMS为内标 ) ;VG Autospec-…     

苦豆籽中总生物碱的含量测定

苦豆籽系槐科植物苦豆子 (Ｓｏｐｈｒａａｌｏｐｅｃａｒｏｉｄｅｓ)的成熟种子。从苦豆籽中分离得到了 2 0余种生物碱[1 ] ,具有广泛的生理活性 ,药用价值很高。苦豆子总生物碱的含量测定有重量法[2 ] ,酸碱滴定法[3] ,因苦豆子生物碱结构多属于喹啉联啶类衍生物 ,可在ｐＨ7.6缓冲液中与溴麝香草酚蓝形成离子对 ,经氯仿提取后于 42 0ｎｍ进行比色测定。我们采用这种酸性染料分光光度法[4] 进行了苦豆籽胶囊中总生物碱的含量测定 ,为其质量标准的测定提供了依据。1　实验部分1 .1　仪器 ,药品72 1型分光光度计、ＰＨ 2Ｓ型酸度计 ,槐果碱(Ｃ…     

[Ni(dmit)(dmise)]~(n-)混合配体配合物的合成与导电性质

合成了 [Ni( dmit) ( dmise) ]n-( n=2 ,1 ,0 )型混合配体配合物 ,用电结晶法制得 [BEDT-TTF]-[Ni( dmit) ( dmise) ]电荷转移盐 ,并用 EA、IR、ESR对目标产物进行了表征 .2 5℃测得化合物 [Ni( dmit) -( dmise) ]和 [BEDT-TTF][Ni( dmit) ( dmise) ]的电导率分别为 0 .2 9和 5.6× 1 0 -3 Ω-1· cm-1.2 98～ 1 0 3 K温度范围内变温电导曲线显示 :化合物 [Ni( dmit) ( dmise) ]具有典型的半导体性质 .     

稀土钬及铒钇丙氨酸配合物的量热与热分析研究

合成了两种固态稀土丙氨酸配合物[Ho2(Ala)4(H2O)8]Cl6和[ErY(Ala)4(H2O)8](ClO4)6 (Ala为丙氨酸),用量热和热分析方法研究了这两种配合物的热力学性质.用全自动高精密绝热量热计测定了在78～377 K温区内的低温热容.对于[Ho2(Ala)4(H2O)8]Cl6,在214～255 K温区内发现一固-固相变,其相变温度为235.09 K.对于[ErY(Ala)4(H2O)8](ClO4)6,在99～121 K温区内也发现一固-固相变,其相变温度为115.78 K. [Ho2(Ala)4(H2O)8]Cl6固-固相变焓为3.02 kJ• mol－1,相变熵为12.83 J•K－1•mol－1； [ErY(Ala)4(H2O)8](ClO4)6 固-固相变焓为1.96 kJ•mol－1,相变熵为16.90 J•K－1•mol－1.同时,用TG技术在40～800 ℃温区研究了两配合物的热稳定性.由TG/DTG曲线分析可知, [Ho2(Ala)4(H2O)8]Cl6从80 ℃到479 ℃热分解分两步完成, [ErY(Ala)4(H2O)8](ClO4)6从120 ℃到430 ℃热分解分三步完成.     

2，4，6-三硝基间苯二酚钡一水化合物的热分解动力学(英)

0IntroductionBarium2,4,6鄄trinitroresorecinatemonohydrate,Ba(TNR)·H2O,hasgooddetonatingpropertiesandissensitivetoflame.Itcanbeusedasinitiatingagent,igniterpowderordelaypowder.Itspreparation[1],pro鄄perties[1],crystalstructure[1]andthermalbehavior[2]haveb…     

BF3活化高锰酸氧化丙烯酸反应机理的 密度泛函研究

用量子化学密度泛函理论(DFT)的B3LYP方法对高锰酸根离子与丙烯酸的环加成反应机理进行了系统研究, 全参数优化了反应势能面上各驻点的几何构型、振动频率和能量. 计算结果表明: 反应有两个竞争通道, 即[2+3]反应通道和[2+2]反应通道, 其中[2+3]通道比[2+2]通道的反应势垒降低了183.89 kJ/mol, 并通过在高锰酸根的氧原子上配位一个或两个BF3分子来研究BF3分子对反应体系的活化效应, 结合两个BF3分子使得[2+3]通道的反应势垒降低为23.97 kJ/mol, 则有利于反应按该通道进行, 然而[2+2]通道的反应势垒仍较高(>195 kJ/mol).这进一步表明该反应体系中加入一定量BF3能提高高锰酸氧化烯烃双键的化学活性.     

反相微乳液介质中Nd2(CO3)3·8H2 O的可控合成

以十六烷基三甲基溴化铵(CTAB)/正丁醇/正辛烷/硝酸钕[Nd(NO3)3]溶液(碳酸钠溶液)所组成的反相微乳液为反应介质, 采用微乳液溶剂热法合成了Nd2(CO3)3·8H2O, 并考察了水/核比([H2O]/[CTAB])和Nd(NO3)3的浓度对其形貌和尺寸的影响. 利用X射线衍射(XRD)、 热分析(DSC-TGA)、 扫描电子显微镜(SEM)和透射电子显微镜(TEM)等对Nd2(CO3)3·8H2O的晶型、 形貌及尺寸进行了表征, 并提出了不同形貌Nd2(CO3)3·8H2O形成的可能机理. 结果表明, 随着水/核比的增大, Nd2(CO3)3·8H2O的形貌从多面体变成鱼尾状, 再变成针状; 随着Nd(NO3)3浓度的增大, 针状Nd2(CO3)3·8H2O的尺寸逐渐减小.     

朝鲜淫羊藿中生物碱类新成分的分离提取及结构鉴定

淫羊藿系小檗科淫羊藿属植物 ,具有补肾壮阳、强筋骨、祛风湿之功效 .现代药理研究表明 ,它还具有防治骨质疏松和提高免疫功能等作用 .2 0 0 0年版中国药典收载了 5种淫羊藿属植物 ,朝鲜淫羊藿为其中一种 ,是长白山道地中药材之一 .朝鲜淫羊藿中化学成分的研究多集中在黄酮类化合物方面 [1～ 6 ] ,而对其生物碱类化合物的研究较少 [7,8] .本文对朝鲜淫羊藿中生物碱类化合物进行了研究 ,并发现了一种新的生物碱 (6-羟基 -1 1 ,1 2 -二甲氧基 -2 ,2 -二甲基 -1 ,8-二氧 -1 ,3 ,4,8-四氢 -2 H -7-氧杂 -2 -氮 -苯并 [c]菲 ) ,采用核磁共振波…     

二维网状冠醚配合物——苯并15-冠-5、二苯并18-冠-6与Na_2[Pt(SCN)_6]配合物的合成与结构

合成了苯并 15 冠 5、二苯并 18 冠 6与Na2 [Pt(SCN) 6]的配合物 :[Na(B15 C 5 ) ]2 [Pt(SCN) 6](1) ,[Na(DB18 C 6 ) ]2 [Pt(SCN) 6](2 ) ,并通过元素分析、红外光谱、单晶X射线衍射进行了表征 .1为单斜晶系 ,空间群P2 1/c,a =1.0 974(5 )nm ,b =1.5 187(7)nm ,c=1.36 32 (6 )nm ,β =96 .40 7(7)°,V =2 .2 5 6 8(18)nm3 ,Z =2 ,Dcalcd=1.746g/cm3 ,F(0 0 0 ) =1184,R1=0 .0 35 7,wR2 =0 .0 86 8.2为三斜晶系 ,空间群P1- ,a =1.2 5 0 0 (3)nm ,b =1.2 82 5 (3)nm ,c=1.934 2 (4 )nm ,α=10 6 .82 (3)° ,β =10 2 .5 1(3)° ,γ =10 3.0 4(3)°,V =2 .75 6 2nm3 ,Z =2 ,Dcalcd=1.5 79g/cm3 ,F(0 0 0 ) =1316 ,R1=0 .0 36 4,wR2 =0 .0 771.配合物分别由两个 [Na(B15 C 5 ) ]+ ,[Na(DB18 C 6 ) ]+ 配阳离子和一个[Pt(SCN) 6]2 -配阴离子组成 .配阳离子和配阴离子通过Na—N键形成二维网状结构     

在平面构型[PdnClm]2-阴离子驱动下三种瓜环基超分子框架化合物的构筑

采用无机阴离子诱导方法,以具有平面构型的[Pd_nCl_m]~(2-)阴离子为结构导向试剂,成功制备了3种具有框架结构特征的瓜环基超分子化合物:{Na_2(H_2O)_6TMeQ[6]}[Pd_2Cl_6]·3H_2O (1)、(H_3O)_2{CyH_5Q[5]}[Pd_2Cl_6]·3H_2O (2)及(H_3O)_2{Q[5]}[PdCl_4]·23H_2O (3)。X射线单晶衍射的结果表明:在1中,Na+离子与TMeQ[6]端口羰基氧直接配位形成一维结构的超分子链,在[Pd_2Cl_6]~(2-)阴离子与TMeQ[6]的外壁作用下,进一步构筑形成三维的框架结构;在2中,在[Pd_2Cl_6]~(2-)阴离子与CyH_5Q[5]的外壁作用下,CyH_5Q[5]以一维链有序排列,且4条CyH_5Q[5]分子链可堆砌成一孔道,孔道中填充了[Pd_2Cl_6]~(2-)阴离子,最终形成三维框架结构;在3中,8个[PdCl_4]~(2-)阴离子与4个Q[5]分子通过瓜环外壁相互作用,形成二维层状框架结构,层与层之间再通过非共价键作用力,最终形成三维层状框架结构。在这3种瓜环基超分子框架化合物中,[Pd_nCl_m]~(2-)阴离子促进了瓜环分子有序化排列,形成了具有框架结构特征的自组装体。这种主要驱动力来源于瓜环的外壁作用,即瓜环"正电性外壁"与[Pd_nCl_m]~(2-)阴离子间的离子偶极作用。     

Erythrinarbine,a Novel nor-A ring Erythrina Alkaloid from Erythrina arborescens

ErythrinaarborescensRoxb.belongstoErythrinagenusofPapilionaceaefamilyplants,andiswidelydistributedintropicalandsubtropicalregionsoftheworld,aswellasinthesouthandsouth-westofChina'.AsaChinesefolkmedicine,itsrootandstemareusedtotreatrheumatismanddysentery'.TheErythrinaalkaloids,normallyaC.,tetracyclicspiroaminesystem,erythrinanel,arethecharacteristicconstituentsinErylhrinagenusandabout100erythrinaalkaloidshavebeensofarreportedfromthisgenusplants'-'.MostoftheseErythrinaalkaloidshaveatetrahydr…     

Geissospermiculatine,a New Alkaloid from Geissospermum reticulatum Bark

A new alkaloid, geissospermiculatine was characterized in Geissospermum reticulatum A. H. Gentry bark (Apocynaceae). Here, following a simplified isolation protocol, the structure of the alkaloid was elucidated through GC-MS, LC-MS/MS, 1D, and 2D NMR (COSY, ROESY, HSQC, HMBC, ¹H-¹⁵N HMBC). Cytotoxic properties were evaluated in vitro on malignant THP-1 cells, and the results demonstrated that the cytotoxicity of the alkaloid (30  μg/mL) was comparable with staurosporine (10  μM). Additionally, the toxicity was tested on zebrafish (Danio rerio) embryos in vivo by monitoring their development (0–72 h); toxicity was not evident at 30  μg/mL.     

A new alkaloid from the marine-derived fungus Hypocrea virens

A new alkaloid, 2-methylimidazo[1,5-b]isoquinoline-1,3,5(2H)-trione, was isolated from the EtOAc extract of the marine-derived fungus Hypocrea virens. Its structure was confirmed by spectroscopic methods (1D and 2D NMR, MS).     

Cimicifine A: A Novel Triterpene Alkaloid from the Rhizomes of Cimicifuga foetida

Cimicifine A ( 1 ), the first cycloartane triterpene alkaloid, was isolated from the rhizomes of Cimicifuga foetida, together with the known compound cimicifugoside H‐1 ( 2 ). Their chemical structures were established by extensive NMR and MS analyses and by comparison with literature.     

Sesquiterpenoid alkaloid from Acroptilon repens

One new sesquiterpenoid alkaloid, namely 3 beta,8 alpha-dihydroxy-13-pyrrolidine-4(15),10(14)-(1 alpha H,5 alpha H,6 beta H,11 beta H)-guaiadien-12,6-olide (1), together with two known guaiane-type sesquiternoids (2-3) was isolated from the aerial part of Acroptilon repens. The structure of 1 was established by spectroscopic methods, especially 2D NMR (HMQC, HMBC, and NOESY). Cytotoxic activity against tumor cell line was assessed for compounds 2-3, and found to show potent cytotoxic activities against tumor cell line P-388.     

A 300 MHz NMR. Evidence for the Configuration of Roxburghine B

The 300 MHz ¹H-NMR. spectrum of the alkaloid Roxburghine B is completely analysed. The coupling constant values give evidence for the configuration, which is revised to epi-allo: H(3β), H(15α), H(20α) and C(18β).     

远程二维NMR用于马尾杉碱M的结构测定

马尾杉碱是一种从华南马尾杉(新品科植物)中分得的新的生物碱。其分子式为C17H20N2O3, 通过紫外, 红外, ^1H和^1^3C NMR谱图分析发现其结构与最近文献报导的福定碱或石杉碱相类似, 本文还采用普通和远程的^1^3C-^1H COSY二维NMR新技术进行了研究, 所得结果与上述分析相符。     

1H and 13C NMR spectra of 3,8-dimethoxyfuro[3,2-g]coumarin and maculine from Esenbeckia grandiflora Martius (Rutaceae)

One- and two-dimensional NMR experiments were used for the unambiguous assignment of the (1)H and (13)C NMR chemical shifts of the furoquinoline alkaloid maculine (1) and the new furanocoumarin 3,8-dimethoxyfuro[3,2-g]coumarin (2).     

Diterpenoid Alkaloids of Delphinium buschianum Grossh.

From the aerial parts of Delphinium buschianum Grossh ., collected in Turkey, a new diterpenoid alkaloid 1 , named budelphine, was isolated along with the known diterpenoid alkaloids karakoline ( 2 ), 18‐hydroxy‐14‐O‐methylgadesine ( 3 ), delsoline ( 4 ), lapaconidine ( 5 ), columbianine ( 6 ), 14‐benzoylneoline ( 7 ), and hetisine ( 9 ). The structure of 1 was established on the basis of ¹H‐, ¹³C‐, DEPT, ¹H,¹H‐COSY, NOESY, HSQC, and HMBC NMR studies.     

In vitro anti-inflammatory activities of naucleoffieine H as a natural alkaloid from Nauclea officinalis Pierrc ex Pitard,through inhibition of the iNOS pathway in LPS-activated RAW 264.7 macrophages

Abstract

Naucleoffieine H, a natural indole alkaloid, was isolated and identified from Nauclea officinalis Pierrc ex Pitard which is a traditional Chinese medicine used for the treatment of various diseases, such as cold, fever, bronchitis, pneumonia, acute tonsillitis, etc. In the present study, the effect of naucleoffieine H on the anti-inflammatory activities was investigated in LPS-induced RAW 264.7 macrophages. The results showed that naucleoffieine H significantly inhibited the release of nitric oxide (the level of nitrite as a stable biomarker of NO production) and tumor necrosis factor-α (TNF-α). Interesting, naucleoffieine H down-regulated the overexpression of inflammatory protein induced nitric oxide synthase (iNOS), but no effect on the expression cyclooxygenase-2 (COX-2) protein. In addition, this bioactive alkaloid suppressed enzymatic activity of iNOS activated by LPS. The above results indicated that naucleoffieine H suppress NO and TNF-α overproduction via block the iNOS pathway in LPS-induced RAW 264.7 macrophages.