STRUCTURE OF [LA(NO3)(3)(OH2)(2)(OHME)(BIPY)].15-CROWN-5

[La(NO3)(3)(OH2)(2)(OHMe)(bipy).15-crown-5 is monoclinic, P2(1)/n, with a = 11.239(6), b = 19.302(7), c = 14.458(8) Angstrom, beta = 92.47(5)degrees, and D-calc = 1.63 g cm(-3) for Z = 4. In the complex, two nitrogen atoms (from bipy) and nine oxygen atom

4－（2－氨基噻唑）－间苯二酚为柱前衍化剂液相色谱／电化学检测Fe、Co、Ni

４－（２－氨基噻唑）－间苯二酚为柱前衍化剂液相色谱／电化学检测Ｆｅ、Ｃｏ、Ｎｉ格日勒，李惠梅，李南强，汪尔康（中国科学院长春应用化学研究所电分析化学开放实验室，北京大学化学系，长春，１３００２２）关键词液相色谱，Ｆｅ，Ｃｏ，Ｎｉ，４－（２－氨基噻唑）...

Diterpenes, sesquiterpenes, and a C-15-acetogenin from the marine red alga Laurencia mariannensis

In addition to 10 known compounds (7-16), one new brominated diterpene, 10-hydroxykahukuene B (1), two new sesquiterpenes, 9-deoxyelatol (2) and isodactyloxene A (3), one new brominated C-15-acetogenin, laurenmariallene (4), and two new naturally occurring halogenated sesquiterpenes (5 and 6) that were previously obtained as intemediates in a biomimetic synthetic study of rhodolaureol and rhodolauradiol have been isolated and identified from the organic extract of the marine red alga Laurencia mariannensis. The structures of these compounds were established by spectroscopic methods. The antibacterial and antifungal activities of new compounds 1-4 were evaluated.

Laurendecumallenes A-B and laurendecumenynes A-B, halogenated nonterpenoid C-15-Acetogenins from the marine red alga Laurencia decumbens

Four new halogenated nonterpenoid C-15-acetogenins, 4:7,6:13-bisepoxy-9,10-diol-1,12-dibromopentadeca-1,2-diene (1, laurendecumallene A), 4:7,6:12-bisepoxy-9,10-diol-1,13-dibromopentadeca-1,2-diene (2, laurendecumallene 13), (3Z)-6:10,7:13-bisepoxy-12-bromo-9-hydroperoxylpentadeca-3-en-1-yne (3, laurendecumenyne A), and (3Z)-6:10,9:13-bisepoxy-12-bromo-7-chloropentadeca-3-en-1-yne (4, laurendecumenyne 13), together with one known halogenated C-15-acetogenin elatenyne (5) were isolated and identified from the organic extract of the marine red alga Laurencia decumbens. Their structures and relative stereochemistry were established by means of spectroscopic analysis including UV, IR, high-resolution electrospray ionization mass spectrometry (HRESIMS), and ID and 2D NMR techniques. All these metabolites were submitted for the cytotoxic assay against tumor cell line A549 (human lung adenocarcinoma), but all of them were found inactive (IC50 > 10 mu g/mL).

Halogenated Terpenes and a C-15-Acetogenin from the Marine Red Alga Laurencia saitoi

Seven parguerane diterpenes: 15-bromo-2,7,19-triacetoxyparguer-9(11)-en-16-ol (1), 15-bromo-2,7,16,19-tetraacetoxyparguer-9(11)-ene (2), 15-bromo-2,19-diacetoxyparguer-9(11)-en-7,16-diol (3), 15-bromo-2,16,19-triacetoxyparguer-9(11)-en-7-ol (4), 15bromo-2,16-diacetoxyparguer-9(11)-en-7-ol (5), 15-bromoparguer-9(11)-en-16-ol (6), 15-bromoparguer-7-en-16-ol (7), two polyether triterpenes: thyrsiferol (8) and thyrsiferyl 23-acetate (9), and one C15-acetogenin, neolaurallene (10), were isolated from a sample of marine red alga Laurencia saitoi collected off the coast of Yantai. Their structures were established by detailed NMR spectroscopic analysis and comparison with literature data.

冲绳海槽黑潮流域近4万年以来的古海洋环境演化

本文采用取自冲绳海槽的91个站位的表层样品和2个柱状岩芯，通过微体古生物有孔虫分析、氧碳同位素测试、AMS~(14)C测年、沉积物粒度和地球化学分析，探讨了现代生物群落、表层沉积物氧同位素与现代海洋环境之间的关系，进而对冲绳海槽区域近4万年来的古海洋环境和古黑潮演化进行了详细的研究。表层沉积物中的浮游有孔虫氧同位素与现代海洋环境之间的关系密切，浮游有孔虫从G.ruber到G.sacculifer到N.dutertrei其δ~(18)O值由轻变重，表明三种有孔虫其生活水层依次由浅到深。在横穿海槽的剖面上浮游有孔虫δ~(18)O在近陆端因受冲淡小影响较强而变轻，而在东侧站位，受黑潮暖流或其支流的影响氧同位素同样有变轻的趋势。N. dutertrei和G.ruber的氧同位素差值表明了冲绳海槽北部区域黑潮支流对表层水体的影响要大于次表层水体，而在冲绳海槽南部区域，黑潮暖流对次表层水体有相对较强的影响。冲绳海槽南部表层沉积物中的浮游有孔虫整体上属于赤道区组合，溶解作用对该区的浮游有孔虫群落有显的影响，冲绳海槽北部区浮游有孔虫组合对具有温带群落的特征。浮游有孔虫分布与海洋环境密切相关，南北区的浮游有孔虫分布都明显受暖流的影响，在暖流的主流轴处浮游有孔虫丰度通常较高。冲绳海槽具有相对较浅的碳酸盐溶跃面，浮游有孔虫丰度和底栖有孔虫深水胶结壳的含量都进一步表明了该区碳酸钙溶跃面大约在1700 m水深左右，比开放大洋明显要浅得多。表层沉积物中的底栖有孔虫主要受水深和水团等因素的制约。水深制约着有孔虫属种的分带，也影响底栖有孔虫的组合。根据Q型因子分析，冲绳海槽南部表层沉积物中的底栖有孔虫从陆架连缘到海槽底部可以划分为5个特定的组合，分别对应黑潮表层水和次层水影响环境、黑潮中层水影响环境、溶跃面以上的黑潮深层水影响环境、黑潮底层水团影响环境和溶解作用较强的槽底环境；北部区的底栖有孔虫群落反映了四个组合，分别代表了陆架混合水团影响环境、黑潮暖流中层水影响环境、冷涡沉积和上升流区影响环境以及对马暖流水团影响下的环境。以氧同位素曲线为基础，结合AMS~(14)C测年和生物地层学对柱状岩芯进行了地层划分和对比，E107孔记录了冰消期以来大约15,000 a来的古环境演化记录，具有较高的沉积速率，DOC－42孔保存在主要是末冰期中40－10ka BP期间的古环境沉积记录，沉积物记录的分辨率相对较低。浮游有孔虫有碎壳比和底栖有孔虫深海胶结壳含量表明了现代冲绳海槽的浅溶跃面是大约最近2000 a BP才开始突然变浅形成的，碳酸盐的溶解作用从冰消期到现在逐增强。冲绳海槽南部E107孔的底栖有孔虫组合把映了15,000 a来的底层水团具有两种完全不同的营养状况，约6500 a BP以前有机质通量较高，6500 a BP以后有机质通量则明显降低。DOC－42孔的底栖有孔虫组合反映该区约4万年以来的底部水团演化主要受有机质通量和氧含量的共同制约，氧同位素3期主要为高有机质通量的沉积环境，伴随有氧含量水平的较大波动；氧同位素2期有机质通量有所降低，氧含量整体为中等水平；氧同位素1期早期义部水体则较高氧含量为主。浮游有孔虫温跃层转换函数反映了冲绳海槽中部的温跃层在约13100 a BP有一个明显的变化，在这之前产温跃层深度较浅，平均89 m，而在该时间以后，温跃层平均深度变为166 m。此外在160 cm处和100 cm的温跃层深度的两次明显的降低，分别对应于新仙女木事件和黑潮暖流的重新入侵，表明这两个事件导致了海洋上层水体结构的突然变化。冲绳海槽北部浮游有孔虫转换函数古温度和浮游有孔虫的低温、低盐特征种反映了在氧同位素3期早期约40000a BP和氧同位素2期间存在两个明显的低温、低盐阶段，可能与沿岸水在该期间加强有关。其中氧同位素3期早期的表层海水古水温比末次冰期还要低，反映了区域海洋环境的重大变化。冲绳海槽南部E107孔的沉积物粒度、地球化学特征、黑潮特征指示种、表层古水温以及底层水团的性质在6500 a BP左右发生了重大的改变，与冲绳海槽南部的其他岩芯反映的古环境化基本一致，表明了南部海槽在6500 a BP前后古黑潮流径发生了重大变化。而冲绳海槽北部区域2万年以来的古环境则与南部有明显差异，总结前人对冲绳海槽古黑潮流径的研究，笔者对未次冰盛期古黑潮流径提出了新的推测。

Studies on two coordination polymers [M(mu(4)-pz25dc)](n) (M = Cd or Zn, pz25dc=pyrazine-2,5-dicarboxylato) with three-dimensional pillared-layer three-nodal framework: Synthesis, structural characterization, strong optical non-linearities and optical limiting properties

Two isomorphous new candidates [M(mu(4)-pz25dc)](n) (M = Cd, 1; Zn, 2; pz25dc = pyrazine-2,5-dicarboxylato)for nonlinear optical (NLO) materials have been synthesized hydrothermally and characterized crystallographically as pillared-layer three-nodal frameworks with one four-connected metal nodes and two crystallographically different four-connected ligand nodes. Their optical non-linearities are measured by the Z-Scan technique with an 8 ns pulsed laser at 532 nm. These two coordination polymers both exhibit strong NLO absorptive abilities [alpha(2) = (63 +/- 6) x 10 (12) mW (1) 1, ( 46 +/- 6) x 10 (11) mW (1) 2] and effective self-focusing performance [n(2) = (67 +/- 5) x 10 (18) 1, (13 +/- 3) x 10 (18) m(2) W (1) 2] in 1.02 x 10 (4) 1 and 1.05 x 10 (4) mol dm (3) 2 DMF solution separately. The values of the limiting threshold are also measured from the optical limiting experimental data. The heavy atom effect plays important role in the enhancement of optical non-linearities and optical limiting properties. (C) 2009 Elsevier B. V. All rights reserved.

2,3,5-triphenyl-2H-tetrazolium chloride and 2,4,6-tri(2-pyridyl)-s-triazine on the corrosion of mild steel in HCl

Electrochemical measurement, quantum chemical method, and scanning electron microscopy (SEM) were performed to investigate the inhibitive effect of 2,3,5-triphenyl-2H-tetrazolium chloride (TTC) and 2,4,6-tri(2-pyridyl)-s-triazine(TPT) on the corrosion of mild steel in 1mol.L-1 HCl at room temperature. Impedance spectroscopy measurement showed that the polarization resistance increased and that double layer capacitance decreased with the increase in the inhibitive concentration, and the results of potentiodynamic polarization showed that the inhibitors suppressed both cathodic and anodic processes of steel corrosion without change in the mechanism. Higher the orbital density distribution strength of the lowest unoccupied molecular orbital, higher is the molecule dipole, and lower energy gap between the energy of the highest occupied molecular orbital and the energy of the lowest unoccupied molecular orbital resulted in higher inhibitory efficiency. The results of SEM analysis showed that the metal was protected from aggressive corrosion by the addition of TTC and TPT.

青海省道地药材唐古特大黄中4种蒽醌衍生物的含量测定

用高效液相色谱法:甲醇∶0.1%磷酸(85∶15),流速为1.0 mL/min,检测波长为254 nm,柱温为室温,按外标法定量,测定青海省道地药材唐古特大黄中芦荟大黄素、大黄酸、大黄素和大黄素甲醚的含量.结果表明,青海省唐古特大黄中蒽醌衍生物的含量较高,明显高于市售药材,为大黄中的上品.

Large-pore mesoporous SBA-15 silica particles with submicrometer size as stationary phases for high-speed CEC separation

A new mesoporous sphere-like SBA-15 silica was synthesized and evaluated in terms of its suitability as stationary phases for CEC. The unique and attractive properties of the silica particle are its submicrometer particle size of 400 nm and highly ordered cylindrical mesopores with uniform pore size of 12 nm running along the same direction. The bare silica particles with submicrometer size have been successfully employed for the normal-phase electrochromatographic separation of polar compounds with high efficiency (e.g., 210 000 for thiourea), which is matched well with its submicrometer particle size. The Van Deemeter plot showed the hindrance to mass transfer because of the existence of pore structure. The lowest plate height of 2.0 mu m was obtained at the linear velocity of 1.1 mm/s. On the other hand, because of the relatively high linear velocity (e.g., 4.0 mm/s) can be generated, high-speed separation of neutral compounds, anilines, and basic pharmaceuticals in CEC with C-18-modified SBA-15 silica as stationary phases was achieved within 36, 60, and 34 s, respectively.