Syntheses and crystal structures of two isomeric pyrazoles with ferrocenyl groups

Ferrocenoylacetone I reacts with terephthaloyl hydrazide in the presence of a catalytic amount of p-toluenesulfonic acid to afford complex 1 whereas acylation of 3(5)-ferrocenyl-5(3)-methylpyrazole II with terephthaloyl chloride leads to an isomer of complex 1, viz. complex 2. Two new complexes have been characterized by elemental analyses and IR,¹H NMR, UV spectra and structurally characterized by single-crystal X-ray crystallography. Complex 1 (C₃₆H₃₀Fe₂N₄O₂) crystallizes in the monoclinic space group P2₁/c, with lattice constants: a = 11.593(2) ?, b = 12.9962(17) ?, c = 10.0030(17) ?, β = 113.227(4)°, V = 1462.1(4) ?³, Z = 4, D _c = 1.505 g·cm⁻³, F(000) = 684, R ₁ = 0.0307, wR ₂ = 0.0739. Complex 2 (C₃₆H₃₀Fe₂N₄O₂) crystallizes in the monoclinic space group P2₁/n, with lattice constants: a = 12.2388(18) ?, b = 7.3200(15) ?, c = 17.288(4) ?, β = 90.89(3)°, V = 1466.9(5) ?³, Z = 2, D _c = 1.500 g·cm⁻³, F(000) = 684, R ₁ = 0.0410, wR ₂ = 0.1247. Supplementary material Full crystallographic data (CCDC No. 602174 for complex 1 and CCDC No. 602175 for complex 2) have been deposited at the Cambridge Crystallographic Database Centre and are available on request from the Director, CCDC, 12 Union Road, Cambridge, CB2 1EZ, UK (Fax: +44-1223-336-033; Email:deposit@ccdc.cam.ac.uk or http://www.ccdc.cam.ac.uk).     

LaCl3对欧洲李(Prunus domestica) GF43试管苗根系生长及衰老作用的影响

研究了2.5 μmol·L-1 LaCl3在GF43试管苗根系生长及衰老过程中的作用. 结果表明, LaCl3可促进GF43试管苗根系生长及干物质积累, 显著提高超氧化物歧化酶 (SOD)、过氧化氢酶 (CAT)和过氧化物酶(POD)等抗氧化酶活性, 降低超氧阴离子自由基(·O-2)产生速率、丙二醛(MDA)含量和膜透性, 对细胞膜结构具有稳定作用, 从而延缓试管苗根系的衰老进程. 此研究对解决核果类果树工厂化育苗过程中的生根及移栽问题具有一定的参考价值.     

化学分离－质谱法定量分析高纯Dy_2O_3中稀土杂质

以Ｐ_（５０７）萃淋树脂为固定相，ＨＣｌ－ＮＨ４Ｃｌ为淋洗液，研究了９９．９９９％～９９．９９９９％高纯Ｄｙ２Ｏ３中痕量稀土与基体Ｄｙ的分离法，以及火花源质谱法的测定条件。可分析９９．９９９９％超高纯Ｄｙ２Ｏ３中痕量稀土杂质，测定限０．００１～０．１×１０－６，误差３０％。     

Multi-element determination in earthworms with instrumental neutron activation analysis and inductively coupled plasma mass spectrometry: A comparison

Earthworms were collected from agricultural fields in Admont, Graz, Piber and Gumpenstein, Austria. Six earthworm samples were investigated with INAA and with ICP-MS in parallel for the element concentrations of As, Ba, Cd, Co, Cr, Cu, Fe, Hg, Pb, Rb, Sb, Se and Zn. With both techniques 14 elements were analysed in a wide concentration range (ng/g to mg/g) GF-AAS and HG-AAS were used for verification of some element concentrations. A comparison of analytical results between INAA and ICP-MS was discussed. In general, good agreement between ICP-MS and INAA was obtained, the relative difference values of most of the elements are within ±20% range, however, a methodical error for the determination of Hg by ICP-MS was found.     

Formation of complexes of Rubisco-Rubisco activase from La3+, Ce3+ treatment spinach

The complex of Rubisco and Rubisco activase from LaCl₃ ^™, CeCl₃ ^™ treated spinachin vivo is induced. SDS-PAGE result shows that the purified proteins from LaCl₃ ^™, CeCl₃ ^™ treated spinach have not only large and small subunits (55 kD, 14.4 kD) of Rubisco, but also two large subunits of 45 kD and 41 kD near the large subunits of Rubisco. Native-PAGE shows that the purified proteins from LaCl₃ ^™, CeCl₃ ^™ treated spinach have not only a band of Rubisco (560 kD), but also a band of about 1100 kD, about twice distant from Rubisco, which might be a complex of Rubisco and Rubisco activase. The purified enzyme activities from LaCl₃ ^™, CeCl₃ ^™ treated spinach are 1.8 and 2.8 times that of the control, the intensities of absorption and fluorescence are significantly higher than that of the purified Rubisco from the control, and the total sulfhydryl groups and available sulfhydryl groups are 36–39 ™SH per mol enzyme, 14–25 ™SH per mol enzyme more than those of the purified Rubisco from the control, respectively. The CD spectra show that the secondary structure of the purified enzyme from LaCl₃ ^™, CeCl₃ ^™ treated spinach is very different from the control. The enzyme activities from LaCl₃ ^™, CeCl₃ ^™ treated spinachin vivo are 1.5 and 1.9 times those of the control.     

6－甲基－2，5－二酮基－吗啉与己内酯的嵌段共聚物的合成与表征

６－甲基－２，５－二酮基－吗啉与己内酯的嵌段共聚物的合成与表征叶卫平，顾忠伟，杨纪元，徐琳，陈先丽（国家计划生育委员会科学技术研究所，北京，１０００８１）侯明山（燕山石化研究院，北京，１０２５４９）关键词生物降解，６－甲基－２，５－二酮基－吗啉，己内...     

Chitosan-coated hemoglobin microcapsules for use in an electrochemical sensor and as a carrier for oxygen

The article describes the preparation of chitosan-coated hemoglobin (Hb-CS) microcapsules by (a) preparing a CaCO₃ precipitate containing Hb, (b) crosslinking Hb with glutaraldehye, (c) coating the particles with chitosan, and (d) preparing Hb-CS microcapsules by removing the CaCO₃ template with a solution of disodium EDTA. The morphology and electrochemical properties of the Hb-CS microcapsules were investigated by scanning electron microscopy, cyclic voltammetry and electrochemical impedance spectroscopy. An oxygen sensor was obtained by immobilizing the Hb-CS microcapsules on the surface of a glassy carbon electrode (GCE) first modified with gold nanoparticles. The application of Hb-CS microcapsules facilitates electron transfer on the surface of GCE and warrants the integrity and biological activity of Hb. The oxygen sensor, operated best at a working voltage of ?0.335  V (vs. SCE), displays a low limit of detection (30 nM). The Hb-CS microcapsules also are shown to release loaded oxygen to an anaerobic aqueous environment within 300 min.

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Graphical abstract The hemoglobin-chitosan microcapsule shows an excellent ability of electrocatalysis and carrying of oxygen.