目的为寻找具有生物活性的fesogenin皂苷,设计并合成了一系列fesogenin的皂苷衍生物。方法采用随机糖苷化策略使fesogenin与单糖供体反应,再脱去单糖上的保护基得到目标化合物。结果与结论所合成的23个fesogenin的皂苷衍生物均为新化合物。

目的建立胸腺五肽分离纯化、分析鉴定方法,有效提高胸腺五肽含量。方法将标准Fmoc方法固相合成的胸腺五肽以Sephadex G225凝胶柱使粗肽脱盐,以循环制备液相色谱仪进行粗肽纯化,以质谱法进行分子质量的鉴定。结果该法得到胸腺五肽的纯度为99102% ,分子质量测定值与理论值相符。结论建立了高效、简便的胸腺五肽分离纯化方法,为工业化生产提供了实验依据。

与常规的液相色谱相比，JAI循环制备液相色谱采用的独特的循环阀控制使整个流路处于闭合状态，使样品多次过柱从而达到很好的分离效果。由于采用了循环系统，我司的循环制制备液相色谱的分离能力更为强大，对于分子体积差异极小的手性物质，通过不断的循环也能达到非常好的分离效果。对于一般的样品，省去了您寻找最佳流动相配比的工作，因为采用循环功能，即使不是最佳的流动相配比，依然能够达到很好的分离效果。 由于JAI循环制备液相色谱具有优异的分离效果，因此不仅仅可以应用在常规的有机合成、天然产物分离纯化、生物化学及无机金属化学领域，对于富勒烯及内嵌金属富勒烯领域，更是有着非常广泛的应用。

与常规的液相色谱相比，JAI循环制备液相色谱采用的独特的循环阀控制使整个流路处于闭合状态，使样品多次过柱从而达到很好的分离效果。由于采用了循环系统，我司的循环制制备液相色谱的分离能力更为强大，对于分子体积差异极小的手性物质，通过不断的循环也能达到非常好的分离效果。对于一般的样品，省去了您寻找最佳流动相配比的工作，因为采用循环功能，即使不是最佳的流动相配比，依然能够达到很好的分离效果。 由于JAI循环制备液相色谱具有优异的分离效果，因此不仅仅可以应用在常规的有机合成、天然产物分离纯化、生物化学及无机金属化学领域，对于富勒烯及内嵌金属富勒烯领域，更是有着非常广泛的应用。

目的　研究分离纯化朝鲜白头翁中三萜皂苷的新方法。方法　利用溶剂提取法、柱色谱法及循环制备HPLC 进行分离纯化。结果　从朝鲜白头翁中分离得到4个化合物, 分别鉴定为: 3-O-α-L-rhamnopyranosyl (1→2)[ β-D-glucopyranosyl (1→4) ] -α-L-arabinopyranosyl hederagenin 28-O-α-L-rhamnopyranosyl (1→4)- β-D-glucopy-ranosyl(1→6)- β-D-glucopyranoside (Ⅰ)、cernuosides A (Ⅱ)、cernuosides B (Ⅲ)、oleanolic acid 28-O-α-L-rhamnopyranosyl (1→4) - β-D-glucopyranosyl (1→6) - β-D-glucopyranoside (Ⅳ)。结论　化合物Ⅳ为首次从该属植物中分离得到, 此外循环制备HPLC可作为天然产物、合成医药研究的有效手段。

Tailoring bicontinuous electron donor (D) and acceptor (A) arrays in solution-processable materials is an essential step for the realization of thin-film organic optoelectronics.1 Casting of a D/A mixture may give rise to photoconductive bulk materials.2 However, without proper choice of the components, many defects are usually formed, leading to trapping and rapid annihilation of charge carriers. In view of photovoltaics, the presence of bicontinuous D and A arrays is essential, but cast films from D/A mixtures likely contain their charge-transfer complexes. So far, nanofibers and tubes with bicontinuous D and A arrays have been obtained by self-assembly of covalently linked D-A dyads.3,4 Nevertheless, solution-processable bulk materials with a D/A heterojunction5 might be more realistic for device applications. Here we report a photoconductive liquid crystal (LC) with bicontinuous arrays of densely packed D and A components, tailored from amphiphilic oligothiophene-C60 dyad 1Amphi (Chart 1).6 Together with contrasting results for a nonamphiphilic reference (1Lipo), we highlight a crucial role of the amphiphilic design both in structuring and in photoconductivity.

Dendrimers are regularly branched three-dimensional macromolecules, whose properties are dependent on the numbers of generation and branch units, along with the structures of building blocks, surface groups, and core modules.1 Site-selective positioning of functional groups in dendritic architectures is expected to induce cooperative phenomena that may lead to a significant enhancement of certain functions. Examples of such cooperative phenomena with dendritic macromolecules have been reported for catalysis, 2 molecular recognition and inclusion,3 and light harvesting.4 We are motivated to explore the potential utility of such a cooperative phenomenon for sensory applications. Here, we report the synthesis of a series of dendritic macromolecules functionalized with multiple zinc porphyrin units (Chart 1) and highlight a clear cooperative effect on chiroptical sensing of an asymmetric ligating molecule.

Abstract: Dendritic molecules appended with multiple zinc porphyrin units (DPm,m [number of zinc porphyrin units] ) 6, 12, and 24) trap bipyridine compounds carrying multiple fullerene units (Py2Fn, n [number of C60 units] ) 1-3), affording coordination complexes DPm_Py2Fn having a photoactive layer consisting of spatially segregated donor and acceptor arrays on their surface. Complexes DPm_Py2Fn are stable enough (K [average binding affinity]) 1.1 _ 106-4.4 _ 106 M-1 in CHCl3 at 25 C) to be isolated by gel permeation chromatography. UHV-STM microscopy enables clear visualization of a petal-like structure of DP12_Py2F3. Photoexcitation of the zinc porphyrin units in DPm_Py2Fn results in a zinc porphyrin-to-fullerene electron transfer to generate a charge separation. The charge-separation rate constant (kCS) in CH2Cl2 at 20 C increases from 0.26 _ 1010 to 2.3 _ 1010 s-1 upon increment ofm and n, whereas the charge-recombination rate constant (kCR) remains almost unchanged at 4.5 _ 106-6.7 _ 106 s-1. Consequently, DP24_Py2F3 furnishes the largest ratio of kCS/kCR (3400) among the family.

Conjugated molecular wires with discrete lengths are important for the exploration of physical properties related to the delocalization of p electrons, and have also attracted attention for their potential application in molecular electronics and photonics. Examples of discrete conjugated wires so far reported include derivatives of polyphenylene, polyacetylene, poly(phenylenevinylene), poly(phenyleneethynylene), polythiophene, and polyporphyrin. However, with the exception of only one example, those oligomers are limited in length to tens of nanometers, because of their low solubility and strong tendency to aggregate. From a photochemical point of view, such a strong tendency to aggregate is a major drawback of “naked” nanowires, which results in collisional deactivation of photoexcited states and hinders their potential utilities. A promising approach to solving this problem is to design “isolated” nanowires bearing “insulating” shells. However, such insulated nanowires with discrete molecular lengths are unprecedented.

We report the synthesis and excellent two-photon-sensitized luminescence properties of a new complex [Eu(tta)3dmbpt] (tta = henoyltrifluoroacetonate; dmbpt = 2-(N,N-diethyl-2,6-dimethylanilin-4-yl)-4,6-bis(3,5-dimethylpyrazol-1-yl)-1,3,5-triazine) that exhibits the highest efficiency of lanthanide luminescence when excited by near-infrared (NIR) laser pulses (action cross section of two-photon-excited fluorescence d ×UF: 85 GM at 812 nm and 56 GM at 842 nm; 1 GM= 10–50 cm4 s photon–1 molecule –1). Compared to a previously reported [Eu(tta)3dpbt] complex, (dpbt = 2-(N,N-diethylanilin-4-yl)-4,6-bis(3,5-dimethylpyrazol- 1-yl)-1,3,5-triazine), [Eu(tta)3dmbpt] has two excess methyl groups at the 2,6-positions of the phenyl ring. Crystallographic data of dmbpt show that the 2,6-dimethyl substitutes bring about a significant twist in the conformation of the diethylamino group compared to that in dpbt, which severely influences the conjugation in the ground state between the electron lone pair of N in the –N(CH2–)2 moiety and the aromatic electron system in dmbpt. The large two-photon absorption (TPA) cross section of dmbpt is mainly derived from its large static dipole moment difference between the S0 and the S1 states, which is partly responsible for the high capability of two-photon-sensitized luminescence of [Eu(tta)3dmbpt]. The broader two- and single-photon excitation windows and the superior two-photon-sensitized luminescent properties in the long-wavelength NIR region of [Eu(tta)3dmbpt] compared to [Eu(tta)3dpbt] are also explained according to the calculated results and twisted structure.

裂解色谱－质谱是一种新的高分子表征手段，可以有效地分离鉴定不同环境下高分子热分解所产生的复杂混合物，为分子水平上研究高分子热分解提供了新的途径。

mini-PAT以Tenax为填充物，并用热箔片将Tenax包裹起来，植入mini-PAT中。实验时，用日本酒滴入mini-PAT管，此后利用便携式居里点裂解仪对GC/MS进行裂解进样。本文为分析方法和测定案例的介绍

橡胶制品的主要性能和其中添加的防老剂有着很大的关系。而由于国内的市场处于比较混乱的状态，因此橡胶企业所购买的防老剂在质量上常常得不到保证。在市场的驱动和利益的诱惑下，企业的采购人员可能购买的是有效成分很低或是假的RD，更有甚者在购买后已经装车的RD同样可能被人掉包。

亚硫酸盐法制浆废液（黑液）中含有大量天然木质素，以该黑液为原料可以合成出一种具有独特性能的多孔磺化木素阳离子交换树脂(LSAR)。本实验对LSAR的裂解机理做了进一步的研究。

以2－（2－吡啶偶氮）－5－二乙氨基苯酚（PADAP）为柱前衍生试剂，在含0.1%酒石酸的10mmol/L（pH3.5）乙酸－乙酸钠缓冲溶液的甲醇－水（50：50，V/V）中（580nm检测），在C18柱上于11min内实现了V、Nb、Ta的同时分离及测定，检测限（S/N=3）为0.34、0.29、7.30ng/mL。该法灵敏度高，用于矿样分析所得结果与推荐值相符，标准加入回收率为99.0%-101.1%。

在金属富勒烯的形成过程中，存在从金属到碳笼的电子转移。La系金属富勒烯中，金属原子转 移2或3个电子给碳笼形成＋2或＋3价的金属离子和带有大量负电荷的碳笼。尽管如此，金属富勒烯仍具有良好的接受电子的能力。大多数的La系金属富勒烯（Y,La,Ce,Pr,Nd,Gd,Tb,Dy,Ho,Er,Lu）的电化学方法研究表明，它们可以接受5到6个电子，但是，Sm的金属富勒烯的氧化还原性质尚未见报道，其主要原因是Sm金属富勒烯的合成产率低，仅是La金属富勒烯的7％，从而使得其分离非常困难，需要通过多步HPLC循环才能得到，高产率地合成与分离是这一金属包合物研究的关键。 本文在高产率合成金属富勒烯的基础上，采用更为有效的方法提取了Sm金属富勒烯，首次利用一步HPLC技术分离出Sm@C82(III)纯品，并对其电化学性质进行了研究。

本文采用HQS作柱前衍生试剂，在ODS柱上，以甲醇－水（38：62，V/V）为流动相（pH 5.6），4.5min内测定痕量Pb。共存离子允许量大，具有很好的选择性，流动相组成简单。当SNR为3时，检出限为1.4ng/ml。方法用于直接测定矿石中痕量钯，结果准确和简便快速。

利用直流电弧法，合成了含钙的富勒烯金属包合物，通过多步高效液相色谱（HPLC）法，首次分离出含钙的富勒烯金属包合物Ca@C_88和Ca@C_90（I,II），用激光解析飞行时间质谱（MAL-DI-TOF-MS）和紫外－可见－近红外（UV-Vis-NIR）光谱进行了表征，并对其分子对称性和电子结构进行了讨论。

本文采用8─羟基喹啉─5─磺酸（HQS）为柱前衍生试剂，用含有10mmol/L的四丁基溴化铵（TBA+Br-）、0.075mmol/L的EDTA和20mmol/L的pH 5.6乙酸－乙酸钠缓冲溶液的甲醇－水（45：55，V/V）溶液为流动相，以C18硅烷化载体为固定相，16min内分离测定Co（Ⅲ）、Fe（Ⅲ）、Al（Ⅲ）和Pd（Ⅱ）的HQS的配合物、信噪比为3时，检出限分别为：Co（Ⅲ）0.9ppb、Fe（Ⅲ）1.5ppb、和Pd（Ⅱ）5.4ppb，方法灵敏度高，干扰少，用于测定试剂级盐酸，硝酸和中国红茶样品中的这些离子，结果良好。

富勒烯综述 在旁人眼里，富勒体的发现历程近乎神奇。本来应由化学家们最早得到的富勒体分子，却由物理学家们在研究星际尘埃工作中意 外的揭开了其神秘的面纱。令C60的发现者们醉心的完美结构竟然是我们再熟悉不过的“足球”！而灵感的源泉却来自于建筑学家的智慧。 这样宇宙与团簇，建筑学家、足球与分子结构这些表面上看起来风牛马不相及的事情，就在这里奇妙的融为了一体。 富勒烯的发现与特征 一、巴基球的发现...... 二、巴基管和巴基葱的发现 ...... 三、富勒烯的结构与特性 ......

RoHS指令、国家质量监督检验检疫总局最近颁布的六个有关RoHS的检测方法标准、ROHS样品制备方案

富勒烯的国内研究进展， 郑兰荪院士发表SCI论文的过程可以说是国内科研学者的一次大联合... 富勒烯的分离方法和分离工具，

在食品和化妆品领域广泛采用天然材料的形势下，强烈要求研究开发以健康和穿着舒适性为主的纤维产品。为此，确立了将天然物质为功能整理剂附着于各种纤维的整理技术，迫切期待研究开发以健康和穿着舒适性为目标的、与人和环境友善的衣料产品。此外，过去对衣料的要求主要是物理性能和装饰性等为主的功能，而现在变为要求穿着舒适性和感性，生态学以及健康功能。 因此，研究了用各种天然整理剂的纤维整理法；通过将有化妆品之类的功能赋予纤维，为确立考虑到人的肌肤与纤维衣料之间关系的整理法以及高功能产品的开发技术进行了研究。为此，对持有护肤功能的衣料产品开发的结果作一报导。

用高分辨及高度灵敏的裂解毛细管气相色谱－硫选择检测器和衍生－毛细管气相色谱联用分析技术，以添加了促进剂CZ,NOBS,NS,DZ的硫化胶为研究对象，进行了硫化胶中次磺酰胺类促进剂母体苯并噻唑及上述促进剂相应的残留胺的测定，然后综合两步的分析结果，准确有效地从硫化胶中鉴定出了上述4种次磺酰胺类促进剂。

脂肪族异氰酸酯是一种重要的化学原料，在制造涂料、弹性体、泡沫塑料、黏合剂等行业中得到了极为重要的应用。脂肪族异氰酸酯可与带有活泼氢的所有化合物反应，如与醇反应生成氨基甲酸酯，制得的各种聚氨酯涂料具有优良的性能。近几年来，脂肪族聚氨酯由于其突出的耐候性和装饰性，正得到越来越广泛的应用。 聚氨酯的定性鉴定一般可通过光谱的方法进行，如IR、NMR，但这些应用常会受到限制，特别是漆膜固化后，而使用裂解－色－质谱技术，则能得到满意的结果。这主要是前者需对固化的漆膜进行前处理后才能进行分析鉴定，而后者则不需要对其进行处理，仅需取微量样品即可进行分析鉴定。本实验采用裂解－色－质谱联接技术，对已知的脂肪族聚氨酯固化漆膜进行分析，对裂解碎片进行检索，并对其裂解机理进行了探索。本文采用的分析方法具有快速准确的特点。

对芸香科黄皮属植物生物碱的研究情况进行了综述。归纳介绍了该属植物生物碱的结构类型、提取分离、结构研究、化学合成方法以及生物活性。

对从重齿毛当归(Angelica pubescens Maxim f. biserrata Shan et Yuan)根及根茎中分得的12种6-或8-脂代-7-氧-香豆素和8种二氢呋喃香豆素衍生物进行了1H和13C NMR分析研究。结合文献，做出规律性总结。运用2D MNR技术，对文献中当归醇类化合物碳谱中的个别错误归属给予了纠正，并首次探讨了此类化合物的MS裂解途径。

在利用电弧放电法合成铽的富勒烯笼内金属包合物时，首次观察到Τb3Ν@C80的存在，并用两步HPLC法将其分离和提。进一步的实验结果表明，氮气的加入是导致Τb3Ν@C80生成的原因。并用MALDI-TOF-MS和UV-Uis-NIR光谱对其进行了表征。

Biomass Integrated This paper describes about a comprehensive economical analysis concerning biomass gasification systems. In Japan,promoting biomass energy systems in domestic area comes to be expected recently. However, there are some problems in achieving this project. The costs for plant building are very expensive comparing with conventional ones. Accordingly, the unit costs of electricity increase up to as high as other environmental energy systems.

The use of pyrolysis-gas chromatography (pyrolysis-GC) for the characterization and analysis of polymers has been used since the development of the technique in 1959. A number of different pyrolyzer designs are currently in general use, each with its own advantages and disadvantages. The major types are resistive filament, Curie point, and furnace pyrolyzers. Pyrolysis-GC, pyrolysis-mass spectrometry (MS), and pyrolysis-GC/MS have been used for decades to elucidate the structures of rubbers. The mechanism for the pyrolysis of polyisoprene has been studied by several groups. The main volatile products formed from polyisoprene by pyrolysis are isoprene and isoprene dimer species. Chien and Kiang11 identified and quantitatively analyzed volatile products obtained from polyisoprene by pyrolysis at 315-384 oC using pyrolysis GC. Matheson and coworkers studied the effect of carbon black filling on the pyrolysis behavior of natural and synthetic rubbers at 850 oC. Ghebrehiwet and coworkers studied analysis of rubber blends using pyrolysis technique coupled with GC/MS at 600 oC. Amounts of volatile products formed from a novolak rein by pyrolysis and their pyrolysis patterns depend on pyrolysis temperatures. Pyrolysis pattern of polyisoprene will also varies depending on the pyrolysis temperature. However, detail studies about this have not been performed. In the present work, the influence of the pyrolysis temperature on the pyrolysis pattern of polyisoprene (the kinds and the relative abundances of the volatile products) was studied using pyrolysis-GC.