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用动态光散射法研究了不同浓度NaCl对液—液扩散法生长溶菌酶晶体的影响, 并测量了晶体生长前后体系的Zeta电势.结果表明,NaCl浓度较高时,在溶菌酶溶 液—凝胶界面处会发生液液分层现象,溶液中一直存在较大的聚集体,生长出的晶 体质量较差.而在合适的NaCl浓度下,随着溶液Zeta电势降低,溶液中溶菌酶的大 的聚集体发生解聚集,生长出的晶体质量较高. 相似文献
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采用配液结晶法制取了溶菌酶蛋白质晶体, 使用动态光散射测量了溶液中聚集体的颗粒度几率分布; 使用Zeiss显微镜测定了溶菌酶(110)晶面的生长速度. 实验表明: 随着蛋白质和NaCl浓度的增加, 溶液中聚集体的颗粒尺寸也相应增加. 随着反应时间的增加, 溶菌酶分子在溶液中的聚集反应, 逐渐达到平衡; 在蛋白质和NaCl浓度较高时, 溶菌酶晶体的(110)面生长较快, 而在蛋白质和NaCl浓度较低时, 该晶面生长较慢. 基于二维成核生长机理, 从晶体生长动力学理论方程出发, 计算了二维成核的形成能α=4.01×10-8 J•cm-2. 相似文献
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采用开环聚合的方法 ,合成了组成不同的PLA b PEO b PLA三嵌段共聚物 .滴加选择性溶剂水于共聚物的良溶剂溶液中 ,制备了共聚物以水为介质的“平头”聚集体胶束溶液 .把聚集体胶束溶液浇铸在云母片上 ,采用扫描探针显微镜 (SPM)表征了其形貌和表面微粘弹性 .发现脱离了极性介质水的聚集体的表面性质发生了不均一化 ,聚集体的顶部比相连接的部分具有较高的储能模量 .聚集体环境的改变使聚集体中不同嵌段的迁移导致了这种表面粘弹性的不均一 .另外 ,采用动态光散射的方法测量了体系溶液中聚集体胶束的尺寸 .实验发现光散射所得到的聚集体的尺寸远远大于SPM所得到尺寸 .增加聚合物的起始浓度使聚集体胶束的尺寸以及多分散性都在不同程度上增大 .然而聚合物的不同 ,这种增加的程度会有比较大的差别 相似文献
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从溶液中聚集体的角度研究了溶液的热历史改变生长出的蛋白质晶体的数目和尺寸的内在原因. 将在281 和309 K下保存1 d的两组溶菌酶溶液按不同比例混合, 加入沉淀剂生长晶体. 随着高温溶液的比例增加, 生长出的晶体数目减少, 同时溶液中生长基元的尺寸增大. 在5周内, 采用动态光散射对281, 293和309 K三种温度下保存的溶菌酶溶液中聚集体的变化情况进行监测, 发现溶液中均存在大小不同的两部分聚集体, 称之为小聚集体与多聚体. 前者的尺寸基本不随保存时间而变化, 而后者尺寸随保存时间增加而减小, 减小的速度与保存温度有关. 多聚体的尺寸经过5周后和小聚集体基本相同. 研究结果表明, 处于无序聚集阶段的溶液的均一化程度和成核阶段生长基元的尺寸受到了溶液热历史的影响, 并最终对晶体的数目产生影响. 相似文献
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疏水改性聚丙烯酰胺的增粘机理研究 总被引:21,自引:0,他引:21
通过与聚丙烯酰胺(PAM)对比,使用荧光光谱、紫外光谱、原子力显微镜以及流变性实验对疏水改性聚丙烯酰胺(HMPAM)的溶液行为和微观结构进行了研究.通过荧光实验I3/I1值的变化确定了HMPAM的临界缔合浓度.结合荧光、紫外及流变性实验,对HMPAM在溶液中通过疏水缔合形成疏水微区、超分子聚集体及发展到空间网络的结构变化进行了研究.用原子力显微镜证实了HMPAM溶液中网络结构的存在.对HMPAM表现出的特殊流变性从微观上找到了依据,提出了HMPAM的增粘机理. 相似文献
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脂双层膜表面结构与稳定性的原子力显微镜研究 总被引:5,自引:1,他引:5
用原子力显微镜研究了1,2-二油酸甘油-3-磷酸-1甘油(DOPG)脂双层膜 的表面结构与稳定性。实验结果表明,原子力显微镜的探针与脂双层膜的相互作用 导致脂双层膜表面产生一个永久的损伤。静电相互作用对脂双层膜结构和稳定性的 影响表明,在NaCl溶液中制成的脂质体,随着NaCl浓度的增加,它们的双层膜更稳 定。在低的NaCl浓度则经常被损伤,在1 mol/L NaCl溶液中制备的指双层变得更稳 定。在KCl溶液中结果恰好相反。在高的KCl浓度中经常被损伤,随着KCl浓度的降 低,它们的双层膜更稳定。葡萄糖和蔗糖对脂双层膜结构有稳定作用。 相似文献
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分别采用静态光散射法(SLS)和凝胶渗透色谱法(GPC)测定了木质素基高效减水剂GCL1-JB的分子量(Mw).由于GCL1-JB直接溶于水中存在聚电解质效应和聚集现象,SLS法测得的分子量(Mw,SLS)远大于GPC测得的分子量(Mw,GPC).为了通过SLS测得GCL1-JB的真实Mw,在GCL1-JB溶液中加入NaCl来屏蔽GCL1-JB的聚电解质效应,并采用0.45μm的微孔滤膜滤除GCL1-JB聚集体.GCL1-JB的动态光散射测试中存在2个扩散峰:快模式峰和慢模式峰.快模式峰对应GCL1-JB的单分子行为,而慢模式峰对应GCL1-JB的聚电解质效应和GCL1-JB聚集体.GCL1-JB动态光散射的慢模式峰随着NaCl的不断加入和进一步的过滤处理而逐渐减弱.当NaCl在溶液中的浓度达到0.1 mol/L,动态光散射的慢模式峰完全消失.在没有慢模式峰存在的条件下利用SLS测得GCL1-JB的绝对分子量为121300,这个分子量被认为是GCL1-JB单分子的真实分子量.然而该条件下SLS法测得的Mw,SLS仍然比GPC法测得的Mw,GPC大,这是由于GCL1-JB与GPC标样NaPSS的构象差异引起的.GCL1-JB的分子构象比NaPSS的更卷曲,所以用NaPSS作为GPC标样得到Mw,GPC比GCL1-JB的真实分子量小.本研究提出了一种利用SLS准确测量GCL1-JB的Mw的方法,对存在聚电解质效应和聚集现象的木质素及其衍生产物的绝对分子量测定具有普遍的借鉴意义. 相似文献
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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments. 相似文献
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KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields. 相似文献
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Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields. 相似文献
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
The review contains a concise historical account and information on the most significant researches undertaken by the staff
at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry
of Heterocyclic Compounds.
Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee.
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008. 相似文献
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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
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The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
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A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL. 相似文献
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An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions. 相似文献
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Mohammed KajjoutChristian Rolando 《Tetrahedron》2011,67(25):4731-4741
Quercetin, the polyphenolic compound, which has the highest daily intake, is well known for its protective effects against aging diseases and has received a lot of attention for this reason. Both quercetin 3-O-β-d-glucuronide and quercetin 3′-O-β-d-glucuronide are human metabolites, which, together with their regioisomers, are required for biological as well as physical chemistry studies. We present here a novel synthetic route based on the sequential and selective protections of the hydroxyl functions of quercetin allowing selective glycosylation, followed by TEMPO-mediated oxidation to the glucuronide. This methodology enabled us to synthesize the five O-β-d-glucosides and four O-β-d-glucuronides of quercetin, including the major human metabolite, quercetin 3-O-β-d-glucuronide. 相似文献