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离子对高效液相色谱—TPPS4光度法测定痕量锰锌铜的研究 总被引:3,自引:0,他引:3
本实验用磺化四苯基卟啉作柱前衍生试剂,研究了在Hg(II)催化下,于PH5.5时,TPPS4与Mn(II),Zn(II),Cu(II)的配位反应,提出了以苄基三乙基氯化铵作离子对试剂,反相离子对高效液相色谱-光度法分离和测定痕量Mn(II),Zn(II),Cu(II)的新方法,检测下限(×10^-9g/mL):Mn^2+0.15,Zn^2+0.20,Cu^2+0.11。所确立的方法用于茶汤中锰,锌 相似文献
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本文报道了以2-(6-甲基-2-苯并噻唑偶氮)-5-二乙氨基酚(MBTAE)作柱前衍生化试剂,在SpherisorbC_8柱上,以甲醇:水=80:20(V/V),含2mmol/LLi_2SO_4和10mmol/LpH5.0醋酸盐缓冲溶液作流动相,反相高效液相色谱分离和测定了Fe ̄(2+)、Co ̄(2+)、Ni ̄(2+)和Cu ̄(2+)。各金属离子的检出限(S/N=3)分别为(pg):Fe ̄(2+)6.40,Co ̄(2-)1.38,Ni ̄(2+)4.47,Cu ̄(2+)7.28。方法用于欧洲标准局,黑麦草标样的分析,所得结果与标准值相符。 相似文献
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丙醇—溴化十六烷基三甲胺—硫酸铵—水体系萃取分离汞(Ⅱ) 总被引:1,自引:0,他引:1
研究了丙醇-溴化十六烷基三甲胺9CTMAB)-(NH4)2SO4-水体系萃取分离泵的行为及与常见离子分离条件。试验表明:调节pH1.0或3.0,能使Hg从Fe^3+,Co^2+,Ni^2+m,Zn^2+,Mn^2+,Cu^2+,Al63+等离子混合液中分离出来。 相似文献
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食管癌患者体内环境与正常人的差异,表现在体内自由基反应的相关因子的含量不同,选取有关的生化指标作统计学分析,结果显示:(1)单相关分析有统计学意义的指标是Cu,Cd,Se,Mn-SOD,MDA,GSH-Px,Cu/Zn,Zn/Cd;(2)逐步回归分析,建立回归方程:y=3.9890+2.2399x(Cu)-22.49x(Cu/Zn)-0.0503x(MDA)-0.4335x(Cd)。以此方程作两值 相似文献
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PTFE-乙醚柱反相萃取层析连续分离和测定镓(Ⅲ)铟(Ⅲ)的研究 总被引:4,自引:0,他引:4
研究了在抗坏血酸存在下的6mol/LHBr介质作流动相,以PTFE(聚四氟乙烯)负载的乙醚作固定相,反相萃取层析使微量Ga(Ⅲ)、In(Ⅲ)与Fe3+、Tl3+、Mo6+、Au3+、Ti4+、Bi3+、Al3+、Mg2+、Ca2+、Ni2+、Co2+、Cd2+、Zn2+、Pb2+、Cu2+等多种离子分离。留于柱上的铟、镓分别用HCl(4mol/L)-H2O2(3%)及HBr(1mol/L)洗脱进行连续分离与测定。本方法已应用于地质样品中微量镓、铟的连续分离与测定 相似文献
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硅胶-TBP 反相萃取层析分离法测定金(Ⅲ)与铊(Ⅲ) 的研究 总被引:4,自引:2,他引:2
以王水(体积分数为20%)作移动相,以硅胶球负载的TBP作固定相,反相萃取层析使微量Au(Ⅲ)、Tl(Ⅲ)与Fe3+、Cu2+、Ag+、Zn2+、Mn2+、Hg2+、Cd2+、Pb2+、Sb5+、As5+、Ga3+、In3+、Pt2+、Pd2+等多种离子分离,留于柱上的铊、金分别用NaAc溶液(量浓度为1mol/L)及Na2SO3溶液(质量浓度为10g/L)洗脱进行连续分离与测定(结晶紫光度法测定铊,孔雀绿光度法测定金),回收率可达96%以上,方法已应用于地质样品中金、铊的连续分离与测定。 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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N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%). 相似文献
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Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones. 相似文献
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In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates. 相似文献
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Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described. 相似文献
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用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在. 相似文献
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Jona Mirnik Eva Pušavec Kirar Sebastijan Ričko Uroš Grošelj Amalija Golobič Franc Požgan Bogdan Štefane Jurij Svete 《Tetrahedron》2017,73(24):3329-3337
A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu0 as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than CuI in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT). 相似文献
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George E. Magoulas Thomas Garnelis Constantinos M. Athanassopoulos Dionissios Papaioannou George Mattheolabakis Konstantinos Avgoustakis Dimitra Hadjipavlou-Litina 《Tetrahedron》2012,68(35):7041-7049
(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C60, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine. 相似文献