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1.
无机偶合流动注射化学发光法测定锑(Ⅲ) 总被引:8,自引:0,他引:8
将锑(Ⅲ)对铬(Ⅵ)氧化I^-产生I2的诱导作用和I2氧化鲁米诺化学发光反应相偶合,建立了一种流动注射化学发光测定痕量锑的新方法。本方法线性范围1×10^-9 ̄1×10^5g/mL;RSD〈4%(n=11,C=7×10^-9g/mL);检出限为1×10^-10g/mL。本法用于矿样中锑的测定,结果令人满意。 相似文献
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高灵敏反应流动注射化学发光法测定抗坏血酸 总被引:5,自引:0,他引:5
基于抗坏血酸对Fe^2+-Luminol-O2体系化学光的抑制效应,利用反应相流注射技术,建立了一个测定抗坏血酸的高灵敏化学发光新方法。该法检出限达2*10^-10g/mL;抗坏血酸浓度在1*10^-9-1*10^-6g/mL范围内与体系化学发光强度减小量呈良好线性相关;相对标准偏差为1.9%。 相似文献
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流动注射化学发光法测定甲氨蝶呤 总被引:8,自引:0,他引:8
研究了甲醛增强高锰酸钾与甲氨蝶呤的化学发光反应,由此建立了一种测定甲氨蝶呤的流动性注射化学发光分析法,方法的检出限为3.4×10^-9g/mL,相对标准偏差为1.1%(2.0×10^-6g/mL甲氨蝶呤,n=11)线性范围为1.0×10^-8~1.0×10^-5g/mL。该法已用于甲氨蝶呤针剂及片剂中甲氨蝶呤含量的测定。 相似文献
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高碘酸钠-过氧化氢-盐酸黄连素化学发光体系的研究 总被引:5,自引:0,他引:5
1引言 盐酸黄连素是一种用于治疗肠道感染,毒性低、副作用小的天然药物。对盐酸黄连素的测定,化学发光法未见报道。本文发现,过氧化氢存在下,磷酸介质中盐酸黄连素与高碘酸钠反应产生强的化学发光。据此结合流动注射技术建立了在NaIO4-H3PO4-H2O2-盐酸黄连素体系中测定盐酸黄连素的化学发光新方法。方法的检出限为 3.8×10-9g/mL。线性范围是 1.0× 10-8- 7.0 ×10-6g/mL。相对标准偏差为 2.3%( C8= 1. 0 ×10-6g/mL; n=11)。该法与药典方法对照,结果满意。… 相似文献
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研究了新吖啶衍生物9,10-二甲基吖啶氟磺酸盐的化学发光特性。建立了测定Co62+的化学发光新体系。方法线性范围为1.0×10^-10-1.0×10^-7g/mL;检测限为5.0×10^-11g/mLCo^2+。测定5.0×10^-9g/mLCo62+的相对标准偏差为6.0%。方法选择性好,用于自来水,江水,池塘水中痕量钴的测定,结果令人满意。 相似文献
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本文采用装有Jones柱的流动注射系统,研究了钒(Ⅱ)-光泽精体系的化学发光反应。在此基础上建立了痕量钒测定的新方法。方法的检出限3×10 ̄(-10)g·mL ̄(-1);对于1.0×10 ̄(-7)g·mL ̄(-1)钒标准溶液测定的相对标准偏差为2%(n=11);线性范围1.0×10 ̄(-9)~9.0×10 ̄(-5)g·mL ̄(-1),相关系数大于0.9980。该方法已用于水样中痕量钒的测定。对于反应机理,本文也进行了探讨。 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