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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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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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空气中肼的流动注射化学发光分析 总被引:6,自引:0,他引:6
研究了肼在碱性条件下与鲁米诺和高磺酸钾产生化学发光行为,建立了流动注射化学发光测定痕量肼的新方法。肼的浓度在1.0×10^-8-1.0×10^-6g/mL范围内与化学光强度成线性关系;检出限为4×10^-9g/mL;相对标准偏差小于3%。 相似文献
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吐温80—AuCl4^—化学发光新体系测定痕量碘离子的研究 总被引:6,自引:0,他引:6
基于碘离子对吐温80-AuCl4^-体系化学发光的强烈抑制作用,提出了一种测定痕量碘离子的新的化学发光分析法。方法的线性范围和检测分别为1.2×10^-8 ̄1.0×10^-6g/mL和5.1×10^-9g/mL碘离子。拟定的方法体系简单,选择性好,加碘酱油和实际水样中碘离子的测定,结果满意。 相似文献
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流动注射化学发光法测定利血平 总被引:9,自引:0,他引:9
研究了利血平在酸性条件下与高锰酸钾和过氧化氢产生化学发光的行为,建立了流动注射化学发光测定利血平的新方法。利血平的浓度在1.0×10^-6 ̄8.0×10^-5h/mL范围内与化学发光强度呈良好的线性关系;检出限为3×10^-7g/mL。对6×10^-6g/mL利血平进行11次平行测定,得方法的相对标准偏差为1.3%。方法用于药剂中利血平含量测定,结果与药典标准方法测得值一致。 相似文献
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流动注射示差动力学化学发光法测定微量硅 总被引:7,自引:0,他引:7
根据硅钼杂多酸氧化Luminol产生化学发光的性质,以及硅钼杂多酸与磷钼杂多酸形成速度的差异,采用停流技术,在硅磷共存时,不经分离,实现了对和钢样中硅的选择性测定。该法检出限为2.0×10^-8g/mL,线性范围1.0×10^-7-1.0×10^-5g/mL,相对标准偏差为2.8%。 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