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在pH 5.80的六亚甲基四胺-盐酸缓冲溶液中,十二烷基硫酸钠(SDS)和铝(Ⅲ)的存在对依诺沙星荧光强度有协同增敏作用,结合流动注射进样技术,采用时间扫描荧光方式,提出了荧光光度法测定依诺沙星含量的方法。在激发波长267.0 nm,发射波长400.0 nm处,依诺沙星的质量浓度在0.002~0.8 mg.L-1范围内与其荧光强度呈线性关系,方法的检出限(3S/N)为1.7μg.L-1。方法用于片剂、胶囊、注射剂中依诺沙星含量的测定,测得其回收率依次为98.5%,100.5%,98.0%,相对标准偏差(n=5)依次为2.1%,1.3%,1.6%。 相似文献
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一种测定三磷酸腺苷二钠的新荧光光度法 总被引:2,自引:1,他引:1
该文利用荧光光谱和吸收光谱研究了三磷酸腺苷二钠(ATP)与依诺沙星(ENX)和Tb^3+的相互作用。依诺沙星与Tb^3+形成二元络合物发射出位于545nm处的特征荧光,加入三磷酸腺苷二钠(ATP)后,体系的荧光强度显著增强,且增强的荧光强度与ATP的加入量成正比,据此建立了荧光分光光度法测量ATP的方法。实验测得,ATP的线性范围是2.00~20.0μmol·L^-1检出限为6.83×10^-8mol·L^-1。研究了共存物质的影响和Tb^3+ -依诺沙星与三磷酸腺苷二钠的相互作用机理。该法成功地用于样品中ATP的测定。 相似文献
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在碱性介质中,发现依诺沙星对Luminol-H2O2化学发光体系有很强的增敏作用。基于此,提出了一种流动注射化学发光测定依诺沙星的新方法。对检测条件进行了优化。在优化条件下,依诺沙星的线性范围为1.5×10-8~2.0×10-7mol/L,检出限为2.8×10-9mol/L。对1.0×10-7mol/L依诺沙星平行测定11次,其RSD为1.7%。将此方法成功应用于注射用葡萄糖依诺沙星、依诺沙星滴眼液和依诺沙星片3种实际样品中依诺沙星含量的测定。结合化学发光光谱和紫外可见吸收光谱,对该反应机理进行了探讨。 相似文献
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依诺沙星在混合粘合剂碳糊电极上的电化学特性 总被引:3,自引:2,他引:3
制备了混合粘合剂碳糊电极。在0.015mol/L,磷酸-0.10mol/LKCl溶液中,依诺沙星在该电极上于-1.26V处产生一灵敏的阴极溶出伏安峰。在-0.90V富集90s后,依诺沙星的线性范围为3.1×10^-7-1.2×10^-5mol/L,检测下限为9.42×10^-8mol/L,所提出的方法用于尿液和血清中依诺沙星测定,回收率在96%-103%之间。 相似文献
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试验发现依诺沙星对鲁米诺与铁氰化钾之间的化学发光反应具有显著的增敏作用,而且当依诺沙星浓度在2.0×10-8~2.0×10-5mol·L-1范围内,与相应的化学发光增强信号值(△I)之间呈线性关系,其检出限(3S)为5.7×10-9mol·L-1,取1.0 × 10-6mol·L-1依诺沙星按试验方法测定11次,算得其相对标准偏差为1.75%.结合应用流动注射技术,提出了流动注射-化学发光法(FI-CL)测定药片中依诺沙星的方法,应用此方法分析了3个依诺沙星片剂试样,所测得的结果与其标示值相符.按标准加入法作了回收率试验,所得结果在96.7%~103.0%之间. 相似文献
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喹诺酮类药物是一类化学合成抗菌素,在临床上有重要用途。由于其分子结构的特殊性,它们可与许多金属离子发生络合反应,根据其分子吸收或荧光光谱的变化可对药物或金属含量进行测定。依诺沙星(Erloxacin)是临床上广泛应用的第三代喹诺酮类药物,其分子本身具有内源性荧光。本文在实验中发现,在表面活性剂十二烷基硫酸钠(SDS)的存在下,微量铁(Ⅲ)的加入可使依诺沙星的内源性荧光显著猝灭,据此建立了铁(Ⅲ)-依诺沙星-SDS三元体系测定微量铁(Ⅲ)的荧光分析方法。该法灵敏、准确,直接用于水样和食品中微量铁的测定,结果满意。 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