流动注射-化学发光法测定盐酸多巴酚丁胺

在磷酸介质中,利用高碘酸钠一过氧化氢-盐酸多巴酚丁胺化学发光体系,结合流动注射技术,建立了一种测定盐酸多巴酚丁胺含量的化学发光新方法。方法的线性范围为2.0×10~(-9)～1.0×10~(-6)g/mL,检出限为2.7×10~(-9)g/mL。测定结果的相对标准偏差为1.6％～2.1％,回收率为93.7％～97.7％。     

纳米金催化鲁米诺化学发光体系测定甲巯咪唑

在碱性介质中,甲巯咪唑能强烈增敏纳米金-鲁米诺-硝酸银化学发光体系产生较强的化学发光信号,据此建立了一种流动注射化学发光测定甲巯咪唑的新方法。在优化实验条件下,该方法对甲巯咪唑的检测线性范围为1.0×10-9~1.0×10-8、1.0×10-8~1.0×10-7、1.0×10-7~1.0×10-6g/mL,检出限(S/N=3)为3.0×10-10g/mL,相对标准偏差为1.2%(n=11,ρ=1.0×10-8g/mL)。将该法用于药物中甲巯咪唑含量的测定,结果满意。同时,采用化学发光光谱表征技术对该体系的化学发光反应机理进行了初步探讨。     

偶合反应化学发光法测定过氧化苯甲酰

基于过氧化苯甲酰可以氧化K4Fe(CN)6生成K3Fe(CN)6,生成的K3Fe(CN)6在碱性溶液氧化鲁米诺可产生强的化学发光的特性,建立了测定过氧化苯甲酰的偶合反应化学发光新方法.该方法测定过氧化苯甲酰的线性范围为1.0×10-8～4.0×10-6 g/mL, 检出限为5×10-9 g/mL,相对标准偏差为3.0% (1.0×10-7 g/mL过氧化苯甲酰溶液,n=11).该方法已用于市售面粉中过氧化苯甲酰的测定.     

纳米银参与的多潘立酮化学发光分析法研究

在碱性介质中,基于多潘立酮对纳米银(AgNPs)增敏Luminol-KMnO4化学发光体系发光信号的抑制作用,结合流动注射技术,提出了测定多潘立酮的化学发光分析新方法。在选定的流路和实验条件下,该方法测定多潘立酮的线性范围为1.0×10-8~5.0×10-6 g/mL,检出限为1.05×10-9 g/mL。对1.0×10-6 g/mL的多潘立酮溶液平行测定11次,其相对标准偏差(RSD)为1.7%。该法灵敏、准确、快速,用于样品中多潘立酮的测定,结果满意。     

流动注射化学发光分析法测定卡马西平

基于酸性条件下溴化钠对NaIO4-H2O2-卡马西平化学发光反应体系具有明显的增敏作用,结合流动注射技术建立了一种测定卡马西平的新方法.在优化的实验条件下,方法的线性范围为1.0×10-9～8.0×10-6g/mL,检出限为3.6×10-10g/mL,相对标准偏差为2.5％(c=2.0×10-7g/mL,n=11),回收率在98.4％～100.6％间.     

流动注射化学发光法测定舒必利

实验发现,在亚硫酸钠存在下,高锰酸钾与舒必利能够发生反应,并产生较强的化学发光。据此采用流动注射技术,建立了利用高锰酸钾-亚硫酸钠-舒必利体系测定舒必利的化学发光分析法。方法线性范围为1.0×10-7~1.0×10-5g/mL;检出限为3.0×10-8g/mL;对1.0×10-6g/mL舒必利测定的相对标准偏差为1.5%(n=11);本法已用于片剂中舒必利含量的测定,结果与药典方法测定值一致。     

NCS-核黄素-盐酸曲普利啶化学发光反应及其分析应用研究

以荧光试剂核黄素为化学发光试剂,构建了N-氯代丁二酰亚胺(NCS)-核黄素-盐酸曲普利啶化学发光新体系。利用此体系建立了测定盐酸曲普利啶的化学发光分析新方法,方法的线性范围为1.0×10-8～9.0×10-7g/mL,检出限为8×10-9g/mL,对浓度为1.0×10-7g/mL盐酸曲普利啶溶液进行11次平行测定的相对...     

流动注射-化学发光法测定富马酸依美斯汀

在酸性条件下,KMnO4与甲醛能够产生微弱的化学发光,而富马酸依美斯汀的存在能够大大增强该化学发光强度;结合流动注射技术,建立了测定富马酸依美斯汀的流动注射-化学发光新方法。该方法的线性范围分别为3.0×10-8～2.0×10-7g/mL,2.0×10-7～1.0×10-6g/mL和1.0×10-6～8.0×10-6g/mL。检出限为1.0×10-8g/mL,对2.0×10-6g/mL富马酸依美斯汀滴眼液平行测定11次,其相对标准偏差为1.3%。该方法已成功应用于滴眼液中富马酸依美斯汀的含量测定。     

K3Fe(CN)6-钙黄绿素体系后化学发光反应测定盐酸氯丙嗪

发现了盐酸氯丙嗪在K3Fe(CN)6-钙黄绿素化学发光反应体系中的后化学发光反应,优化了反应条件,建立了一种利用后化学发光反应测定盐酸氯丙嗪的流动注射化学发光分析法.方法的检出限为3×10-8/mL,相对标准偏差为2.0%(2.0×10-6 g/mL盐酸氯丙嗪,n=11),线性范围为1.0×10-7～1.0×10-5 g/mL.此法已用于盐酸氯丙嗪片剂中盐酸氯丙嗪含量的测定,结果与药典方法测定值一致.     

流动注射-化学发光法测定非洛地平

基于非洛地平在碱性条件下对鲁米诺-K3Fe(CN)6化学发光体系具有很强的增敏作用,结合流动注射技术,建立了直接测定非洛地平的流动注射-化学发光新方法.方法的线性范围为6.0×10(-9)～3.0×10(-6)g/mL,检出限为2.1×10(-9)g/mL,对浓度为1.0×10(-7)g/mL非洛地平平行测定11次,其...     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

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.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

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.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

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%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

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.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

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.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

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.     

正丁胺对激光染料荧光谱影响的研究

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.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

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 Cu^I 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).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(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.