荧光法测定环境水中的痕量砷

建立了测定环境水中痕量砷的荧光新方法,在ＰＨ６．５－７．５的缓冲介质中,利用２′,７′－二氯荧光素（ＤＣＦ）作为荧光试剂,激发波长λｅｘ＝５１０ｎｍ,发射波长λｅｍ＝５２８ｎｍ下,测定痕量砷,亚砷酸根浓度在０．２５－３．５０μｇ／２５ｍＬ范围内,相对荧光强度差值与亚砷酸根浓度呈线性关系,检测限为０．１６μｇ／２５ｍＬ,用于检测自来水和池塘水中的痕量砷,回收率为９５％－１０５％。     

双波长分光光度法同时测定贵金属钯和锇

本文提出了在对羟基苯基荧光酮和溴化十六烷基三甲烷基甲胺存在下，双波长分光光度法同时测定微量和锇的新方法，在ｐＨ＝７．６～８．０的磷酸盐介质中，钯和锇的对羟基苯基荧光酮－ＣＴＭＡＢ配合物吸收光谱相互重叠，选择测定钯配合物的波长对为５８０．５ｎｍ与５３０．５ｎｍ，测定锇配合物的波长对为５５３．５ｎｍ与６０４．５ｎｍ，钯含量在０～７．０μｇ／１０ｍＬ范围内，锇含量在０～９．０μｇ／ｍＬ范围内，与ΔＡ值呈     

荧光光度法快速测定片剂中氨酰心安的含量

研究了氨酰心安的荧光光度法，其最大激发波长和荧光波长分别为２２２．３ｎｍ和２９７．４ｎｍ。该法灵敏度高，操作简便，氨酰心安浓度在０～３．００μｇ／ｍＬ范围内与相对荧光强度呈线性关系，相关系数为０．９９９７，检测限为０．０１６９μｇ／ｍＬ。该法用于测定片剂中氨酰心安含量，结果满意。     

流动注射—胶束荧光法快速测定葡萄糖中的微量铝

本提出Ａｌ－Ｃａｌｃｅｉｎ－ＣＴＭＡＢ－Ｔｗｅｅｎ－８０体系，用流动注射－胶束荧光法快速测定葡萄糖中微量铝的方法。荧光最大激发波长和发射波长分别为４７８．０和５０９．０ｎｍ．Ａｌ＾３＋的浓度在０－６μｇ／ｍＬ范围内标准曲线呈线性关系，方法检出下限为８．４２×１０＾－３μ／ｍＬ。方法已用于测定葡萄糖中微量铝，相对标准偏差为１％左右，回收率为９５－１０１％，进样频率为１４０次／ｈ，进样量为０．４４３     

荧光光度法直接测定环境水中苯酚和十二烷基苯磺酸钠的含量

本文研究了用荧光分光光度法直接测定环境水中苯酚和十二烷基苯磺酸钠（ＳＤＢＳ）二种水中污染物。在ｐＨ〉１１直接测定ＳＤＢＳ含量，波长为λｅｘ／λｅｍ＝２３０／２９５ｎｍ，检出限４．４ｎｇ／ｍＬ，线性范围０￣２．２μｇ／ｍｌ。在ｐＨ＝６，波长为λｅｘ／λｅｍ＝２３０／２９５ｎｍ，测得二者合量，从合量中减去ＳＤＢＳ含量即得苯酚含量，检出限４．０ｎｇ／ｍｌ，线性范围０￣０．８５μｇ／ｍＬ，回收率达９９％￣     

荧光光谱法研究利血平的氧化作用及其分析应用

利血平自身有弱荧光,氧化后可形成较强荧光物质。本文系统地研究了稀ＨＮＯ３对利血平的氧化作用,提出了高灵敏度测定利血平含量的荧光光度分析新方法。结果表明,荧光强度和利血平的浓度在０．０２－０．４μｇ／ｍＬ范围内呈良好的线性关系,方法的检出限为０．００２μｇ／ｍＬ（６．７３＊１０＾－９ｍｏｌ／Ｌ）。该法简便,快速、灵敏度高,用于注射液中利血平含量的测定,结果令人满意。     

流动注射光化学荧光法测定药物制剂中的盐酸氯丙嗪

氯丙嗪的流动注射光化学反应在一编结反应器中进行，该反应器盘绕在一荧光灯上并接受由该灯发生出的最大幅波长为３６５ｎｍ的紫外线照射。用２５３．０ｎｍ的激发波长和３７４．５ｎｍ的荧光波长在线测定光化学反应产物的荧光强度。在最佳条件下，检测限为５．４μｇ／Ｌ，采样速度为９０次／ｈ，１ｍｇ／Ｌ的分析物１１次测定的相对标准偏差为０．５％，动态线性范围为０．０１－６．００ｍｇ／Ｌ。所建立的方法已成功地地用于片剂     

钯（Ⅱ）—二溴羟基苯基荧光酮—溴化十六烷基三甲铵体系分光光度法的…

在ＰＨ６．１－６．７的磷酸盐介质中，钯（Ⅱ）与二溴羟基苯荧光酮溴化十六烷基三甲铵于室温下反应，生成水溶性和稳定性皆佳的紫色三元配合物，最大吸收波长为６００ｎｍ，对比度为７０ｎｍ，表观摩尔吸光系数为９．４８ ×１０＾４Ｌ．ｍｏｌ＾－１ｃｍ＾－１，桑德尔灵敏度为１．１２×１０＾－３μｇ．ｃｍ＾－２，钯含量在０．７．０μｇ／１０ｍＬ范围内服从比尔定律。据此了一个灵敏、简便分光光度法测定钯的瓣方法，用于合     

荧光法测定环境水中微量久效磷

采用荧光分光光度法测定了环境水中微量久效磷的含量。在０．２５％的吲哚丙酮溶液与０．２５％的过硼酸钠溶液的混合液中，体系温度为５℃时，λｅｘ／λｅｍ＝４２０ｎｍ／５００ｎｍ，检测限为４．０μｇ／Ｌ，线性范围为０－３．２μｇ／ｍＬ，回收率为９８％－１０４％，结果令人满意。     

二溴羟基苯基荧光酮荧光猝灭法测定Br~－

本文报道了以二溴羟基苯基荧光酮（ＤＢＨ－ＰＦ）为指示剂，在阳离子表面活性剂ＣＰＣ存在下荧光猝灭间接测定Ｂｒ￣－的新方法。在０．６ｍｏｌ／ＬＨ＿２ＳＯ＿４介质中，Ｂｒ￣－和ＢｒＯ反应生成Ｂｒ＿２，Ｂｒ＿２与ＤＢＨ－ＰＦ（λ＿（ｅｘ）＝４９５ｎｍ，λ＿（ｅｍ）＝５２０ｎｍ）生成红色化合物，使体系荧光猝灭。Ｂｒ￣－含量在０．２５～６．２５μｇ／２５ｍＬ范围内有良好的线性关系，检测限为０．２５μｇ／２５ｍＬ。该法灵敏度高，选择性好，用于合成海水样品中Ｂｒ￣－的测定，结果满意。     

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.