K系数－多波长最小—乘回归分光光度法同时测定三组分的研究

将双波长Ｋ系数分光光度法和多波长线性回归分光光度法相结合，并采用最小一乘法准则计算回归系数，提出了一种同时测定三组分的新方法，即Ｋ系数－多波长最小一乘回归分光光度法。该法不需要吸收曲线交点和等吸收点，且能较好地克服异常点的影响，得到比最小二乘法更好的回归稳健性。方法用于测定模拟混合色素样品和饮料样品中的柠檬黄、胭脂红、果绿，相对误差为—３．６％～２．８％，回收率为９６．３％～１０４．８％，变异系数小于２．７９％。     

多波长线性回归——阶导数分光光度法同时测定水中 NO_3~-和 NO_2~-

NO_3~-和 NO_2~-是水质监测的重要指标,测定方法已有报道,但多数采用常规分光光度法,操作较为麻烦,灵敏度不高。本文提出了多波长线性回归一阶导数分光光度法同时测定两个组分的原理,并应用于水中 NO_3~-和 NO_2~-的同时测定。样品分析结果表明,精密度和准确度良好,并且,本法的吸光系数较常规多波长线性回归法的吸光系数提高10倍,最低检测限(本法是0.004μg/ml)较常规多波长线性回归法的最低检测限降低了10倍。该法具有简单、灵敏、准确的优点。     

K系数—多波长最小一乘回归分光光度法同时测定三组分的研究

将双波长Ｋ系分光光度法和多波长线性回归分光光度法相结合，并采用最小一乘法准则计算回归系数，提出了一种同时测定三组分的新方法，即Ｋ系数－多波长最小一乘回归分光光度法。     

多波长线性回归紫外吸光光度法同时测定炼油厂污水苯？…

提出用多波长线性回归紫外吸光光度法同时测定炼油厂污水中的苯酚和苯胺。方法省去了萃取，蒸馏，显色等步骤，操作简单，对合成水样进行测定，相对标准偏差≤４．５７％，相对误差≤±２．３％。对炼油厂水样进行测定并进行加标回收试验，苯酚和苯胺的回收率分别为９９．４％－１０３．０％和９７．２％－１０４．）％，结果良好，苯酚和苯胺的最低检出限分别为０．０１０和０．０４８μｇ．ｍｌ＾－１。     

导数—多波长线性回归吸光光度法同时测定锰钴锌

研究了以5-Br-PADAP为显色剂,导数-多波长线性回归吸光光度法同时测定锰、钴、锌。在pH 9.2的氯化铵-氨水和乳化剂OP介质中,锰、钴和锌与5-Br-PADAP发生较灵敏的显色反应。在波长560～574nm范围内每隔2nm进行导数-多波长线性回归,方法应用于大米、面粉和啤酒中的锰、钴、锌同时测定,获得了较好的结果。     

三波长校正光度法测定水果蔬菜中多菌灵残留量

研究了三波长光度法测定水果蔬菜中多菌灵残留量的最佳测定条件，在pH8．3的条件下，测定278，281和290nm波长处的吸光度，计算出校正吸光度，校正吸光度与多茵灵含量在0～50μg范围内呈线性关系，相关系数为0．9991，方法检出量为0．773μg；样品的加标回收率在93．5％～101．0％范围内，测定结果满意。     

多波长线性回归—导数吸光光度法同时测定三组分混合物

提出了等吸收点-多波长线性回归-(导数)吸光光度法同时测定三组分混合物的原理,以5-Br-PADAP-溴代十六烷吡啶(CPB)-金属离子显色体系为例,通过测定合成样品及铝合金中的锰、铜、锌.对方法的可行性进行了验证,结果良好.     

比值导数波谱-多波长最小一乘回归分光光度法同时测定饮料中糖精钠、苯甲酸和山梨酸

提出了比值导数波谱－多波长最小一乘回归分光光度法。该法能同时测定三组分混合物而毋需零交点波长和等吸收点，且回归稳健性好．可消除异常点的影响。方法用于合成样品和饮料中糖精钠、苯甲酸和山梨酸的同时测定，相对误差＜± ３． ５％，回收率为 ９６． ６％～１０４．４％，相对标准偏差为２．０％～３．１％．     

7-(对甲酰基苯偶氮)-8-羟基喹啉-5-磺酸的合成及其双波长分光光度法测定镓

7－（对甲酰基苯偶氮）－8－羟基喹啉－5－磺酸是一新显色剂。该试剂在微碱性介质中（pH＝7．5）与镓形成黄色络合物。络合物λmax＝392nm，摩尔吸光系数ε392＝2．24×104L·mol-1·cm-1。同时在500nm呈现负峰，用双峰观波长法测定镓ε392～500＝6．89×104L·mol-1·cm－1，灵敏度是单波长法的三倍多．线性范围0～2．0×10－5mol／L。用拟定的方法测定了掺硅的GaAS材料及岩石中的镓，加入回收率为106％～110％；方法的相对标准偏差小于1．6％。     

两次双波长分光光度法同时测定痕量钴和镍

以PAR为显色剂，乳化剂OP为增敏剂，采用系数补偿和双峰双波长的两次双波长分光光度法同时测定痕量钴(Ⅱ)和镍(Ⅱ)，钴(Ⅱ)、镍(Ⅱ)的线性范围分别为0～25、0～20μg/(25mL)，回收率分别为97．0％～102．0％、92．4％～105．0％。该法用于矿样的测定，测定结果的相对标准偏差为0．76％～2．9％。     

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.