三试剂自动分析法测定血清总铁结合力——5-Br-PADAP直接光度法

为建立简便、灵敏的测定血清总铁结合力(TIBC)自动化分析法,在表面活性剂存在下,用2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚(5-Br-PADAP)为显色剂测定血清TIBC。该法线性范围0~180μmol/L,平均回收率为99.71%,批内变异系数(CV)和批间变异系数分别为0.024、0.041,与临床检验操作规程推荐的方法比较具有良好的相关性,线性回归方程和相关系数分别为y=0.994 3x 1.220 6,r=0.996 8。血清TIBC含量测定结果(-x±2s):105例健康男性48.0~76.0μmol/L,98例健康女性血清52.0~76.0μmol/L。可见用5-Br-PADAP三试剂自动化分析法测定血清TIBC方法简便、灵敏可靠,适合临床应用。     

三试剂自动分析法测定血清总铁结合力：Nitro—PAPS直接光度法

为建立简便、灵敏的三试剂自动化分析法测定血清总铁结合力（TIBC）,在表面活性剂存在下,用2-（5-硝基-2-吡啶偶氮）-5-[N-正丙基-N-（3-磺酸丙基）氨基]苯酚二钠（Nitro—PAPS）为显色剂测定了血清TIBC。结果表明,该法线性范围0～195μmol／L,平均回收率为100．7％,批内变异系数（CV）和批间变异系数分别为0．019、0．032;与临床检验操作规程推荐的方法比较具有良好的相关性,线性回归方程和相关系数分别为Y=1．0021x＋1．2100,r=0．9798;78例健康男性血清TIBC含量（x±2s）为46．8—76．1μmol／L,75例健康女性为52．8—77．6μmol／L。方法简便、灵敏可靠,适合临床应用。     

血清铜自动分析法试剂盒的研制与分析: 5-Br-PADAP直接光度法

为研制、评价血清铜 5 -Br -PADAP自动分析法试剂盒 ,在表面活性剂存在下 ,用2 -(5 -溴 -2 -吡啶偶氮 ) -5 -二乙氨基酚 (5 -Br -PADAP)作显色剂 ,双试剂两点终点法测定血清铜。结果表明 ,该法线性范围 0～ 80 μmol L ,平均回收率为 1 0 0 7% ,批内变异系数 (CV)和批间变异系数分别为 0 0 1 5～ 0 0 2 0和 0 0 2 3～ 0 0 3 0 ,与原子吸收分光光度法比较具有良好的相关性 ,y =1 0 0 1x -0 0 93 ,r=0 9948,P >0 0 5。 1 0 7例健康人血清铜含量为 1 6 68± 2 62 μmol·L-1(x± 2S)。可见用本试剂盒双试剂自动化分析法测定血清铜方法简便、灵敏可靠 ,适合临床应用     

5-Br-PADCAP 直接光度法测定血清未饱和铁结合力

为建立简便、灵敏的双试剂自动化分析法测定血清未饱和铁结合力(UIBC),在表面活性剂存在下,用2-(5-溴-2-吡啶偶氮)-5-[(N,N-二羧基甲基)氨基]苯酚(5-Br-PADCAP)为显色剂测定血清UIBC。结果表明,线性范围0~90μmol/L,平均回收率101.57%,批内变异系数(CV)和批间变异系数分别为0.028、0.046,与日本和光UIBC测定试剂盒比较具有良好的相关性,线性回归方程和相关系数分别为y=1.0133x-0.3356,r=0.9961。108例健康人血清UIBC含量为31.65~50.81μmol/L(±2s)。用5-Br-PADCAP双试剂自动化分析法测定血清UIBC方法简便、灵敏可靠,适合临床应用。     

以Nitro-PAPS为显色剂计算法测定血清总铁结合力

建立了以2-(5-硝基-2-吡啶偶氮)-5-[N-正丙基-N-(3-磺酸丙基)氨基]苯酚二钠(nitro-PAPS)为显色剂、计算法测定血清总铁结合力(TIBC)的方法,通过测定血清铁和血清未饱和铁(UIBC)含量,以血清铁和血清UIBC含量之和计算血清TIBC含量。该法线性范围0～170μmol/L,平均回收率为101.1%,批内变异系数(CV)和批间变异系数分别为0.033、0.042,与临床检验操作规程推荐的方法比较具有良好的相关性,线性回归方程和相关系数分别为y=1.002 3 x 1.44,r=0.971 21。86例健康男性血清TIBC含量为47.5～76.6μmol/L(x±2 s),70例健康女性血清TIBC含量为52.7～77.6μmol/L(x±2 s)。以nitro-PAPS为显色剂计算法测定血清总铁结合力TIBC方法简便、灵敏可靠,适合临床应用。     

铁-荧光镓极谱络合吸附波的研究

在 p H6.1 0的 0 .1 mol/L ( CH2 ) 6 N4-HCl底液中 ,用单扫示波极谱法可获得铁( ) -荧光镓体系灵敏的络合吸附波。在 1 .0× 1 0 - 7～ 7.0× 1 0 - 6 mol/L范围内 ,铁浓度与波高呈线性关系 ,检测限达 7.0× 1 0 - 8mol/L,已成功地应用于金属镁粉中的铁和铝的测定 ,并测得电活性络合物的组成为铁∶荧光镓 =1∶ 1 ,条件形成常数β=3 .2× 1 0 4,表面电极反应速率常数 ks为 2 .9s- 1 。     

铬蓝黑R-示波计时电位法快速测定天然水中不同形态的铝浓度

本文报道铬蓝黑 R-示波计时电位法快速测定天然水中不同形态的铝。在 0 .5mol/L 乙酸 -乙酸铵 - 1× 1 0 - 3mol/L铬蓝黑 R( p H4.6)底液中 ,铝 -铬蓝黑 R铬合物在 - 0 .80 V电位处产生灵敏切口 ,切口深度与铝浓度成正比 ,线性范围为 8× 1 0 - 7～6× 1 0 - 5mol/L,检测下限为 6× 1 0 - 7mol/L,相对标准偏差为 4.8% ( n=1 0 ,4× 1 0 - 5mol/L Al)。应用该法测定了天然水中不同形态的铝浓度 ,并同 Driscoll的 MIBK-GF/AAS法进行了比较 ,结果基本一致     

新的铬天青B直接光度法测定血清总铁结合力

为建立新的铬天青B直接光度法测定血清总铁结合力（TIBC）,在表面活性剂存在下,用铬天青B（CAB）为显色剂测定了血TIBC。结果表明,该法线性范围0～160μmol／L,平均回收率为99．4％,批内变异系数（CV）和批间变异系数分别为0．020、0．035,与临床检验操作规程推荐的方法比较具有良好的相关性,线性回归方程和相关系数分别为y=1．0033x＋0．4510,r=0．9982;60例健康男性血清TIBC含量为46．2～75．8μmol／L（x±2s）,60例健康女性血清TIBC含量为51．8～76．9μmol／L（x±2s）。用新的铬天青B直接光度法测定血清总铁结合力方法简便、灵敏可靠,适合临床应用。     

5-Br-PADCAP分光光度法测定血清锌

为建立快速、简便、灵敏的分光光度法测定血清锌 ,在表面活性剂TritonX -1 0 0存在下 ,用 2 -(5 -溴 -2 -吡啶偶氮 ) -5 -[N ,N -二羧基甲基 ]苯酚 (5 -Br-PADCAP)作显色剂 ,不去蛋白分光光度法测定血清锌。结果表明 ,锌络合物最大吸收波长为 5 5 7nm ,线性范围 0～ 5 0 0μmol L ,摩尔吸光系数为 1 1 2× 1 0 5L·mol-1·cm-1。回收率为 99 9% ,批内变异系数 (CV)为2 1 % ,批间变异系数为 2 9% ,与原子吸收分光光度法 (x)比较具有良好的相关性 ,y =1 0 1 0x-0 1 5 4,r=0 991 8,P >0 0 5。可见本法测定血清锌不必去蛋白、用血量少、方法简便、灵敏可靠 ,适合临床应用     

以5-Br-PADAP为显色剂计算法测定血清总铁结合力

建立了以5-Br-PADAP为显色剂计算法测定血清总铁结合力(TIBC)的方法,通过测定血清铁和血清未饱和铁(UIBC)含量,以血清铁和血清UIBC含量之和计算血清TIBC含量。该法线性范围0~168μmol/L,平均回收率为100.4%,批内变异系数(CV)和批间变异系数分别为0.031、0.046,与临床检验操作规程推荐的方法比较具有良好的相关性,线性回归方程和相关系数分别为y=0.9978x 1.26,r=0.9745。65例健康男性血清TIBC含量为47.61~76.24μmol/L(x±2s),57例健康女性血清TIBC含量为52.56~77.45μmol/L(x±2s)。以5-Br-PADAP为显色剂计算法测定血清总铁结合力TIBC方法简便、灵敏可靠,适合临床应用。     

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.