ICP-MS法测定彭泽贝母中微量元素的含量及形态分析

目的:测定彭泽贝母中微量元素含量,研究彭泽贝母中微量元素的存在形态,探讨微量元素的含量和形态.方法:采用HNO3-H2O2微波消解体系,电感耦合等离子质谱法(ICP-MS)测定彭泽贝母中铅、钙、铁、锰、锌、镉、钡、铬等10种微量元素的含量,初步探究微量元素的存在形态.结果:Ca元素在彭泽贝母中含量最高,而Mo元素含量最低;彭泽贝母中微量元素是以无机态为主、多种形态共存的复杂体系.结论:彭泽贝母中含有丰富的人体必需微量元素,可能促进其有效成分作用的发挥.     

火焰原子吸收光谱法分析香菇中微量元素的形态

对香菇中Cu、Zn、Fe、Mn、Ca和Mg进行了微量元素的含量和形态分析.分别用0.45μm滤膜,D101型大孔吸附树脂,将香菇水煎掖中Cu、Zn、Fe、Mn、Ca和Mg分为悬浮态和可溶态、有机态和无机态,用HCl和CCl4处理煎渣,得煎渣无机态和有机态,火焰原子吸收光谱法测定香菇各形态含量.方法的回收率在95.0%～101.7%范围内,相对标准偏差均在2%以下.     

原子吸收法对藏草药川木香中12种元素的初级形态分析

用原子吸收分光光度法,测定了产于青藏高原的藏草药川木香的全药材、水提液、醇提液中12种元素(Cr、Cu、Fe、Mn、Ni、Se、Zn、K、Ca、Mg、Cd、Pb)的含量,以及水提液中各元素可溶态、水溶态的含量,同时采取正辛醇-水分配体系模拟藏药水提液中各微量元素在人体胃肠中的分配情况,对藏药中微量元素的初级形态进行了分析,初步探讨了酸度变化(人体胃肠酸度)对微量元素的影响,结合藏药药效讨论其相关性,为进一步研究微量元素与藏药药性、药效的关系提供科学的依据和奠定基础.     

全蝎不同部位的宏量和微量元素含量比较

为探讨雌雄全蝎及不同药用部位的宏量和微量元素含量差异及与药效和毒性的相关性,采用发射光谱法测定雌雄全蝎及不同药用部位中宏量元素 Ca、Mg及微量元素 Fe、Cu、Zn、Mn、 Pb七种元素的含量.结果表明,雌雄蝎尾宏量元素 Ca、Mg和微量元素 Fe、Cu、Zn、Pb均明显低于全蝎和全蝎头部及腹部,其微量元素谱为 Fe＞Zn＞Cu＞Mn＞Pb;雄性全蝎 Zn含量明显低于雌性全蝎,而其含水量和有毒微量元素 Pb却明显高于雌性全蝎,雄性全蝎各药用部位宏量和微量元素亦明显低于雌性全蝎;全蝎宏量元素 Ca比文献高6～8倍,而 Mg含量与文献一致.可认为雌性全蝎及其药用部位药材质量和微量元素含量均明显优于雄性全蝎;蝎尾的镇痛和毒性作用与宏量和微量元素含量无关.     

原子吸收法对藏草药水母雪兔子和多刺绿绒蒿中12种元素的初步形态分析

用原子吸收光谱法,对产于青藏高原的藏草药水母雪兔子和多刺绿绒蒿,测定了全药材、水提液、醇提液中12种元素(Cr、Cu、Fe、Mn、Ni、Se、Zn、K、Ca、Mg、Cd、Pb)的含量,以及水提液中各元素可溶态、水溶态的含量,同时采取正辛醇-水分配体系模拟藏药水提液中各微量元素在人体胃肠中的分配情况,对藏药中微量元素的初级形态进行了分析,初步探讨了酸度变化(人体胃肠酸度)对微量元素的影响,结合藏药药效讨论其相关性,为进一步研究微量元素与藏药药性、药效的关系提供科学依据.     

玄参、生地黄、紫草等六种中药中微量元素含量的测定

为了解中药中微量元素的含量与其药物的作用机制关系,用原子吸收分光光度计测定了玄参、生地黄、紫草、水牛角、牡丹皮、赤芍中铁(Fe)、镁(Mg)、铜(Cu)、钙(Ca)、锌(Zn)、铬(Cr)、钼(Mo)等7种微量元素的含量.结果表明,Ca的含量最高,Cu的含量几乎最低.这6种中草药含有多种对人体有益的微量元素,与它们的药...     

北五味子果实、茎和叶中微量元素的测定

采用硝酸和过氧化氢混合酸体系作消化液,利用电感耦合等离子质谱(ICP-MS),对延边地区不同产地五味子中微量元素的含量,进行了测定和研究。测定了不同产地五味子叶、茎、果实中Mg、Ca、Fe、Zn、Cu、Mn、Cr?Ni?Pb?Cd等19种元素的含量水平。测定结果显示五味子中K、Ca、Mg、Fe含量丰富,而Pb、Cd的含量很低。不同地区的五味子茎、叶、果实中微量元素含量存在很大差异。     

2型糖尿病患者血清微量元素分析

为探讨2型糖尿病与患者血清微量元素的关系,对105例2型糖尿病患者血清Fe、Zn、Cu、Cr、Mg、Ca进行了观察,并与正常对照组做比较,各指标间做相关分析,结果表明,2型糖尿病患者血清Zn、Cr含量明显低于对照组,Cu的含量明显高于对照组,Fe、Mg、Ca的含量两组无差异。提示糖尿病患者体内微量元素的含量与糖尿病具有密切的关系。     

苏州市儿童血清中微量元素含量分析

为了解苏州市儿童血清中微量元素的含量,用OlympusAu 40 0 (日本)全自动生化分析仪检测了苏州大学附属儿童医院儿保门诊3 5 0例体检儿童血清中的微量元素含量。结果表明,本地区儿童血清中Ca、P、Mg、Cu、Fe、Zn含量依次为:(2 .3 4±0 . 1 4)mmol/L、(1 .5 8±0 . 2 3 )mmol/L、(0 .89±0 . 1 1 )mmol/L、(2 4. 62±5 .0 5 ) μmol/L、(1 5 . 0 2±5. 63 ) μmol/L、(2 0 . 86±5 . 74) μmol/L。男、女儿童间Ca、P、Mg、Cu、Fe、Zn含量差异无显著性(P值均>0 . 1 0 ) ;在不同年龄组间,Mg、Zn含量差异无显著性(P值均>0 . 1 0 ) ,Ca、P、Cu、Fe含量差异显著(P值均<0 .0 1 ) ;Fe含量随年龄的增长而逐步增加,Ca含量随年龄的增长而逐步降低。     

微波消解-FAAS法测定大别山区三种中药中的微量元素

采用微波消解-火焰原子吸收光谱(FAAS)法对大别山区3种中药(何首乌、黄精和拐枣)中的微量元素进行测定。用微波消解仪处理样品,对消解条件及消解程序进行优化,在最佳微波消解条件下,结合FAAS法测定上述3种中药中Ca、Mg、Cu、Zn、Fe、Mn 6种元素的含量。结果表明,微波消解的最佳条件为:何首乌和拐枣采用HNO3-H2O2混酸体系,配比分别为5∶2和5∶3,固液比1∶20,最高功率(700W)时的保温时间分别为8min和6 min;黄精采用HNO3-HCl,混酸体系,配比5∶2,固液比1∶28,保温时间为8 min。所建立的定量分析方法回收率为95.63%～101.36%,相对标准偏差小于3.0%,线性相关系数大于0.999,方法检出限为0.18～2.20 ng/mL。3种中药中均含有丰富的微量元素,尤其是黄精中Fe、Ca和Mn的含量较高;何首乌中Mg、Zn和Fe含量相对较高;拐枣中Fe和Ca含量相对较高。研究结果可为上述3种中药中微量元素的含量与其药效的相关性提供科学依据。     

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.