氢化物-原子荧光法测定粮食中的砷

研究了氢化物－原子荧光法测定粮食中砷的适宜条件,试验了酸介质和还原剂的用量对测定砷的影响,选择了仪器的最佳工作条件及氢化物发生条件,试验了生成氢化物元素及粮食中常见元素对测定的干扰情况。在测定条件下,砷的线性范围为０～８０μｇ／Ｌ,检出限为０．３μｇ／Ｌ。用该法测定了标准物质小麦粉及大米,结果与推荐值吻合。方法快速、准确,应用于进口粮食中砷的检测,获得满意结果     

健康猕猴血液和毛发微量元素含量的正常值测定和差异比较

对猕猴(Macaca mulatta)血液和毛发的镁、锰、钼、镍、铅、铬、镉、锌、铁、铜、钙等11种元素的含量，用电感耦合高频等离子体发射光谱仪进行了测定．给出了各个元素在血液和毛发中的平均含量值和变动范围．指出毛发中的微量元素含量一般较血液为高，且变动较小．与人体内含量比较，猴毛发的Cu、Mo、CA、Ni的含量与人发接近；猴血液的Zn、Fe、Ca、Mn、Ca亦与人的接近．对猴血液微量元素含量随年龄、体重、性别变化及血液含量和毛发含量的相关关系进行了统计学检验．通过对测定值的比较分析，认为尽管动物体内的微量元素含量随种类、环境、个体差异变化较大，就群体平均含量而言，仍存在着相似的变化规律。本文的测定结果对了解猕猴对微量元素的需要提供了初步依据．     

用多变量统计分析方法辨识肺癌患者分类中的关键元素(英文)

用逐步判别、主成分分析和聚类方法研究了根据血清和毛发样品中元素含量对正常人和肺癌患者分类中的关键元素．用主成分分析的结果表明,在肺癌患者与正常人的分类中,血清中的Ｃａ,Ｃｒ,Ｃｕ,Ｐ和Ｚｎ是关键元素,而毛发中的Ａｌ,Ｂ,Ｃｒ,Ｐ和Ｓｒ是关键元素．对于正常人和癌症患者元素之间的欧氏距离不同     

小鼠血清,全血和鼠毛中的元素含量研究

报告了健康Ｃ５７ＢＬ小鼠血清，全血和鼠毛中９种元素含量。在３种生物样品中测定的元素以鼠毛中含量最高，血清中最低，本文讨论了小鼠和人的血清和毛发元素水平之间的关系，Ｃ５７ＢＬ小鼠作为研究元素和疾病关系的实验动物有其优点。     

小麦粉的ICP-AES多元素同时测定

本文报告了ICP-AES法同时测量小麦粉中Ca、Mg、Al、Fe、Cu、Zn、Mn、Ba、Y、Ni的含量。采用元素间干扰系数法校正主要基体元素对微量元素测定的光谱干扰。本法应用于湖南省粮食中重金属含量调查与评价,获得了令人满意的结果。     

ICP－AES测定东北虎、梅花鹿等动物毛发中的微量元素

研究了东北虎、梅花鹿等动物毛发中元素的ＩＣＰ－ＡＥＳ分析方法，报道了上述动物毛发中的Ａｌ、Ｃａ、Ｃｕ、Ｆｅ、Ｍｇ、Ｍｎ、Ｐ、Ｐｂ、Ｓｒ、Ｚｎ等元素的含量，为研究微量元素与动物健康的关系提供了参考。     

ICP—AES测定东北虎,梅花鹿等动物毛发中的微量元素

研究了东北虎，梅花鹿等动物毛发中元素的ＩＣＰ－ＡＥＳ分析方法，报道了上述毛发中的Ａｌ，Ｃａ，Ｃｕ，Ｆｅ，Ｍｇ，Ｐ，Ｐｂ，Ｓｒ，Ｚｎ等元素的含量，为研究微量元素与动物仞关系提供了参考。     

罗丹明3B分光光度法测定食品和生物样品中微量汞

本文采用双硫腙-四氯化碳萃取浓集汞以分离干扰物质,研究了罗丹明3B置换光度法测定汞,提高了测定微量汞的灵敏度和稳定性。水样的分析灵敏度达0.5ppb。食品可测至0.02ppm(对5克试样)。对生物样品采用了不同回流装置的五氧化二钒催化消化法,方法简便,汞的回收率在90％以上。本法适用于粮食、酵母、毛发、牛奶和水中微量汞的测定。     

男性型秃发患者发中K,Na,Ca,Mg元素含量分析

采用火焰原子吸收法对３０例男性型秃发患者及３８例毛发健康男性对照者发中宏量元素Ｋ、Ｎａ、Ｃａ、Ｍｇ的含量进行了测定。结果表明，男性型秃发患者发Ｋ含量明显高于对照组，具有统计学上的显著差异（Ｐ〈０．０１）。发Ｎａ、Ｃａ、Ｍｇ含量在两组间未见显著差异（Ｐ〉０．０５）。本文提示，体内某些宏量元素变化对男性型秃发可能产生一定影响。     

食品中重金属元素检测方法研究进展

食品安全问题是直接关系到人民健康的重大民生问题。简要阐述了食品中重金属对人体的影响与危害,全面分析了重金属元素对食品的污染,从不同种类的食品,包括农作物(粮食、蔬菜、水果、食用菌、茶叶)、水产品、畜禽产品、食用油、食用酒精等方面,综述了近年来食品中重金属检测方法研究的进展。随着检测技术的不断发展进步,快速、灵敏、无损的多元素在线检测的方法必将在食品中重金属元素的测定方面得到广泛的应用。     

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.