卷心菜和芹菜中的17种元素测定

采用微波消解法处理卷心菜和芹菜样品,并用ICP-AES法测定这两种蔬菜中的17种微量元素Ca,Mg,K,Na,P,Zn,Fe,Cu,Mn,Al,Se,Cr,Ni,Cd,As,Pb,Hg。结果表明,两种蔬菜中均含有丰富的矿物元素Ca,Mg,K,Na,P,芹菜中的矿物元素更高,也存在少量能调节人体生理机能的有益微量元素Zn、Fe、Mn、Al、Cu、Ni,除了卷心菜中Hg含量超标外,其它有害重金属元素均属国家食品安全卫生标准之内。     

藏药材白花龙胆花中微量元素的分析

对藏药材白花龙胆花中17种微量元素（Cu、Zn、Fe、Mn、Co、Ni、Se、Cr、Mg、Ca、K、Na、P、As、Hg、Pb、Cd）的含量作了测定。结果表明,白花龙胆花中含有较高的人体必需微量元素和常量元素,其中常量元素K、Ca、Na、Mg和微量元素Zn、Fe、Mn的含量均较高。     

白族长寿地区硬果仁中19种元素的测定分析

用电感耦合等离子体发射光谱法（ICP－AES）,对云南省白族长寿区的葵花子仁、麻子仁和核桃仁中的Ca、Mg、P、S、Na、AI、B、Fe、Zn、Cu、Mo、Sr、Mn、Cr、Se、Ge、Cd、Pb、As等19种元素进行了测定分析。结果表明,3种硬果仁中含有丰富的人体必需的Ca、Mg、P、S、Na、Fe、Zn、Mn、Se、Cu、Cr、Sr、Mo等有益元素,且P、Mg、S、Ca、Na、Zn、Mn、Fe、Se的含量较高。这些生命元素在3种硬果仁中的含量存在差异。有害元素Cd、Pb均未检出,核桃仁中As含量较高。硬果仁中富含这些生命元素是该地区老人健康长寿的一个重要原因。     

三七生长初期不同部位微量元素的含量测定

采用电感耦合等离子体发射光谱法(ICP-AES),对文山地区GAP种植及农户常规种植的生长初期三七不同部位中的微量元素Mg、P、Ca、Mn、Na、Fe、Co、Cu、Zn、Mo、Cr、Ni、Ge、Se等14种元素进行了测定分析。结果表明,三七的根、茎、叶中含有丰富的人体必需Mg、P、Ca、Mn、Na、Fe、Co、Cu、Zn、Mo、Ge、Se等有益元素,且P、Ca、Mg、Fe含量较高,Na、Mn、Co、Zn次之,Co、Mo、Cr、Ni、Ge、Se含量均较低。为三七GAP栽培标准和特征制订、三七道地药材的化学特征——化学指纹图谱的建立及研究提供理论依据。     

电感耦合等离子体原子发射光谱法测定新疆洋葱籽中常量/微量元素

采用微波消解法处理样品,以电感耦合等离子体原子发射光谱法(ICP-AES)测定新疆洋葱籽样品中Co、Cr、Ca、K、Mg、P、Fe、Mn、Na、Ni、Sn、Zn、Cd、As、Se、Cu、Mo和V 18种常量/微量元素。结果显示,新疆洋葱籽中含有丰富的K、Mg、P、Ca和Na等常量元素,此外微量元素Fe、Mn、Zn、Cr、Ni、Cu的含量也较丰富。新疆洋葱籽中含有很多对人体有益的常量及微量元素,有较高的药用价值。     

前列舒通胶囊中26种无机元素的分析

目的：明确造成前列舒通胶囊不同批次间差异的标志性无机元素,并进行安全性评价。方法：采用ICP-MS测定制剂中Al、As、B、Ba、Ca、Cd、Co、Cr、Cu、Fe、K、Mg、Mn、Mo、Na、Ni、Pb、Sb、Se、Sn、Sr、Ti、Tl、V、Zn和Hg元素含量并进行数据分析。运用主成分及综合评分结合聚类分析手段,确定制剂的特征性元素;进行元素含量和相关性分析,明确不同批次各元素的差异及元素之间的关系;以多元素含量为指标,绘制无机元素谱图。结果：19批样品中均未检测出Se、Mo、Sn、Sb、Tl和Hg,且Pb、Cd、As、Cu、Hg均符合限量标准,无机元素含量谱图趋势一致。主成分分析提取了4个主成分,确定元素B、K、Al、V、Cr、Ca、Ti、Na、Co和Mn可作为特征元素。主成分得分图将19批样品分为两类,聚类分析及综合评分结果与其一致,两类样品中各元素含量存在差异性。相关性分析中,明确了B与K、Al、Cr正相关,K与Cr、Co正相关,V与Cr、Mn正相关,Mn与Co正相关,Ca、Ti、Na两两正相关。结论：通过分析前列舒通胶囊中无机元素含量,确定了特征元素,为前列舒通胶囊质量全面控制研究提供科学依据。     

电感耦合等离子体原子发射光谱法(ICP-AES)测定不同品种山药中矿物质元素与对比研究

采用微波消解样品,运用电感耦合等离子体原子发射光谱法同时测定山药中K,Na,Ca,Mg,Zn,Fe,Cu,Mn,Se,Pb,Cd和Cr 12种元素。结果表明:方法简便、快速、准确;山药富含对人体有益的K,Ca,Fe,Mg,Zn,Mn,Se等矿物质元素,其肉质中重金属元素Pb,Cd,Cr含量均未超过国家食品卫生标准。     

青藏高原多年冻土区高寒草甸植物群落主要植物化学元素含量特征

分析了青藏高原北麓河地区29种高寒植物15个元素含量的特征。结果表明,这些植物中元素平均含量>400μg/g的元素有Ca,Mg,Na,K,Fe,10～100μg/g的有Mn,Cr,Zn,Cu,<10μg/g的有Ni,Co,As,Pb,Cd,Hg;种间同种元素的含量变化规律不统一。相关性分析表明,Cu与Cd,Fe与Cd和Hg,Cr与Ni,Co和Mg极显著正相关,Cr和Ca极显著负相关;聚类分析表明,Na,As元素对本区植物聚类的影响最大,莎草科、禾本科、菊科科内植物元素含量相似。     

微波消解/ICP—AES法测定不同品种山药中矿物质元素与对比研究

采用微波消解样品,运用电感耦合等离子体原子发射光谱法同时测定山药中K、Na、Ca、Mg、Zn、Fe、Cu、Mn、Se、Pb、Cd和Cr等12种元素。结果表明：方法简便、快速、准确度高;四种山药均富含对人体有益的K、Ca、Fe、Mg、Zn、Mn、Se等矿物质元素,其肉质中Pb、Cd、Cr含量均未超过国家食品卫生标准。     

微波辅助消解ICP-AES法测定小茴香中20种元素

采用微波消解法处理小茴香样品,电感耦合等离子体发射光谱(ICP-AES)测定其中Na、K、Sr、Ca、Mg、P、As、Zn、Pb、Co、Cd、Ni、Ba、Fe、Mn、Cr、Cu、Al、Ti和B 20种常量和微量元素的含量。20种元素的检出限为0.00002~0.00468μg·mL-1,回收率为89.50%~107.89%,相对标准偏差(RSD)均小6%。结果显示,小茴香果实及其嫩叶中除含有人体必需的常量元素K,Na,Ca,Mg,P外,还含有Fe、Zn、Mn、Cr、Co等必需的微量元素和其他元素Ti、B、Ni、Al、Sr、Ba等。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

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.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.     

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%).     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

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.