高效毛细管电泳法同时测定减肥类功能食品中7种违禁成分

建立了同时测定减肥类功能食品中违禁成分芬氟拉明、伪麻黄碱、去甲伪麻黄碱、安非拉酮、西布曲明、西地那非和士的宁的高效毛细管电泳分析方法。以20 mmol/L硼砂-10 mmol/L SDS-5%乙腈溶液(pH9.0)为运行缓冲液,在25℃,17 kV条件下测定,检测波长为195 nm。各待测物线性范围上限均为100 mg/L,线性相关系数均大于0.998,相对标准偏差为4.5%~7.9%(n=7);平均加标回收率为79.6%~112.0%;检出限(S/N=3)为0.16~0.65 mg/L。本方法简便快速、灵敏准确、分析成本低,已成功应用于功能食品中上述减肥类违禁添加成分的测定。     

固相萃取–高效液相色谱串联质谱法测定食品中麻黄碱、芬氟拉明、西布曲明和酚酞

建立固相萃取–高效液相色谱串联质谱法同时检测食品中可能非法添加的4种违禁添加药物(麻黄碱、芬氟拉明、西布曲明、酚酞)的分析方法.样品经0.1 mol/L盐酸水溶液提取后,经过Oasis HLB柱净化,采用电喷雾(ESI)离子源电离,正离子多反应监测(MRM)模式检测,以保留时间和子离子比进行定性分析,外标法定量分析.结...     

催化柴油中氮化物分布的气相色谱-原子发射光谱分析方法的研究

建立了催化柴油馏分中各种氮化物类型分布的气相色谱-原子发射光谱(GC-AED)分析方法,考察了色谱条件和不同的试剂气压力对各种氮化物分离和检测灵敏度的影响,定性(或归类)了某典型催化柴油中的73个氮化物,计算了程升条件下各种氮化物的保留指数,为不同实验室的定性比较提供了依据。以峰面积对质量浓度作图,氮化物在2.0~600 mg/L浓度范围内,AED检测器对不同氮化物有良好的线性响应,线性相关系数达0.998。几种氮化物(吲哚、1-甲基吲哚、C2-吲哚、咔唑、1-甲基咔唑、1,8-二甲基咔唑)峰面积的相对标     

氮杂吲哚合成

氮杂吲哚是一类重要的杂环分子,在材料科学以及药物设计与合成中具有重要地位。由于氮杂吲哚在结构上区别于吲哚,所以一些经典的合成吲哚的方法并不很适用于氮杂吲哚的合成。近年来,金属有机化学的发展为氮杂吲哚的合成提供了更多的原料选择以及更有效的成环方式,从而为氮杂吲哚的合成开辟了新的方向。本文综述了氮杂吲哚有机合成方法学近年来的进展,介绍了通过Bartoli合成、Fischer吲哚合成、有机锂试剂、过渡金属促进以及其他方法来合成氮杂吲哚类化合物的研究,总结了合成各类氮杂吲哚(4-氮杂吲哚、5-氮杂吲哚、6-氮杂吲哚以及7-氮杂吲哚)的常用有机合成方法,为促进氮杂吲哚类化合物在药物合成化学以及材料科学方面的应用提供了基础。     

基质分散固相萃取-高效液相色谱-串联质谱法同时测定减肥保健食品中20种违禁添加药物

建立了测定减肥保健食品中20种违禁添加药物(芬氟拉明、苯丙醇胺、西布曲明、舍曲林、利莫那班、安非他酮、西酞普兰、氟西汀、苯氟雷司、托吡酯、唑尼沙胺、咖啡因、酚酞、大黄素、吲达帕胺、布美他尼、托拉塞米、三氨喋啶、奥利司他、苯乙双胍)的基质分散固相萃取-高效液相色谱-电喷雾串联质谱分析方法。不同类型的样品经乙醇-丙酮(7∶3,V/V)超声提取后,提取液经N-丙基乙二胺(PSA)、十八烷基硅烷(ODS)净化,以Waters Atlantis T3柱(150 mm×2.1 mm,3μm)分离,采用HPLC/MS/MS电喷雾电离,多反应监测模式检测,以保留时间和子离子比进行定性分析,外标法进行定量分析。20种减肥药物的检出限为0.05~3.0 mg/kg,在不同添加水平范围内的回收率为67.1%~101.4%,日内精密度均小于10%,日间精密度均小于15%。本方法分析速度快,适用于减肥保健食品的实际检验工作。     

减肥保健品中芬氟拉明等8种合成食欲抑制剂的分析测定

建立了用气相色谱同时测定减肥保健品中芬氟拉明、苯丁胺 ,苄非他明、氯苯丁胺、氯苄苯丙胺、苯双甲吗啉、苯甲吗啉及安非泼拉酮等 8种合成食欲抑制剂的方法 ,检出限 <10 0 μg /L。分析结果用GC/MSD进一步确证 ,准确、可靠。     

N-(3-吲哚甲酰基)-β-丙氨酸甲酯的结构鉴定

为研究吲哚衍生物的生理活性,对吲哚进行三氯乙酰化、并与β-丙氨酸甲酯缩合,合成了含吲哚环氨基酸甲酯.通过1H NMR,IR,MS和元素分析对产物结构进行了鉴定,确证其为N-(3-吲哚甲酰基)-β-丙氨酸甲酯.     

吲哚甲酰腙化合物的微波合成和表征

微波辐射条件下,以甲醇作溶剂,6-吲哚甲酸甲酯与水合肼反应合成6-吲哚甲酰肼(1),进一步在微波辐射条件下,以醋酸为溶剂,由6-吲哚甲酰肼(1)与取代芳香醛反应制得目标化合物2(a~f).合成的6个目标化合物通过熔点测定和质谱、红外光谱、核磁共振氢谱和元素分析对其结构进行确证.     

金催化的吲哚与末端炔烃的分子间烷基化反应

尝试了用金(Au)催化吲哚和炔烃的Friedel-Crafts烷基化反应, 具体探讨了金(I)配合物催化吲哚与末端炔烃的烷基化反应的条件, 并制备了一系列尚未见文献报道的双取代β-吲哚烷基化衍生物. 产物的结构经1H NMR, 13C NMR, MS和元素分析确证. 并对其反应机理可能性进行了推测.     

用液相制备色谱从菜籽中分离、纯化制备硫代葡萄糖苷

从我国甘蓝型、芥菜型油菜籽中,用弱离子交换剂ＤＥＡＥＳｅｐｈａｄｅｘＡ－２５作固定相,Ｋ＿２ＳＯ＿４作流动相,采用自动柱色谱仪分离制备非吲哚类硫代葡萄糖苷和吲哚类硫代葡萄糖苷结晶粗品。从非吲哚类硫代葡萄糖苷结晶粗品中进一步分离和纯化,制得２－羟基－３－丁烯基硫代葡萄糖苷和３－丁烯基硫代葡萄糖苷的钾盐晶体。经元素、熔点分析和质谱、红外图谱、紫外图谱、ＨＰＬＣ图谱证实,结晶物可作为硫代葡萄糖苷定性和定量分析时的标准物。     

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.