无溶剂条件下碘催化不对称双吲哚的合成

在室温以及无溶剂条件下,吲哚与烷基-3-吲哚基甲醇在碘的催化下以73％～99％的高收率得到不对称双吲哚烷基化合物。其结构经^1H NMR,IR及MS表征。     

酸度调控的3,3-二乙硫基丙烯酸酯的吲哚化反应

探讨了酸度调控的3,3-二乙硫基丙烯酸酯的吲哚化反应,选择性地合成3,3-二吲哚基丙烯酸酯和3-吲哚基-3-氧代丙酸酯.研究表明,3,3-二乙硫基丙烯酸酯与吲哚反应时,在稀酸条件下,高产率生成3,3-二吲哚基丙烯酸酯,而在浓酸条件下,生成的3-吲哚基-3-乙硫基丙烯酸酯不稳定,在后处理和柱层析分离时易水解,高产率得到3-吲哚基-3-氧代丙酸酯.     

铜催化加成/取代串联反应构建四取代的三吲哚甲烷

在温和的条件下,利用3-乙酰基吲哚与吲哚的加成/取代串联反应,高效地合成了一系列高度拥挤的四取代三吲哚甲烷.该方法通过在3-乙酰基吲哚的氮原子上引入吸电子基团,提高了3-乙酰基吲哚的反应活性,具有原料廉价易得、底物适用性广、操作简便等优点.     

吲哚美辛的毛细管电泳测定法研究

建立了制剂和体液中吲哚美辛的毛细管电泳高频电导分析法,并用于吲哚美辛肠溶片、复方吲哚美辛酊及血清、尿液中吲哚美辛含量的测定。对电泳介质的种类、浓度以及操作电压和进样量等影响因素进行了优化。实验采用3.0mmol／L乳酸＋0．68mol／L乙醇为电泳介质,分离电压为20.0kV,可在10min内实现对吲哚美辛的分离检测。在最佳实验条件下,吲哚美辛的线性范围为0.05μg／mL—100μg／mL,检出限为0．01μg／mL,回收率92.0％-105．1％。     

2-吲哚酮和5-甲基-2-吲哚酮的无溶剂法制备

以苯胺和氯乙酰氯为原料在NaOH存在下酰化合成N-氯乙酰基苯胺,然后N-氯乙酰基苯胺在无水AICI,催化下环化合成2-吲哚酮．对由N-氯乙酰基苯胺合成2-吲哚酮的工艺条件进行了改进．结果表明合成2-吲哚酮的最佳条件为：反应温度为220℃,反应时间为60min,加料时温度为180℃,N-氯乙酰基苯胺与氯化钠,无水AlCl3的重量比为1：1：5．5．改进后的合成2-吲哚酮收率达到88．3％,纯度99％,收率比原工艺提高了24．6％．在此基础上,还合成了5-甲基-2-吲哚酮,并得到其最佳条件为：反应温度为190℃,反应时间为30min,加料时温度为180℃,4-甲基-N-氯乙酰基苯胺与氯化钠,无水AlCl3的重量比为1：1：5．5,收率达到83．1％,纯度为99％．     

自支撑柔性聚(5-吲哚硼酸)膜的电化学合成及表征

在三氟化硼乙醚/乙腈的混合体系中,5-吲哚硼酸的电化学氧化可以获得导电率为9×10-4 S·cm-1的自支撑柔性聚(5-吲哚硼酸)膜.5-吲哚硼酸在80％的三氟化硼乙醚亿腈溶液中的起始氧化电位约为0.80V红外光谱确定了5-吲哚硼酸的聚合位点在C2和C3位上.紫外可见光谱测试结果表明聚(5-吲哚硼酸)的能隙约为2.48...     

碘作用下吲哚3位硫醚化反应

本文发展了碘作用下吲哚及其衍生物与芳香族硫醇类化合物的直接硫醚化反应,在吲哚3位形成C-S键。在温和的反应条件下,多种杂环硫醇能够与吲哚反应高产率地得到3位硫醚化合物。     

铜催化加成/取代串联反应构建四取代的三吲哚甲烷（英文）

在温和的条件下,利用3-乙酰基吲哚与吲哚的加成/取代串联反应,高效地合成了一系列高度拥挤的四取代三吲哚甲烷.该方法通过在3-乙酰基吲哚的氮原子上引入吸电子基团,提高了3-乙酰基吲哚的反应活性,具有原料廉价易得、底物适用性广、操作简便等优点.     

褪黑激素的合成

以5－甲氧基吲哚为起始原料，经4步反应合成了褪黑激素（MLT).5－甲氧基吲哚和草酰氯在0℃-5℃定量反应生成5－甲氧基吲哚－3－草酰氯（I），I直接用氨水胺化得98％的5－甲氧基吲哚－3－草酰胺（Ⅱ），Ⅱ用氢化铝锂还原得到5－甲氧基色胺（Ⅲ），收率57％，Ⅲ经乙酰化即得目标产物MLT，收率80％。     

吲哚与亚胺的Friedel-Crafts反应的研究进展

由于吲哚类化合物具有许多生物特性等优点,在众多天然产物和相应的具有生物活性的化合物中起重要的骨架构筑作用,其合成方法的研究格外令人注目.近年来,关于吲哚与亚胺在催化剂作用下发生Friedel-Crafts反应来制备3-取代吲哚甲胺衍生物的报道剧增.对近年来吲哚与亚胺Friedel-Crafts反应的研究情况进行了综述.     

延边地区65～108岁健康老人头发中锌、铜、铁、锰、镁的含量

用原子吸收光谱法测定延边地区317名65～108岁老人头发中锌、铜、铁、锰、镁含量，观察不同民族、性别、年龄老人这些元素的差异。结果表明：1.朝鲜旗发锌低于汉族，满族发铜低于汉族、朝鲜族，汉族发镁高于朝鲜族、满族，发铁、发锰在汉、朝、满民族之间无区别。2．汉族、朝鲜族男发锌高于女性，汉族女性发铜高于男性，发铁、发锰、发镁在性别之间无区别。3、90岁组朝鲜族发锰、发镁低于65岁、76岁组，朝鲜族发锌、发铜、发铁在65～108岁之间无统计学意义。     

Analytical strategies to determine antibiotic residues in fish

The accelerated growth of aquaculture has resulted in a series of harmful effects to human health. The widespread and unrestricted use of antibiotics in this industry, to prevent bacterial infections, leads to remaining amounts in the aquatic environment. This has resulted in the emergence of antibiotic-resistant bacteria in aquaculture environments, in the increase in antibiotic resistance in fish pathogens as well as in the transfer of these resistance determinants to human pathogens. Moreover, the use of large amounts of antibiotics may lead to the presence of residual antibiotics in fish tissue and fish products. Fluoroquinolones, tetracyclines, penicillins, sulphonamides and other antibiotics, exhibiting activity against both Gram-positive and Gram-negative bacteria, are widely used for the treatment and prevention of diseases in fish. An extended and comprehensive review on the recent analytical methodologies concerning antibiotic residues in fish reported in the literature is provided in the present article. Emphasis is given on sample preparation regarding isolation and purification, chromatographic conditions and method validation according to legislation. Results of published assays are comparatively presented and criticised.     

煤烘玉米和饮水为介质地氟病区骨畸形病人全血尿多元素含量的分析

采集了贵族个煤烘玉米为主要介质和河北２个饮水为介质氟病区内骨畸形病人的全血、尿、检测了其中８种元素含量,结果表明,贵州各氟病区少儿骨软化与成年骨硬化畸形病人的全血铝、钙、磷、铁和尿氟、铝均显著高于同龄对照组,尿磷均低于同龄对照组。少儿骨软化病人全血锌均下降,尿锌多下降。某水型氟病区骨软化经产妇尿氟、全血铜升高;骨软化少年全血铝显著升高,锌、铁下降,尿氟升高,尿锌,磷下降。海边的典型氟骨症病人全血、     

Calibration methods for microdialysis sampling in vivo: muscle and adipose tissue

Calibration methods for microdialysis sampling were studied in the muscle and adipose tissue of rats. Both the delivery method and the no-net-flux method were used to determine the extraction efficiency (EE) of acetaminophen and caffeine in both tissues. There was no concentration dependence of the EE either in vitro or in vivo for either acetaminophen or caffeine. The EEs determined by the delivery and no-net-flux methods were not different. However, the EEs of both caffeine and acetaminophen determined in vitro were significantly higher than those determined in the muscle and adipose. This indicates that mass transfer in the tissue is the rate-determining factor for the EE in vivo. The relative difference between the EE in vitro and the EE in the muscle was smaller than the difference between the EE in vitro and the EE in the adipose. In addition, the EE in the muscle decreased more than the EE in the adipose after the animal was euthanized. This indicated that exchange between the extracellular fluid and plasma is the rate-determining step in mass transport relative to microdialysis sampling. This has a more significant effect on the EE in the muscle than the EE in the adipose. Both the delivery and no-net-flux methods can be used to calibrate microdialysis probes in the muscle and adipose.     

Evaluation of the Fate of Aldicarb and Its Metabolites in Oranges

Abstract

The accumulation, persistence and fate of systemic pesticide aldicarb was melencholy evaluated in orange crops. The concentration of this pesticide and its two toxic metabolites, aldicarb sulfoxide and aldicarb sulfone was determined in leaves, rind and pulp of three orange varieties (Satsuma, Navelina and Clemetina de Nules) and in the top soil of the orange groves. The groves were located in two different places in the Valencia Community (Spain). The analysis showed that the aldicarb concentration was lower than those of aldicarb sulfoxide and aldicarb sulfone. In all cases, the residues persisted at least 160 days in vegetable samples and between 157 and 227 days in soil samples. Residue concentrations measured in the soil samples were highly variable but a relation with the organic matter content can be observed. The residue levels found in vegetal products were higher in leaves than in rind, and in rind than in pulp. The maximum residue values were obtained between 47 and 70 days after the application. One hundred days after treatment (Security period) the residue levels of total fruit were lower than the maximum residue level of 0.2 mg/kg established by law.     

Enantioselectivity Effects in Clinical Metabolomics and Lipidomics

Metabolomics and lipidomics have demonstrated increasing importance in underlying biochemical mechanisms involved in the pathogenesis of diseases to identify novel drug targets and/or biomarkers for establishing therapeutic approaches for human health. Particularly, bioactive metabolites and lipids have biological activity and have been implicated in various biological processes in physiological conditions. Thus, comprehensive metabolites, and lipids profiling are required to obtain further advances in understanding pathophysiological changes that occur in cells and tissues. Chirality is one of the most important phenomena in living organisms and has attracted long-term interest in medical and natural science. Enantioselective separation plays a pivotal role in understanding the distribution and physiological function of a diversity of chiral bioactive molecules. In this context, it has been the goal of method development for targeted and untargeted metabolomics and lipidomic assays. Herein we will highlight the benefits and challenges involved in these stereoselective analyses for clinical samples.     

环境中锑的分布、存在形态及毒性和生物有效性

由于自然过程及人类活动的影响,锑及其化合物在环境中普遍存在,环境中锑的污染也日益严重.近年来,国外对锑污染的研究日益重视.锑不是植物必需的,但能够被植物根系吸收.已有证据表明锑对生物及人体产生毒性.本文主要对环境中锑的分布和存在形态,及对动物和人体的毒性和对生物有效性研究进展进行评述。     

糖尿病患者治疗前后血细胞内液和血浆锌、铜、铁、镁和铷含量的研究

采用原子吸收分光光度计对６４名糖尿病患者血细胞内液和血浆中锌、铜、铁、镁、铷含量进行了测定．结果发现糖尿病组血细胞内液锌含量显著低于正常对照组（Ｐ＜０．０１），血细胞内液铁含量亦显著低于正常对照组（Ｐ＜０．０１），血浆铜含量显著高于正常对照组（Ｐ＜０．０１）．提示糖尿病患者锌、铁、铜的代谢方面均存在一定缺陷，认为糖尿病患者补充锌、铁元素，可能对治病有益处．     

Effects of dilute acid and steam explosion pretreatments on the cellulose structure and kinetics of cellulosic fraction hydrolysis by dilute acids in lignocellulosic materials

Worldwide, yellows diseases impact plants important in human nutrition, the natural environment, and the culture and commerce of humans. Since the presumed pathogens, mycoplasma-like organisms (MLOs), have not been isolated in pure culture in vitro, their study must proceed by other experimental approaches. In a study of disease affecting grapevines in Europe and North America, polymerase chain reactions (PCR) and restriction analyses of PCR-amplified DNA were used to detect and differentiate strains of MLOs associated with grapevine yellows. MLOs were detected both in naturally diseased grapevines and in experimentally inoculated host plants. The data indicated an unexpected genomic diversity among grapevine-infecting MLOs, and supported their classification with MLOs in the aster yellows, X-disease, and elm yellows groups. The presence of diverse MLOs in grapevines provokes consideration that these MLOs may be present in overlapping geographic ranges and that multiple MLO infections may occur in individual plants, increasing the complexity of grapevine yellows epidemiology and control and the significance of sensitive MLO detection in planting stock and phytosanitary-regulated germplasm.     

Contrasting Roles of Ang II and ACEA in the Regulation of IL10 and IL1β Gene Expression in Primary SHR Astroglial Cultures

Angiotensin (Ang) II is well-known to have potent pro-oxidant and pro-inflammatory effects in the brain. Extensive crosstalk between the primary Ang II receptor, Ang type 1 receptor (AT1R), and the cannabinoid type 1 receptor (CB1R) has been demonstrated by various groups in the last decade. Since activation of glial CB1R has been demonstrated to play a key role in the resolution of inflammatory states, we investigated the role of Ang II (100 nM) and/or ACEA (10 nM), a potent CB1R-specific agonist in the regulation of inflammatory markers in astrocytes from spontaneously hypertensive rats (SHR) and Wistar rats. Astrocytes were cultured from brainstems and cerebellums of SHR and Wistar rats and assayed for IL1β and IL10 gene expression and secreted fraction, in treated and non-treated cells, by employing qPCR and ELISA, respectively. mRNA expression of both IL10 and IL1β were significantly elevated in untreated brainstem and cerebellar astrocytes isolated from SHR when compared to Wistar astrocytes. No changes were observed in the secreted fraction. While ACEA-treatment resulted in a significant increase in IL10 gene expression in Wistar brainstem astrocytes (Log2FC ≥ 1, p < 0.05), its effect in SHR brainstem astrocytes was diminished. Ang II treatment resulted in a strong inhibitory effect on IL10 gene expression in astrocytes from both brain regions of SHR and Wistar rats (Log2FC ≤ −1, p < 0.05), and an increase in IL1β gene expression in brainstem astrocytes from both strains (Log2FC ≥ 1, p < 0.05). Co-treatment of Ang II and ACEA resulted in neutralization of Ang II-mediated effect in Wistar brainstem and cerebellar astrocytes, but not SHR astrocytes. Neither Ang II nor ACEA resulted in any significant changes in IL10 or IL1β secreted proteins. These data suggest that Ang II and ACEA have opposing roles in the regulation of inflammatory gene signature in astrocytes isolated from SHR and Wistar rats. This however does not translate into changes in their secreted fractions.