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71.
建立了新型的解吸附电晕束离子源耦合离子阱质谱法(DCBI-MS),在无需复杂的样品前处理及色谱分离的条件下,可快速检测降血压中成药及保健食品中非法添加的7种β-受体阻滞剂阿替洛尔、比索洛尔、美托洛尔、普萘洛尔、盐酸塞利洛尔、盐酸贝凡洛尔和卡维地洛.采用一级质谱快速筛选和二级质谱确证的方法对目标化合物进行了定性和半定量测定.各目标物的检出限均低于0.1 mg/L,在0.5~100 mg/L浓度范围内线性关系良好.实验获得的7种β-受体阻滞剂的裂解规律为芳氧丙醇胺类化合物的质谱检测提供了参考依据.通过与高效液相色谱-电喷雾离子化质谱法(HPLC-ESI/MS)对比表明,DCBI-MS方法的检测结果可靠.对9种市售样品进行检测,有1批次中成药检出含有未标示的卡维地洛.结果表明,DCBI-MS法测定单个样品的时间不超过1 min,分析速度快,可以在大批量复杂基质样品中β-受体阻滞剂的筛查和药品品质的在线监测中发挥重要作用. 相似文献
72.
应用TG-FTIR技术研究黄土庙煤催化热解特性 总被引:1,自引:0,他引:1
用浸渍法制备过渡金属氧化物担载型催化剂MOx/USY(M=Co、Mo、Co-Mo),用热重红外联用技术考察了MOx/USY催化剂对黄土庙(HTM)煤热解失重特性和热解产物生成规律的影响。热重实验结果表明,MOx/USY催化剂可使HTM煤热解的二次脱气条件更为温和,热解峰温分别提前14、23和9℃。动力学分析结果表明,MOx/USY催化剂可降低HTM煤样热解的活化能。FT-IR研究表明,MOx/USY催化剂可有效改善HTM煤热解产物的组成和分布,CoOx/USY催化剂能显著提高HTM煤热解产物中高热值气体(CO、CH4)和轻质芳烃以及脂肪烃类化合物的含量;MoOx/USY催化剂没有明显改善HTM煤热解产物组成和分布;MoOx-CoOx/USY催化剂可促进CO、CH4、轻质芳烃和脂肪烃类化合物的生成,却使热解产物的生成向高温区移动,说明USY负载的不同过渡金属氧化物对煤样热解行为和热解产物有较大影响。 相似文献
73.
74.
Iulius I. E. Markovits Dr. Wilhelm A. Eger Dr. Shuang Yue Dr. Mirza Cokoja Christian J. Münchmeyer Bo Zhang Dr. Ming‐Dong Zhou Dr. Alexander Genest Prof. Dr. János Mink Prof. Dr. Shu‐Liang Zang Prof. Dr. Notker Rösch Prof. Dr. Fritz E. Kühn 《Chemistry (Weinheim an der Bergstrasse, Germany)》2013,19(19):5972-5979
Imidazolium‐based ionic liquids that contain perrhenate anions are very efficient reaction media for the epoxidation of olefins with H2O2 as an oxidant, thus affording cyclooctene in almost quantitative yields. The mechanism of this reaction does not follow the usual pathway through peroxo complexes, as is the case with long‐known molecular transition‐metal catalysts. By using in situ Raman, FTIR, and NMR spectroscopy and DFT calculations, we have shown that the formation of hydrogen bonds between the oxidant and perrhenate activates the oxidant, thereby leading to the transfer of an oxygen atom onto the olefin demonstrating the special features of an ionic liquid as a reaction environment. The influence of the imidazolium cation and the oxidant (aqueous H2O2, urea hydrogen peroxide, and tert‐butyl hydrogen peroxide) on the efficiency of the epoxidation of cis‐cyclooctene were examined. Other olefinic substrates were also used in this study and they exhibited good yields of the corresponding epoxides. This report shows the potential of using simple complexes or salts for the activation of hydrogen peroxide, owing to the interactions between the solvent medium and the active complex. 相似文献
75.
Shan Wang Dr. Haolong Li Shuang Li Fang Liu Dr. Dongqing Wu Prof. Dr. Xinliang Feng Prof. Lixin Wu 《Chemistry (Weinheim an der Bergstrasse, Germany)》2013,19(33):10895-10902
Herein, we present an electrochemically assisted method for the reduction of graphene oxide (GO) and the assembly of polyoxometalate clusters on the reduced GO (rGO) nanosheets for the preparation of nanocomposites. In this method, the Keggin‐type H4SiW12O40 (SiW12) is used as an electrocatalyst. During the reduction process, SiW12 transfers the electrons from the electrode to GO, leading to a deep reduction of GO in which the content of oxygen‐containing groups is decreased to around 5 %. Meanwhile, the strong adsorption effect between the SiW12 clusters and rGO nanosheets induces the spontaneous assembly of SiW12 on rGO in a uniformly dispersed state, forming a porous, powder‐type nanocomposite. More importantly, the nanocomposite shows an enhanced capacity of 275 mAh g?1 as a cathode active material for lithium storage, which is 1.7 times that of the pure SiW12. This enhancement is attributed to the synergistic effect of the conductive rGO support and the well‐dispersed state of the SiW12 clusters, which facilitate the electron transfer and lithium‐ion diffusion, respectively. Considering the facile, mild, and environmentally benign features of this method, it is reasonable as a general route for the incorporation of more types of functional polyoxometalates onto graphene matrices; this may allow the creation of nanocomposites for versatile applications, for example, in the fields of catalysis, electronics, and energy storage. 相似文献
76.
Sheng‐Run Zheng Xi‐Ling Wen Zi‐Meng Liu Tao Xie Jing‐Bo Tan Jun Fan Shuang‐Shuang Hou Wei‐Guang Zhang 《无机化学与普通化学杂志》2014,640(10):2057-2061
Two coordination polymers (CPs), namely, [Cu(Hptz)2(Hhba)2]n ( 1 ) [Hptz = 5‐(4‐pyridyl)‐1H‐tetrazole, H2hba = 2‐hydroxybenzoic acid] and [Zn3(ptz)2(hpa)2]n ( 2 ) (H2hpa = 2‐hydroxy‐2‐phenylacetic acid), were synthesized by solvothermal reactions. Both complexes were characterized by elemental analysis, infrared spectroscopy, powder X‐ray diffraction, thermogravimetric analysis, and single‐crystal X‐ray diffraction analysis. Compound 1 exhibits a 2D (4,4) network, where each layer connects to four adjacent layers to construct a 3D supramolecular framework. Compound 2 has a 3D framework structure composed of 1D SUBs, which are formed by both carboxyl and tetrazole groups. The complexes represent two rare examples of CPs constructed from Hptz and organic carboxyl acid ligands. Complex 2 exhibits intense, red‐shifted emissions in the visible region at room temperature. 相似文献
77.
78.
Graphene‐sensitized microporous membrane/solvent microextraction for the preconcentration of cinnamic acid derivatives in Rhizoma Typhonii 下载免费PDF全文
A novel graphene‐sensitized microporous membrane/solvent microextraction method named microporous membrane/graphene/solvent synergistic microextraction, coupled with high‐performance liquid chromatography and UV detection, was developed and introduced for the extraction and determination of three cinnamic acid derivatives in Rhizoma Typhonii. Several factors affecting performance were investigated and optimized, including the types of graphene and extraction solvent, concentration of graphene dispersed in octanol, sample phase pH, ionic strength, stirring rate, extraction time, extraction temperature, and sample volume. Under optimized conditions, the enrichment factors of cinnamic acid derivatives ranged from 75 to 269. Good linearities were obtained from 0.01 to 10 μg/mL for all analytes with regression coefficients between 0.9927 and 0.9994. The limits of quantification were <1 ng/mL, and satisfactory recoveries (99–104%) and precision (1.1–10.8%) were also achieved. The synergistic microextraction mechanism based on graphene sensitization was analyzed and described. The experimental results showed that the method was simple, sensitive, practical, and effective for the preconcentration and determination of cinnamic acid derivatives in Rhizoma Typhonii. 相似文献
79.
Shu-hua Yao Shuang Chen Zhong-liang Shi 《化学物理学报(中文版)》2014,(3):343-349
A series of Ce, H3PW12O40 co-doped TiO2 hollow fibers photocatalysts have been prepared by sol-gel method using ammonium ceric nitrate, H3PW12O40 and tetrabutyltitanate as precursors and cotton fibers as template, followed by calcination at 500 ℃ in N2 atmosphere for 2 h. Scanning electron microscopy, X-ray diffraction, nitrogen adsorption-desorption mea- surements, and UV-Vis spectroscopy are employed to characterize the morphology, crystal structure, surface structure, and optical absorption properties of the samples. The photo- catalytic performance of the samples has been studied by photodegradation phenol in water under UV and visible light irradiation. The results show that the TiO2 fiber materials have hollow structures, and the co-doped TiO2 hollow fibers exhibit higher photocatalytic activities for the degradation of phenol than un-doped, single-doped TiO2 hollow fibers under UV and visible light. In addition, the recyclability of co-doped TiO2 fibers is also confirmed that the TiO2 fiber retains ca. 90% of its activity after being used four times. It is shown that the co-doped TiO2 fibers can be activated by visible light and may be potentially applied to the treatment of water contaminated by organic pollutants. The synergistic effect of Ce and H3PW12O40 co-doping plays an important role in improving the photocatalytic activity. 相似文献
80.
M. Q. Mehmood Hong Liu Kun Huang Shengtao Mei Aaron Danner Boris Luk'yanchuk Shuang Zhang Jinghua Teng Stefan A. Maier Cheng‐Wei Qiu 《Laser \u0026amp; Photonics Reviews》2015,9(6):674-681
This work presents analytical, numerical and experimental demonstrations of light diffracted through a logarithmic spiral (LS) nanoslit, which forms a type of switchable and focus‐tunable structure. Owing to a strong dependence on the incident photon spin, the proposed LS‐nanoslit converges incoming light of opposite handedness (to that of the LS‐nanoslit) into a confined subwavelength spot, while it shapes light with similar chirality into a donut‐like intensity profile. Benefitting from the varying width of the LS‐nanoslit, different incident wavelengths interfere constructively at different positions, i.e., the focal length shifts from 7.5 μm (at λ = 632.8 nm) to 10 μm (at λ = 488 nm), which opens up new opportunities for tuning and spatially separating broadband light at the micrometer scale.