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101.
Three novel amphiphilic poly(ionic liquid) (PIL)/Wells–Dawson-type phosphovanadomolybdate (V-POM) ionic composites with tunable oxidative catalytic activity and unique nanostructure were synthesized using carboxylic acid-functionalized PIL and H7[P2Mo17VO62], H8[P2Mo16V2O62] and H9[P2Mo15V3O62] as synthetic units via self-assembly in water. The results of characterization indicated that V-POM anions were finely dispersed in the PIL cation framework, and their structures were well preserved. The three composites are amorphous V-POM salts of PIL cation with a considerable thermal stability, and an open three-dimensional network structure with hierarchical porosity. The as-synthesized composites were found to be efficient heterogeneous catalysts for the direct hydroxylation of benzene to phenol with H2O2 in the liquid phase. Under optimum conditions, a phenol yield of 37.3% was achieved with selectivity of 100%. The high catalytic performance could be attributed to the synergistic catalytic effect between V-POM anion and carboxylic acid-functionalized PIL cation framework, and good benzene adsorption and phenol desorption ability of amphiphilic micropores in the structure of the composites. Additionally, these composites exhibited high stability under the reaction conditions and could be easily recovered and reused at least six times without noticeably loss of activity. 相似文献
102.
S-Monofluoromethyl phosphorothioates represent an important class of organofluorine compounds and are re ported here for the first time.A series of S-monofluoromethyl phosphorothioates are conveniently synthesized from different PⅤ-H compounds and PhSO2SCH2F under mild conditions.The method is compatible with common functional groups and provides potential opportunities to synthesize new bioactive molecules for medicinal chemistry. 相似文献
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Quantification of complanatoside A in rat plasma using LC‐MS/MS and its application to a pharmacokinetic study
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Complanatoside A is a flavonol glycoside isolated from Astragalus complanatus, and currently it is used as a quality control index for A. complanatus in the 2010 edition of the Chinese Pharmacopoeia. For the first time, a simple and sensitive LC‐MS/MS method was developed for the determination of complanatoside A in rat plasma over the range of 2.3–575 ng/mL. Complanatoside A was extracted from plasma by a protein precipitation procedure, separated by LC and detected by MS/MS in positive electrospray ionization mode. The method was validated for selectivity, carryover, sensitivity, linearity, extraction recovery, matrix effect, accuracy, precision and stability studies. The lower limit of quantification was established at 2.3 ng/mL. Intra‐ and inter‐day precisions (LLOQ, low‐QC, med‐QC and high‐QC) were <7.9%, and accuracies were between 94.0 and 105.1%. Matrix effect was acceptable (97.9–103.0%) and extraction recovery was reproducible (88.5–94.4%). Complanatoside A was stable in the investigated conditions. The method was applied to the pharmacokinetics of complanatoside A in rats. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
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采用电感耦合等离子体原子发射光谱法(ICP-AES)法测定钛合金中W,Nb,Ta元素的含量。样品采用盐酸、氢氟酸和硝酸溶解,并对仪器工作参数和试验条件进行了优化试验,确定了仪器最佳工作条件,考察了钛合金基体和共存元素对待测元素的影响,确定了各待测元素谱线为W207.911nm,Nb309.418nm,Ta240.063nm。选定的待测元素分析线不受合金基体和共存元素的干扰,通过基体匹配消除基体的影响。加标回收率在98%104%之间,测定结果的相对标准偏差为0.3%~2.4%(n=8),方法的检出限为0.003-0.013μg/mL。进行了标准物质对照试验,试验结果与标准值相符。 相似文献
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A nitrite sensor based on Dawson vanodotungstophosphates α2-K7P2VW17O62·18H2O (P2W17V) and carbon nanotubes (CNTs) was prepared by electrostatic layer-by-layer self-assembly technique. The sensor {PEI/PSS/[PDDA/P2W17V-CNTs]n} was characterized by UV–vis spectroscopy, atomic force microscopy (AFM), scanning electron microscopy (SEM) and X-ray photoelectron spectra (XPS). The electron transfer and sensing ability of this sensor were explored using cyclic voltammetry (CV) and electrochemical impedance spectra (EIS) technology. The results show that the incorporation of CNTs and P2W17V into the composite film endowed the modified electrode with fast transfer rate and high electrocatalytic activity towards oxidation of nitrite. This nitrite sensor with 10 bilayers has a broad linear range of 5 × 10−8 to 2.13 × 10−3 M, a low detection limit of 0.0367 μM (S N−1 = 3), a high sensitivity of 0.35 mA mM−1 NO2−, an excellent anti-interference property in the presence of other potential interfering species and a good stable. It was successfully employed for determination of nitrite in real towards. 相似文献
110.
Peixu Zhang Yongri Jin Jiafeng Chen Hua Yao Hanqi Zhang Aimin Yu Xuwen Li 《Chromatographia》2013,76(15-16):967-974
In this work, a novel method based on ultrasonic-assisted nebulization extraction coupled with solid phase extraction (UANE-SPE) and determined by high performance liquid chromatography was developed for the determination of triterpenoids in root of Euphorbia pekinensis Rupr. The experimental conditions for the UANE-SPE, such as type of extraction solvent, sample amount, type and amount of sorbent, extraction time and volume of the elution solvent, were examined and optimized. The method was successfully applied to determine euphol and tirucallol in the dried root of E. pekinensis Rupr. The recoveries of the analytes were in the range of 89.1–102.0 %. The limits of detection were 12 μg g?1 for tirucallol and 10 μg g?1 for euphol. The extraction yields obtained by the proposed method are higher than those obtained by the conventional extraction methods, such as reflux and ultrasonic-assisted extraction. Compared with the traditional methods, the proposed method can reduce the consumption of the labor, shorten the sample preparation time and increase the efficiencies in the extraction of active constituents from plant materials. 相似文献