黄芩中黄芩苷的亚临界水提取及高效液相色谱分析

建立了黄芩药材中黄芩苷的亚临界水提取 高效液相色谱测定方法。分别考察了温度、压力、提取时间、提取物颗粒度、溶剂比等因素对提取量的影响,并与有机溶剂提取法比较。结果表明,当两者具有相同的提取效果时,亚临界水提取法的提取时间及提取溶剂的消耗量大大减少,避免了使用有机溶剂造成的污染。黄芩苷提取最佳条件为:样品颗粒度80～100目,溶剂比0.2 mL/mg ,5 MPa,130 ℃保持10 min。并通过提取 高效液相色谱联机分析实现了对提取物的实时监测。该技术有望成为从中药材中提取脂溶性成分的有效方法。     

Precise Design of Millimeter Wave Quasi-Optical Faraday Rotators

A method of designing high performance millimeter wave quasi-optical Faraday rotators (QOFR) is reported in this paper. First, the dielectric and magnetic parameters for the ferrite sample are determined by fitting theoretical curves to the measured data. These fitted parameters are then used in a precise numerical model to predict the rotation angle and insertion loss of the QOFR. Finally, the parameters of the QOFR are optimized according to the requirements of devices. Examples are given showing the performance of the QOFR with an isolation better than 20 dB and an insertion loss less than 0.6 dB from 75 GHz to 95 GHz.     

Microstructure,Tribological Behavior,and Corrosion-Resistant Performance of Bonded MoS2 Solid Lubricating Film Filled with Nano-LaF3

The anti-friction and wear-resistant performances of bonded MoS₂ solid lubricating films filled with nano-LaF₃ filler were investigated under in drying wear conditions, the corrosion-resistant performances of bonded lubricating films was evaluated according to ASTM-B117, and the characteristics of the bonded lubricating films were examined by TEM and elemental x-ray map. The wear-resistant performance of the bonded lubricating films filled with nano-LaF₃ filler increases with increasing content of nano-LaF₃ filler within a content range between 0 and 5 wt%, whereas the bonded lubricating films filled with 0.5–1 wt% micro-LaF₃ filler exhibit the better wear-resistant performances. The incorporation of both nano-LaF₃ and micro-LaF₃ filler leads the increase of the coefficient of friction of the bonded lubricating films. The LaF₃ filler can improve the corrosion-resistant performance of the bonded MoS₂ solid lubricating films, whereas the incorporation of nano-LaF₃ filler is more effective to improve the corrosion-resistant performance of the bonded lubricating films than micro-LaF₃ filler. The improvement in the wear-resistant and corrosion-resistant performances of the bonded lubricating films by the incorporation of the nano-LaF₃ filler is attributed to the strengthened interfacial bonding among the nano-LaF₃ and the MoS₂ lubricant and the polymeric matrix. However, a too high mass fraction of the nano-LaF₃ filler in the bonded lubricating films will increase surface and interface defects, and lead the worsening of corrosion-resistant performance of the bonded lubricating films.     

Effects of Magnetic Nanofluid Fuel Combustion on the Performance and Emission Characteristics

Although the compression ignition engines are a significant source of power, their detrimental emissions create considerable problems to the environment as well as to humans. The objective of the present experimental investigation is to examine the effects of the magnetic nanofluid fuels on combustion performance characteristics and exhaust emissions. In this regard, the Fe₃O₄ nanoparticles dispersed in the diesel fuel with the nanoparticle concentrations of 0.4 and 0.8 vol% were employed for combustion in a single-cylinder, direct-injection diesel engine. After a series of experiments, it was demonstrated that the nanoparticle additives, even at very low concentrations, have considerable influence in diesel engine characteristics. Furthermore, the results indicated that the nanofluid fuel with nanoparticle concentration of 0.4 vol% shows better combustion characteristics in comparison with that of 0.8 vol%. Based on the experimental results, NO _x and SO₂ emissions dramatically reduce, while CO emissions and smoke opacity noticeably increase with increasing the dosing level of nanoparticles.     

Rapid quantitative analysis of individual anthocyanin content based on high‐performance liquid chromatography with diode array detection with the pH differential method

A new quantitative technique for the simultaneous quantification of the individual anthocyanins based on the pH differential method and high‐performance liquid chromatography with diode array detection is proposed in this paper. The six individual anthocyanins (cyanidin 3‐glucoside, cyanidin 3‐rutinoside, petunidin 3‐glucoside, petunidin 3‐rutinoside, and malvidin 3‐rutinoside) from mulberry (Morus rubra) and Liriope platyphylla were used for demonstration and validation. The elution of anthocyanins was performed using a C₁₈ column with stepwise gradient elution and individual anthocyanins were identified by high‐performance liquid chromatography with tandem mass spectrometry. Based on the pH differential method, the high‐performance liquid chromatography peak areas of maximum and reference absorption wavelengths of anthocyanin extracts were conducted to quantify individual anthocyanins. The calibration curves for these anthocyanins were linear within the range of 10–5500 mg/L. The correlation coefficients (r²) all exceeded 0.9972, and the limits of detection were in the range of 1–4 mg/L at a signal‐to‐noise ratio ≥5 for these anthocyanins. The proposed quantitative analysis was reproducible with good accuracy of all individual anthocyanins ranging from 96.3 to 104.2% and relative recoveries were in the range 98.4–103.2%. The proposed technique is performed without anthocyanin standards and is a simple, rapid, accurate, and economical method to determine individual anthocyanin contents.     

Simultaneous determination of four sedative-hypnotics in human urine based on dendritic structured magnetic nanomaterials

A magnetic solid-phase extraction technique based on magnetic dendritic structured nanoparticles (Fe₃O₄@SiO₂-NH₂-G5) as adsorbent coupled with ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) has been developed to detect diazepam, midazolam, zolpidem, and zaleplon in human urine. With Fe₃O₄@SiO₂-NH₂ as the central core, dendrimer (G5) grafted alternately with cyanuric chloride and imidazole were bonded to the surface of the core to synthesize Fe₃O₄@SiO₂-NH₂-G5. The morphology and structure of the magnetic materials were characterized by transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), and dynamic light scattering (DLS). The key parameters affecting the extraction efficiency were optimized. A satisfactory performance was obtained under the optimum extraction conditions. The proposed method was validated, and the limits of detection of zaleplon, diazepam, zolpidem, and midazolam were 0.05, 0.05, 0.02, and 0.02 ng mL^?1, respectively. The linear correlation coefficients r of the four analytes were > 0.996, the intra-day precision was between 2.4 % and 9.4 % with the recoveries between 88.3 % and 104.8 %, and the inter-day precision ranged from 3.9 % to 15.2 % with the recovery in the range of 94.1 %?108.3 %. The magnetic dendritic structure nanomaterial Fe₃O₄@SiO₂-NH₂-G5 was successfully used to extract sedative-hypnotic drugs from human urine samples. The Fe₃O₄@SiO₂-NH₂-G5-based magnetic solid-phase extraction method eliminates centrifugation and filtration steps as in conventional extraction. Only one step of vortex dispersion extraction could achieve the separation and purification of the target compounds. The proposed method was simple, rapid, environment-friendly, and suitable for the analysis of sedative-hypnotic drugs in human urine.     

Upgrading Solid Digestate from Anaerobic Digestion of Agricultural Waste as Performance Enhancer for Starch-Based Mulching Biofilm

Developing a green and sustainable method to upgrade biogas wastes into high value-added products is attracting more and more public attention. The application of solid residues as a performance enhancer in the manufacture of biofilms is a prospective way to replace conventional plastic based on fossil fuel. In this work, solid digestates from the anaerobic digestion of agricultural wastes, such as straw, cattle and chicken manures, were pretreated by an ultrasonic thermo-alkaline treatment to remove the nonfunctional compositions and then incorporated in plasticized starch paste to prepare mulching biofilms by the solution casting method. The results indicated that solid digestate particles dispersed homogenously in the starch matrix and gradually aggregated under the action of a hydrogen bond, leading to a transformation of the composites to a high crystalline structure. Consequently, the composite biofilm showed a higher tensile strength, elastic modulus, glass transition temperature and degradation temperature compared to the pure starch-based film. The light, water and GHG (greenhouse gas) barrier properties of the biofilm were also reinforced by the addition of solid digestates, performing well in sustaining the soil quality and minimizing N₂O or CH₄ emissions. As such, recycling solid digestates into a biodegradable plastic substitute not only creates a new business opportunity by producing high-performance biofilms but also reduces the environmental risk caused by biogas waste and plastics pollution.     

The Effects of a Third Generation Combined Oral Contraceptive Pill on the Classical Singing Voice

The success of professional operatic singers depends upon the quality of their vocal mechanism. This is known to be sensitive to changes in the endocrine environment. Despite a widespread belief among singers that vocal quality changes according to the stage of the menstrual cycle, this has received little attention. In particular, the possibility that use of the contraceptive pill might stabilize vocal quality by "dampening" hormonal fluctuations has not previously been studied systematically. Here, we show that drospirenone containing oral contraceptive pill (Yasmin, Schering AG, West Sussex, UK) with antiandrogenic and antimineralocorticoid properties demonstrates a significant reduction in the irregularity of the pattern of vibration of the vocal folds during the performance of highly trained classical singers. This study constitutes the first double blind, randomized placebo controlled trial to assess the effects of the contraceptive pill on the patterns of vibration of the vocal folds during the performance of Western classical singing repertoire.     

Correlation of the loss in photovoltaic module performance with the ageing behaviour of the backsheets used

The influence of the type of backsheet on the electrical performance of test modules was evaluated before and after increasing time of accelerated ageing (damp heat [DH] exposure). Besides the measurement of the electrical power of the modules and the performance of the cells by electroluminescence, the ageing‐induced changes within the polymeric encapsulate and backsheets were investigated by means of vibrational spectroscopy and by thermo analytical methods. In addition, the permeability of the backsheets in the original and aged state was determined. This wide set of test parameters and methods allowed for the detection of correlations between (i) physical and chemical properties as well as their ageing‐induced changes of the materials and (ii) the module performance. A clear dependence of the relative loss in power output upon exposure under DH conditions for 2000 h could be observed for a set of identical test modules varied in composition only in the type of back cover used. While the modules containing gas‐tight backsheets and glass experienced only little loss in the relative power output, some modules with permeable backsheets showed a significant relative decrease in the power output and fill factor in dependence of the backsheet type used. Cell degradation could be visualised by recording electroluminescence images before and after the accelerated ageing test. The permeation properties of the backsheet used and their ageing‐induced changes seem to have an influence on the module performance. However, the absolute values neither of the water vapour transmission rate (WVTR) nor of the oxygen transmission rate (OTR) are directly linked to the loss in power output upon accelerated ageing under DH conditions. It could be shown that the ageing‐induced changes (relative transmission rates) between WVTR and OTR can be correlated with the module performance. These ageing‐induced changes in the permeation behaviour of the backsheets can be explained by (i) physical changes (e.g. post‐crystallisation, changes in the crystal structure or the crystalline microstructure) and (ii) chemical ageing effects such as a decrease in the molecular mass of the polyester (PET) polymer chains because of hydrolytic polymer degradation leading to a change in the crystallisation behaviour of PET. Hydrolytic degradation (= chemical ageing) of the PET core layer was observed (with varying extent) for all PET‐based backsheets and can, thus, not be directly correlated with the loss in performance of the corresponding test modules. The physical ageing effects, however, were detected only for those backsheets showing (i) strong deviating changes in the relative permeation rates for oxygen and water vapour upon accelerated ageing and (ii) a clear loss in electrical performance. Copyright © 2015 John Wiley & Sons, Ltd.     

Porous Tantalum Nitride Single Crystal at Two-Centimeter Scale with Enhanced Photoelectrochemical Performance

Porous tantalum nitride (Ta₃N₅) single crystals, combining structural coherence and porous microstructure, would substantially improve the photoelectrochemical performance. The structural coherence would reduce the recombination of charge carriers and maintain excellent transport properties while the porous microstructure would not only reduce photon scattering but also facilitate surface reactions. Here, we grow bulk-porous Ta₃N₅ single crystals on a two-centimeter scale with (002), (023), and (041) facets, respectively, and show significantly enhanced photoelectrochemical performance. We show the preferential facet growth of porous crystals in a lattice reconstruction strategy in relation to lattice match and lattice channel. We present the facet engineering to enhance light absorption, exciton lifetime and transport properties. The porous Ta₃N₅ single crystal boosts photoelectrochemical oxidation of alcohols with the (002) facet showing the highest performance of >99 % alcohol conversion and >99 % aldehyde/ketone selectivity.