Liquid Chromatograph Detector for Trace Analysis of Non-Volatile N-Nitroso Compounds

Abstract

A Thermal Energy Analyzer has been interfaced to a high performance liquid chromatograph. The hplc-TEA system can be used for analysis of nanogram amounts of N-nitroso compounds.     

三(4-甲基苯甲酰基)纤维素酯的合成及其涂敷手性固定相的制备和表征

以微晶纤维素为原料合成三（４－甲基苯甲酰基）纤维素酯,涂敷在平均粒径为６μｍ、平均孔径为１５ｎｍ、比表面积为６７ｍ２／ｇ的堆积硅珠上,制备成手性固定相。用扫描电子显微分析考察了固定相的表面形貌。用高效液相色谱法分离了（±）－α－苯乙醇对映异构体,考察了洗脱液正己烷／异丙醇（９８∶２,Ｖ／Ｖ）的流速和洗脱液的组成对（±）－α－苯乙醇对映异构体分离的影响。     

反相高效液相色谱法制备银杏叶中聚戊烯醇同系物单体

利用制备高效液相色谱法从银杏叶中分离制备了聚戊烯醇同系物单体。在HiQ sil C18柱上,以异丙醇-甲醇-正己烷-水(体积比为50∶25∶15∶4)为流动相,流速10 mL/min,采用等度洗脱方式,制备了8种化合物,经紫外光谱、红外光谱及质谱分析,确认它们分别为C70,C75,C80,C85,C90,C95,C100和C105聚戊烯醇,其中主要成分为C85及C90聚戊烯醇。高效液相色谱分析表明,制备的C75C105聚戊烯醇化合物的纯度均在96%(质量分数)以上。在该色谱条件下,各色谱峰达到了基线分离,     

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.     

基于HMM的机载设备状态健康评估方法研究

针对机载设备的状态健康评估问题,采用隐马尔科夫模型(HMM)对其进行性能退化程度的评估。首先引入状态条件概率矢量对HMM进行不确定性改进,并推导了其表达式;其次以状态条件概率比值为基础,给出了机载设备状态等级量化分值的计算方法,并据此设计了机载设备状态健康评估流程。最后以飞机发动机温控放大器为例进行仿真验证,结果表明上述方法能够给出直观、准确的状态评估结果。     

基于ANP-MCGC的装备保障性评价建模研究

从装备保障性满足装备保障能力及其执行任务能力的角度出发,对装备保障性评价内涵进行了界定,在综合考虑装备执行任务能力和保障能力生成过程的基础上,构建了装备保障性评价指标体系。针对评价指标的内部依存性及外部依赖性,采用网络分析法(ANP)及超级决策软件对评价指标体系进行赋权;针对评价过程中的模糊性和随机性,采用云重心评判法(MCGC)对装备保障性的评价。结果表明：此模型对装备保障性能够给出有效的综合评价,为装备保障性科学评价提供了一种适用有效方法。     

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.