无机阴离子的毛细管电泳分析

本文研究了常见无机阴离子的毛细管电泳规律，考察了分离电压、电解质熔液组成、浓度、ｐＨ值等对分离的影响，建立了高效、快速的无机阴离子毛细管电泳分析方法。在选定的实验条件下，各种常见无机阴离子在５ｍｉｎ内达到完全分离，对Ｂｒ＾－和Ｃｌ＾－的分离柱效每米可达７６万理论板数。迁移时间的相对标准偏差小于１％，峰面积的相对标准偏差小于５％，各离子的最低检测浓度为０．０５￣０．５μｇ／ｍｌ。     

Surface modification by calcium ions—Effect on chromatographic properties of silica

Summary A liquid chromatographic method incorporating column-switching and fluorimetric detection for the determination of triamterene in untreated urine, is described. The urine samples (5 L) were directly introduced onto an Hypersil ODS-C18, 30 m (20 mm×2.1 mm I.D.) pre-column. Polar urinary compounds were removed by flushing the pre-column with water for 1 min, and the analyte was then switched onto an HP-LiChrospher RP C18,5 m (125 mm×4mm ID) analytical column using an acetonitrile/phosphate buffer gradient elution. Fluorescence detection was performed at 230 nm excitation and 430 nm emission wavelengths. The recovery of drug was 102±2% in the 0.10–20.0 g/mL concentration range, the limit of detection being 5 ng/mL. A validation of the usefulness of this procedure was accomplished by analysing urine extracts obtained from real samples.Hypersil ODS is not a product of Merck, Germany. Please give supplier (p. 5).     

烟叶和烟草料液中氨基酸的直接检测及碳水化合物的去除

建立了高效阴离子交换色谱-积分脉冲安培法(HPAEC-IPAD)直接检测烟叶和烟草料液中氨基酸的方法。利用离线除糖的方法,去除烟叶和烟草料液中大量干扰糖类,包括葡萄糖、果糖和蔗糖及麦芽低聚糖等。采用AminoPac PA10阴离子交换柱,以NaOH和NaAc的强碱性溶液为淋洗液,采用梯度洗脱,流速为0.25 mL/min;积分脉冲安培法对氨基酸进行检测,回收率可达76%~105%。此方法可以有效的解决烟叶、烟草料液等含糖量高的样品中糖类化合物的干扰,对氨基酸实现灵敏、准确的定量分析。     

金属元素在氢能利用过程中的作用

将金属元素分为主族、Ⅷ、镧系、其他d区等4个类别,综述了它们在氢气的生产、储存、氢燃料电池等3个氢能利用的主要过程中的作用。对现有研究结果的不完全统计表明,在元素周期表中除放射性金属元素之外的65种金属元素中,有46种金属元素以单质、合金、氧化物、盐等多种形式参与了氢能利用过程,包括作为载体、反应物、催化剂等,其中以铂系为代表的d区金属元素和以镧为代表的轻稀土金属元素应用最为广泛。     

A study for quality evaluation of Taxilli Herba from different hosts based on fingerprint-activity relationship modeling and multivariate statistical analysis

In this study, a fingerprint-activity relationship modeling between chemical fingerprints and antirheumatic activity was established, and multivariate statistical analysis was used to evaluate the quality of Taxilli Herba (TH) from different hosts. Characteristic fingerprints of 20 batches of TH samples were generated by high-performance liquid chromatography coupled with triple quadrupole-time of flight tandem mass spectrometry (HPLC-Triple TOF-MS/MS), and the similarity analysis was calculated based on thirteen common characteristic peaks by hierarchical clustering analysis (HCA). Subsequently, nine efficacy markers were discovered by combining fingerprints and antirheumatic activity through grey correlation analysis (GCA) and bivariate correlation analysis (BCA). Meanwhile, the content of 5 constituents in 9 markers was determined by high-performance liquid chromatography coupled with triple quadrupole-linear ion trap tandem mass spectrometry (HPLC-QTRAP-MS/MS). The comprehensive quality of TH was assessed using multivariate statistical analysis, including principal components analysis (PCA) and technique for order preference by similarity to ideal solution (TOPSIS). The results showed that a high dose of TH extract could markedly ameliorate arthritis damage compared to other doses, with flavonoids playing an important role in the antirheumatic activity. The comprehensive quality of samples from Morus alba L. (SS) was superior to those from Liquidambar formosana Hance (FXS). The present study will demonstrate the markers associated with efficacy, and provide an applicable strategy for more comprehensive quality control and evaluation of TH.     

Synthesis of novel soluble poly(imide-siloxane)s via hydrosilylation: Characterization and structure property behaviour

A series of novel poly(imide-siloxane)s (PIS) were synthesized by the grafting of amine terminated soluble imides to the siloxane backbone. The amine terminated imides were synthesized by choosing suitable anhydrides and amines to get the imides that are soluble in polar and non-polar solvents. The imides were grafted to the siloxane backbone by the epoxy group cleavage. All the polymers were obtained in quantitative yields with the inherent viscosities ranging from 0.22 to 1.2 dL g⁻¹. The polymers were characterized by FT-IR, ¹H and ¹³C NMR, and were examined for their thermal properties. The polymers were found to be stable up to a temperature 350 °C. The DSC results showed a single glass transition in the negative temperature, whereas the DTA revealed another glass transition in the positive end for some of the polymers showing phase separation. Polymer films were prepared employing the coupling reaction between PIS and the polydimethylsiloxane matrix by varying the amount of incorporation of PIS in the films. The polymer films had a tensile strength of 35-82 MPa with a percentage elongation of 86-271%. The contribution of polar and dispersion component towards the total surface energy was studied by the contact angle measurement and a reduction in surface tension of 14 mN m⁻¹ was achieved with the fluorine containing PIS membrane.     

On the cavitation energy of water

Free-energy-perturbation theory from molecular dynamics calculations has been used to obtain the DeltaG of adjoining cavities' formation in water. The DeltaGs for systems with three, five and seven cavities are compared with that of a single cavity of the same volume, and found to be in good agreement. The conditions under which the analytical formulation of the energy of cavity formation proposed by Pierotti holds are discussed. The data for a single cavity have been tabulated and can lend themselves to a simple numerical implementation in standard quantum chemical packages, which can be used when high accuracy for DeltaG(cav) is required.     

Analysis of carbohydrates using different quaternized polystyrene-divinylbenzene particles and pulsed amperometric detection

Summary This paper reports on the use of a polymer-based, strong anion-exchange stationary phase for rapid, selective and sensitive analysis of physiological important mono-, di- and oligosaccharides by high-performance anion-exchange chromatography (HPAEC) with pulsed amperometric detection (PAD) under alkaline conditions. The adsorbent was obtained by direct nitration of 3 and 5 μm, spherical non-porous highly cross-linked, styrene-divinylbenzene copolymer (PS-DVB) beads, followed by reduction of superficially introduced nitro groups with nascent hydrogen and quaternization of the resultant amino groups with iodomethane. Extended exposure to high pressure and strong alkaline conditions did not have any untoward effect on mechanical stability and chromatographic performance. A comparison of the 3 and 5 μm beads showed, that the synthesized 3 μm highly cross-linked PS-DVB particles are the preferred phases for the separation of monosaccharides and the 5 μm particles are preferable for the separation of oligosaccharides. To demonstrate the suitability for the analysis of complex samples, the optimized and validated system was used for the determination of glucose, fructose and sucrose in apple juice and other soft drinks such as Coca Cola. Finally, analysis within a few minutes without sample pretreatment down to a lower limit of detection of 0.174–0.504 μg mL⁻¹ at a linearity with R²>0.994 and a repooducibility higher than 98% further confirmed the efficiency of these polymeric sorbents.     

凝胶渗透色谱法测定聚丙烯腈共聚物分子量中宽分布校正法的应用

应用宽分布校正法对凝胶渗透色谱(GPC)进行了校正，将校正曲线用于聚丙烯腈(PAN)共聚物分子量的计算。对扣除色谱峰扩展效应前后的测试结果与乌氏粘度法测得的数据进行比较。结果表明，应用宽分布校正法时，必须扣除色谱峰扩展效应，才能得到较为准确的测试结果。     

从能源产业发展和人才需求浅谈“能源化学”新工科改造

Based on building emerging engineering education of "energy chemistry", we investigated the state key petro-chemical enterprises according to the industrial development and the demand of professional talents. The research report summarizes, analyzes and discusses the current priority development fields of industry, the talent training status, curriculum structure and education program of the chemistry and chemical engineering in universities. The ideas on emerging engineering education of "energy chemistry" have been proposed, and it will be beneficial to building a novel education program for talents training, which integrates the principle of chemistry, energy conversion and information science, etc.