Synthesis of monodisperse poly(chloromethylstyrene-co-divinylbenzene) beads and their application in separation of biopolymers

The monodisperse, porous poly(chloromethylstyrene-co-divinylbenzene) beads of 7.9 microm were prepared by a single-step swelling and polymerization method. The seed particles prepared by dispersion polymerization exhibited good absorption of the monomer phase. Based on this media, a weak cation-exchange (WCX) stationary phase for HPLC was synthesized by a new chemically modified method. The prepared resin has advantages of biopolymer separation, high column efficiency, low column backpressure, high protein mass recovery, and good resolution for proteins. The dynamic protein-loading capacity of the synthesized WCX packings was 18.2 mg/g. Five proteins were separated in 3.0 min using the synthesized WCX stationary phase. The experimental results show that the obtained WCX resin has very weak hydrophobicity. The WCX resin was also used for the rapid separation and purification of lysozyme from egg white in 5.0 min with only one step. The purity and specific bioactivity of the purified lysozyme were found to be more than 93% and 70 245 U/mg, respectively.     

四（对羟基苯基）卟啉—硅胶固定相的合成及在核苷酸分析中的应用

以大孔微硅胶作基体，经γ－氨丙基三乙氧基硅烷活化与间隔臂氯代环内烷反应后，再与预先合成的四（对羟基苯基）卟啉配体键合，构成电荷转移型亲和色谱固定相。以ＰＨ＝７．０的磷酸盐缓冲溶液作流动相，成功实现对一些核苷酸的高效液相亲和色谱分离。     

Analysis of preservatives in cosmetics—Methylisothiazolones

Summary Antimicrobially active formulations based on 2-methyl-3(2H)-isothiazolone and 5-chloro-2-methyl-3(2H)-isothiazolone (Kathon CG, Euxyl K 100) are incorporated into manufactured cosmetics as preservatives. In this paper we report on the analysis of these active components by means of liquid chromatography. It is conventional for the original methylisothiazolone components in cosmetics to be analyzed by reversed phase high-performance liquid chromatography after column chromatographic separation and flash chromatographic purification. In our new analytical method the methylisothiazolones are converted into the respective -thiosubstituted acrylamide derivatives, which are ionic substances, with the help of the nucleophilic reagent hydrogensulfite. An ion pair high-performance liquid chromatographic method has been developed for the separation and quantification of these derivatives.     

Enantioseparation of Novel Chiral Tetrahedral Clusters on a Chiral Stationary Phase (CSP) by High Performance Liquid Chromatography

In recent years, the synthesis of chiral tetrahedral clusters has been studied extensively and various types are accessible , which are a kind of organometallic compounds with greatly growing interest due to their potential application to asymmetric reaction catalysts. As an efficient     

亲和标记-基质辅助激光解吸电离飞行时间质谱用于蛋白质相对定量方法的研究

将亲和标记技术和基质辅助激光解吸电离飞行时间串联质谱联用,建立了蛋白质相对定量方法,以牛血清白蛋白为实验对象,考察了该方法的准确度、重现性等指标;又以数种标准蛋白混合物为研究对象,考察了该方法的动态范围及相应的标准偏差,为实际生物样品中差异蛋白质分析奠定了基础。     

环境样品中痕量邻苯二甲酸酯的分离与测定

本文研究了以小粒径（１０－４０μ）硅胶柱色谱分离富集、反相高效相色谱分析测定大气颗粒物、土主植物样品中痕量邻苯二甲酸酯的方法，方法操作简单，回收率高，空白值低，利用该方法分析了部分环境样品中邻苯二甲酯酯含量。     

聚2,6-二甲基苯醚树脂分子量分布及其与冲击强度关系的研究

本工作建立了室温下用凝胶色谱法(GPC)测定聚2,6-二甲基苯醚(PPO)树脂分子量、分子量分布的方法。淋洗剂不采用文献申报道的毒性较大者,也不在较高柱温下进行,而采用甲苯(或氯仿)在室温下测定。对样品在甲苯中溶解温度、浓度和稳定性等都进行了系统研究,找到了最优化条件。GPC数据结合改性PPO(MPPO)产品性能测定结果,经仔细分析找到了影响MPPO产品质量的一个重要因素是PPO树脂中低分子量部分含量。它与产品冲击强度有明显的依赖关系。提出了一个从CPC谱图确定低分子量部分含量的方法。     

Use of Two-Dimensional Liquid Chromatography Combined with Diode-Array and Mass Spectrometric Detection for Analysis of Compounds in Flos Lonicera

Comprehensive two-dimensional liquid chromatographic separation by means of a combination of ion-exchange chromatography (IEC) and reversed-phase liquid chromatography (RPLC) has been realized and applied to the analysis of components of a traditional Chinese medicine Flos Lonicera. In the first dimension the components of a Flos Lonicera extract is separated on strong anion-exchange (SAX) column according to the charge-exchange properties of the components. In the second dimension the components are further fractionated by reversed-phase liquid chromatography (on ODS) on the basis of their hydrophobicity. The RPLC effluent is desalted and split and the components are identified on-line by use of both diode-array detection and mass spectrometry with atmospheric pressure chemical ionization (APCI–MS). In this way, the extract of Flos Lonicera can be rapidly separated, desalted, and analyzed, with determination of molecular weight. More than 58 components of an extract of Flos Lonicera were well resolved and six were tentatively identified from their UV and mass spectra.     

离子色谱法同时测定水中六种阳离子

研究了用抑制电导离子色谱法一次进样同时测定水中Li^ ,Na^ , NH4^ ,Mg^2 ,Ca^2 的色谱法条件，相对标准偏差小于0．5％，加标回收率在97．5％－104．0％。在水质分析中运用t检验法，比较了用钙、镁离子浓度计算和传统方法测定的总硬度之间是否存在显著性差异。     

Concentration and clean-up of trace hydrocarbons from atmospheric particulate matter

Summary The aim of this work is to establish the best conditions for concentration and purification steps in the trace analysis of aliphatic and polycyclic aromatic hydrocarbons (PAH) from atmospheric particulate matter by gas chromatography-flame ionisation detection (GC-FID) and high performance liquid chromatography with ultraviolet and fluorescence detection (HPLC-UV-FL). The best results for the more volatile compound were obtained with a combination of rotary evaporation and a stream of nitrogen (near to 100% for aliphatic hydrocarbons and from 70 to 105% for PAH). Two types of solid phase extraction (SPE)cartridges (Supelclean ^tm LC-Silica SPE tubes and Sep-Pak^? Plus silica cartridges) and glass column were examined for the purification and fractionation step. Blank chromatograms of both types of cartridges analysed by GC-FID made this study difficult, because a PSS (programmed split-splitless) injector was employed thereby increasing the sensitivity. This problem was not observed in the HPLC-UV-FL blank chromatograms of these cartridges. Glass columns filled with silica and alumina were chosen because no interference was found in the GC-FID blank chromatograms and the best recoveries in the fractionation of both aliphatic hydrocarbons and PAH were achieved. This is especially important when aliphatic hydrocarbons concentrations are lower than 1 μg mL⁻¹. Finally, the selected conditions were applied to the analysis of hydrocarbons in real atmospheric particulate samples.