清除试剂在液相组合化学中的应用

综述了近年来清除试剂在液相组合化学中的应用,并介绍了一些采用清除试剂对液相化合物库进行分离和纯化的实例。对清除试剂进行了分类,各类清除试剂参与的液相反应以及被清除的非目标产物类型也作了相应的介绍。     

“树脂-捕获-释放”技术在有机合成中的应用

“树脂-捕获-释放”技术使用功能化聚合物清除剂选择性地吸附目标产物,液 相组合合成小分子化合物库。这一技术结合了固相和液相的优点,操作简便、快捷 ,反应容易控制,产物易分离,且产率高,纯度好。     

液相组合化学

综述了液相组合化学的研究进展，重点介绍了液相组合合成中的分离纯化方法和合成方法策略，基本分离纯化方法包括利用固相载体协助分离纯化法，相萃取分离纯化法和色谱法，主要合成方法策略有平行合成策略和索引合成策略。     

天然植物中生物碱的提取及树脂法在其纯化中的应用

总结了近期提取和分离纯化方法在天然植物中生物碱类有效成分研究中的应用,特别是对于吸附树脂法在生物碱纯化中的应用进行了系统综述,归纳了具有不同结构的大孔吸附树脂、凝胶型离子交换树脂和大孔型离子交换树脂对生物碱纯化效果的影响规律,进而为高效、高选择性纯化生物碱的专用吸附树脂结构设计和应用提供了可借鉴的研究思路.     

AB-8型大孔树脂分离提纯葛根素的研究

采用AB-8型大孔树脂对纯化葛根素的分离条件进行了研究,分别采用HPLC和薄层层析法研究了大孔树脂从葛根素粗品中分离葛根素的条件及影响因素。结果表明：采用AB-8型大孔树脂分离葛根素能够获得良好的分离效果。用大孔树脂分离葛根素具有操作简单、分离效果好等优点。     

利用离子液体负载反应底物的有机合成

综述了固相、液相组合化学中以可溶性离子液体为载体的有机合成新概念及最新研究进展,并主要介绍了离子液体作为载体负载反应底物在有机合成中的一些应用,如有关的重要有机反应、组合化学、小分子库合成等。该方法具有上载率高、适用反应范围宽、分离纯化简便、结构检测容易和可回收重复使用等诸多优越性,这对于传统的固相、液相合成方法是一个重大的进步。     

聚氯乙烯-漆酚树酯为载体的氟西汀化学传感器

１引言 盐酸氟西汀（ＦＸＨＣＩ）化学名Ｎ－甲基－γ－［４－（三氯甲基）苯氧基］苯丙胺盐，别名为氟苯氧丙胺、百解忧，是近期开发的抗抑郁药，它能高选择性地抑制神经元对５－羟色胶的再摄取，延长并增加５－羟色胺对受体的作用，主要适用于中度及重症抑郁症。其分析检测方法文献报道有高效液相色谱法、紫外分光光度法等，操作繁杂。本文以山漆（生漆）为原料，合成漆酚树脂，以此漆酚树脂为载体研制了测定ＦＸＨＣＩ的ＰＶＣ膜电位型化学传感器，用以测定口服ＦＸＨＣＩ丸剂，结果较为满意，且仪器价廉，操作快速简便。以电位型化学传…     

离子交换树脂纯化酪蛋白磷酸肽研究

通过单因素实验和正交试验确定了使用D-201型大孔强碱性阴离子交换树脂纯化酪蛋白磷酸肽(CPPs)的操作条件为：洗脱温度40℃、洗脱酸(HCI)浓度0．2mol／L、洗脱速度2．3ml／min、进样浓度2％(w／v)，进一步应用HPSEC技术分析考察了离子交换树脂纯化后含磷洗脱峰分子量分布情况，并计算了产品氮磷比与纯化收率．     

采用大孔型树脂除去照相明胶中微量Fe3+的研究

利用大孔树脂吸附和分离照相明胶中的微量铁，比较了6种树脂对微量铁的吸附效果，讨论了温度等因素对树脂吸附微量铁的影响．结果显示，D412大孔螯合树脂对铁的吸附效果较好；宜选用NaCl和络合剂EDTA混合溶液将树脂再生转化为Na型；采用D412大孔螯合型、732强硬型和711强碱型3种树脂的串联组合处理方式，除铁效率达50%-90％；容液pH值对Fe^3 在D412树脂上的吸附行为影响较小．     

PEG化的聚合物载体树脂研究进展

组合化学已成为发现和优化新药、亲和配体和催化过程中的重要组成部分.高分子载体树脂在组合化学中起着关键的作用,各种类型的聚合物树脂在有机合成中已被广泛开发为载体、反应物和催化剂.与传统的Merrifield树脂相比较,聚乙二醇(PEG)化的聚合物树脂具有与极性溶剂更好的相容性、更高的溶剂吸收和溶胀性能.本文主要综述与PEG相关联的聚合物树脂在有机合成载体领域中的最新成果.     

Solution-phase library synthesis of furanoses

The solution-phase synthesis of amido-, urea-, and aminofuranoses was achieved. Alkylated furanose aldehydes were treated with primary amines in the presence of sodium triacetoxyborohydride to give secondary amines. Subsequent acylation with acid chlorides and isocyanates afforded amidofuranoses and ureafuranoses, respectively. Second, reductive amination of furanose aldehydes with secondary amines yielded tertiary amines. The resulting acetonides were treated with alcohols in the presence of acid to yield mixed acetals. In the library syntheses, functionalized scavenger resins were used in the purification of intermediates and products.     

Resolution enhancement in hydrophobic interaction chromatography via electrostatic interactions

In this work, a new type of hydrophobic stationary phase that provide electrostatic interactions with analytes was developed by bonding β-phenylethylamine as a functional ligand to silica. This stationary phase can separate proteins with similar hydrophobicity that traditional hydrophobic resins cannot. Hen egg white was separated to examine the selectivity. The results show that the introduced electrostatic interactions are an important factor for the resolution enhancement and the new resin could have important applications in separation and purification of biological macromolecules.     

大孔吸附树脂结合酶解法分离纯化虎杖中白藜芦醇的研究

研究了大孔吸附树脂结合酶解法提取和纯化虎杖中白藜芦醇的方法,采用HPLC法测定虎杖中白藜芦醇的含量,考查了β-糖苷酶对虎杖药材酶解前后白藜芦醇含量的变化,并经静态吸附考察了4种树脂,最后确定以H1020作为提取分离白藜芦醇的树脂.此树脂吸附量较高,脱附容易,有利于得到质量较好的白藜芦醇产品,经该树脂吸附解吸,饱和吸附量可达51.4mg/g,解吸率达92.5%.大孔树脂分离纯化白藜芦醇的含量可达71.5%,而上柱前粗提物中白藜芦醇含量为8.71%,说明采用本法分离纯化虎杖中白藜芦醇是可行的.     

Simultaneous determination of components released from dental composite resins in human saliva by liquid chromatography/multiple-stage ion trap mass spectrometry

Dental composite resins are widely used for fixing teeth; however, the monomers used in dental composite resins have been found to be cytotoxic and genotoxic, namely triethylene glycol dimethacrylate (TEGDMA), urethane dimethacrylate (UDMA), and bisphenol A glycol dimethacrylate (Bis-GMA). In this study, we incubated dental composite resins with human saliva for demonstrating the released monomers and biodegradation products. A simple saliva sample dilution method without purification or derivatization was used for quantification. We found that liquid chromatography coupled with multiple-stage ion trap mass spectrometry (LC-MS(n) ) operated in selected reaction monitoring (SRM) mode was able to separate the three monomers within 10 min. The calibration curves were linear (R2 >0.996) over a wide range for each monomer in saliva: TEGDMA, 5-500 ppb; UDMA, 5-100 ppb, and Bis-GMA, 5-700 ppb. Furthermore, several biodegradation products were discovered with data-dependent MS/MS scan techniques. Although TEGMA degradation products have previously been reported, we identified two previously unknown UDMA degradation products. The LC-MS/MS method developed in this study was able to successfully quantify monomers and their principal biodegradation products from dental composite resins in human saliva.     

大孔离子交换树脂及新型吸附树脂的结构与性能

该项研究发现了大孔交联聚苯乙烯型离子交换树脂的合成方法,研究了惰性溶剂的性质与树脂的孔结构、树脂的孔结构与树脂的性能、树脂的特性与用途等方面的关系。在此基础上,研制出高强度、抗辐射、动力学性能优越的大孔型离子交换树脂,使其不仅能更好地应用于无机离子的交换,还开拓了在有机合成、制药等领域的催化、脱色、提纯等多方面的广泛应用。在多孔性离子交换树脂的基础上,还研制出系列吸附树脂。此类提取、分离材料,可以有不同的结构和不同的吸附性能,在天然产物的提取分离、抗菌素的提取、纯化、医疗、环境保护等领域有实际用途。上述两类功能高分子材料在多家企业实现了产业化,为化工、制药、环保、医疗、分析等诸多行业提供了必要的材料,在国民经济的发展中发挥了重要作用。     

MODIFICATION OF X-5 RESIN AND ADSORPTION PROPERTY OF THE MODIFIED RESINS

1. INTRODUCTION Adsorption capacity and selectivity are improved when some ion exchange groups or hydrogen bonding acceptor or/and donors are introduced into common polymeric adsorbents [1~5]. R. F. Shi et al have synthesized a series of bifunctional ads…     

Development of Methods for the Synthesis of Neopentyl Glycol by Hydrogenation of Hydroxypivaldehyde

Neopentyl glycol (NPG) is a precursor for the manufacture of many valuable products of industrial importance such as polyester, polyurethane and alkyd resins, synthetic lubricants, hydraulic fluids, drugs, etc. The structure of NPG provides the resins with excellent hydrolytic stability, resistance to weather conditions, good flexibility-hardness balance, and outstanding functional properties. The paper presents a literature review on the development of methods for NPG preparation, focusing primarily on the synthesis of NPG by hydrogenation of hydroxypivaldehyde, which is obtained by the crossed aldol condensation of isobutyraldehyde and formaldehyde. Preparation of the substrates, catalysts, technical and apparatus solutions, and NPG purification were discussed.     

Protein A chromatography: Challenges and progress in the purification of monoclonal antibodies

Antibodies for therapeutic use are being continuously approved and their demand has been steadily growing. As known, the golden standard for monoclonal antibody (mAb) purification is Protein A affinity chromatography, a technology that has gained high interest because of its great performance and capabilities. The main concerns are the elevated resins costs and their limited lifetime compared to other resins (e.g. ion exchange chromatography). Great efforts have been carried out to improve purification conditions, such as resin characterization and designing alkali/acid stable resins with a longer lifetime. Modification of Protein A ligands and alternative formats such as monoliths membranes and microshperes have been tested to increase the purification performance. New technology has been proposed to improve the large‐scale separation; in addition, alternative ligands have been suggested to capture mAbs instead of Protein A ligand; however, most of the information is locked by pharmaceutical companies. This mini review summarizes and describes the advances, results, and impact on the Protein A chromatography purification processing.     

Preparation of Low-dielectric Permittivity Polyimide Resins with High Surface Activity from Chemically Bonded Hyperbranched Polysiloxane

Thermosetting resin matrix is the key component of advanced wave-transparent composites,where low dielectric constant,excellent processability,high thermal stability,as well as good bonding ability are required for resins.Herein,we prepared a series of phenylethynyl terminated polyimide(PI)resins by grafting amine-functionalized hyperbranched polysiloxane(HBPSi)to PI chains during the in situ polymerization.The effects of HBPSi on the processability of oligomers,molecular packing,thermal stability,dielectric property and bonding ability to reinforce Kevlar fibers of the cured PI/HBPSi composite resins have been examined in detail.The dielectric constants of the cured composite resins were greatly reduced from 3.29 to 2.19 without compromising its processability and thermal stability.Meanwhile,the 10 wt％HBPSi-containing PI resin demonstrated better bonding ability to reinforce fibers with the interfacial shear strength(IFSS)of 37.64 MPa,compared with that of neat PI-6 matrix(27.34 MPa),and better adhesion to metal with the lap shear strength of 10.48 MPa,50％higher than that of neat resin PI-6(6.98 MPa).These resultant PI/HBPSi composite resins exhibit excellent comprehensive properties,indicating their great potential as low-dielectric constant resin matrix in radar radome.     

Purification of aqueous glyoxal from organic acids by ion exchange

A procedure for the purification of aqueous glyoxal (obtained by the partial oxidation of glycol) from carboxylic acids was described. Mono- and dibasic organic acids can be removed from solution without any substantial losses of glyoxal by using weakly basic EDE-10P and AN-31 anionites. A mechanism of the adsorption of carboxylic acids on weak resins was suggested based on the IR spectra recorded in a study of AN-31 anion-exchange resin. Using this method of purification also allowed the removal of the glyoxal condensation products from solution.