攀枝花A型正长岩体的成因及构造意义

攀枝花正长岩体与含超大型钒钛磁铁矿矿床的辉长岩体在空间上共生、侵位时间近于一致，均为晚古生代峨眉山地幔柱岩浆活动的产物。该正长岩岩体由成分连续的中酸性侵入岩组成并伴生酸性喷出岩和正长斑岩。本研究以攀枝花正长岩体及相关的酸性岩石为研究对象，在较为系统的矿物化学、主量元素、微量元素和Sr-Nd同位素等方面研究基础上，并结合前人的相关研究成果，探讨了该岩体的岩浆演化过程、成因及其对于地幔柱活动条件下地壳演化机制的指示意义。本文取得的主要认识如下： （1）岩体中的闪长岩由中酸性斜长石、普通辉石、铁橄榄石等组成。正长岩由条纹长石、钠长石、普通辉石、Na-Ca和Ca角闪石等组成。石英正长岩主要矿物为条纹长石、石英。碱性花岗岩由条纹长石、石英、普通辉石和Na和Na-Ca角闪石构成。相关的正长斑岩的斑晶为微斜长石和钠长石，基质主要由条纹状的微斜长石、钠长石、石英、黑云母、磷灰石组成。伴生粗面岩的斑晶为钠长石、石英和普通辉石。流纹岩的斑晶为条纹长石和石英，基质有钠长石、钾长石、Na角闪石。 （2）矿物化学特征显示，从中性岩到酸性岩，长石向贫Ca，富Na、K趋势演化；普通辉石向贫Mg，富Fe、Na、Ca趋势演化；角闪石向贫Ca、Mg，富Fe、Na趋势演化。因此，不同类型岩石中矿物的成分变化主要受母岩浆的结晶分异作用控制。 （3）元素地球化学研究表明，攀枝花正长岩体富含高场强元素和具高Ga/Al比值，显示典型A型花岗质岩石的特征。Nb/Ta、Zr/Hf比值与OIB源区的相应比值接近表明岩体中不同类型岩石来自同一地幔源区。 （4）攀枝花正长岩体中各类岩石具有一致的Sr、Nd同位素组成，表明其母岩浆来源相似。该正长岩体主要源于两种不同的正长质熔体，由与峨眉山地幔柱有关的底侵弱碱性玄武岩浆在地壳深部经分异产生。这两类正长岩浆在地壳浅部岩浆房进一步经历分离结晶作用并最终形成闪长岩、正长岩、正长斑岩、石英正长岩和花岗岩，部分岩浆喷出地表形成粗面岩、流纹岩。 （5）本研究认为巨量的玄武质岩浆底侵于下地壳是峨眉山大火成岩省内带A型花岗岩体形成的必要前提。晚古生代峨眉山地幔柱活动对于大火成岩省内带的地壳垂向增生起到极为重要的作用。

岩浆－热液过渡阶段体系中不相容元素地球化学行为及其机制－以新疆阿尔泰3号伟晶岩脉研究为例

伟晶岩形成和演化中岩浆-热液过渡阶段物理化学性质、过铝质富挥发分岩浆体系岩浆液相不混溶、流体相出溶事件的相对时间尺度以及在岩浆-热液过渡阶段体系中稀土和其它微量元素地球化学行为(稀土“四重效应”机制和微量元素分异及控制因素等)是目前过铝质岩浆体系研究的焦点问题。对上述问题的研究和探讨，将有助于了解伟晶岩形成和演化的全过程，有助于了解挥发分(H_20、F、B、P)对过铝质岩浆体系物理性质以及对REE和其它微量元素地球化学行为影响，这对于理解过铝质岩浆体系成岩、成矿作用过程具有重大的理论和实际意义。本论文选择著名的新疆阿尔泰3号伟晶岩脉为研究对象，由于它具有完美的分带特征，使我们有可能通过各结构带矿物学、地球化学的研究揭示伟晶岩成因和演化过程以及讨论岩浆-热液过渡阶段体系中的稀土和微量元素地球化学行为。由于LCT型伟晶岩具有明显的分带性、矿物颗粒大小不均匀性等特点，因此利用全岩样品研究伟晶岩往往因取样没有代表性而被大多数岩石学家和地球化学家所否定。考虑到这点，本文系统采集阿尔泰3号伟晶岩脉各结构带磷灰石、电气石、碱性长石、石英矿物，部分结构带的石榴石、绿柱石、锂辉石矿物以及伟晶岩冷凝边和蚀变围岩的全岩样品，通过各结构带磷灰石矿物化学组成和~(87)Sr／~(86)Sr比值测定，电气石矿物的化学组成和硼同位素组成分析，碱性长石中磷含量的电子探针分析和碱性长石-石英矿物对的氧同位素体系研究以及蚀变围岩和冷凝边的化学组成分析，本文较为详尽系统地探讨以上所有的问题。通过本次多年的研究，我们获得了以下几点新的认识：f1) 富挥发分过铝质岩浆体系的样品存在稀土“四重效应”和Y-Ho、Zr-Hf、Nb-Ta、Sr-Eu元素对的显著分异，表明在过铝质岩浆演化过程中含氟流体相起着重要的作用；目前，稀土“四重效应”机制被认为是含水流体相与过铝质岩浆熔体相互作用的结果(Irber 1999；Bau 1997)，而不是独居石、磷钇矿、石榴石矿物等矿物的早期结晶引起的残余熔体稀土含量的异常变化。由于阿尔泰3号伟晶岩脉各带磷灰石以及与其共生的石榴石、绿柱石、碱性长石、锂辉石矿物均存存明显的稀土“四重效应”以及相同电价、相似离子半径的不相容元素间存在显著的分异，并结合最近赵振华等(1999)和Sba and Chappell(1999)报道S型花岗岩全岩和单矿物(磷灰石、独居石、长石、黄玉等)均存在稀土“四重效应”这一现象，本文研究提出，稀土“四重效应”是富挥发分过铝质岩浆体系的一个基本特征，其机制既不可能由含稀土的副矿物早期结晶引起残余熔体相中REE含量变化的结果，也不能定性地归因于流体相与熔体相相互作用过程中稀土元素在流体／熔体之间分异的结果，而很可能与伟晶岩岩浆形成之前某些过程密切相关，S型花岗岩岩浆在液相线以上存在硅酸盐熔体与高盐熔体(或卤水相)的不混溶液相分离有可能是过铝质岩浆体系产生稀土“四重效应”的主要原因。(2) 由于Sr~(2+)与Eu~(2+)具有相同的电价、相似的离子半径，根据经典的地球化学原理，它们具有相似的地球化学行为，在各种地质过程中其它们具有紧密的一致性。阿尔泰3号伟晶岩磷灰石中Sr／Eu比值具有二歧变化现象，其中I、Il、III和IV带磷灰石具有低的Sr／Eu比值(16:0～111.2)，而V、VI、VII带、核部带和IV带中的一个磷灰石则显示较大的Sr／Eu比值(主要在246．6～514:9范围，其中IV带的一个磷灰石该比值在10000以上)。对世界范围内的过铝质花岗岩统计表明，过铝质岩浆岩的全岩样品中的Sr／Eu也呈现二歧变化，由此本文提出Sr／Eu比值是指示过铝质岩浆体系中岩浆流体相出溶的有效地球化学参数，大于300的Sr／Eu比值是Eu~(2+)强烈分配进入流体相的地球化学标志。(3) 阿尔泰3号伟晶岩I、II、III带电气石矿物的硼同位素组成(δ~(11)B)分布在-41.11‰～-30.90‰之间，V、VI、VII带电气石矿物硼同位素组成(δ~(11)B)在-15.23‰～-9.20‰范围，IV带电气石硼同位素分布于-39.19～13.10‰范围，如此大的硼同位素分馏无法根据实验研究获得的熔体／流体相间的分馏系数进行合理解释。我们的研究表明岩浆成因电气石的B同位素组成与电气石化学组成具相关性，随电气石Y位上AI、Li阳离子数的增大，δ~(11)B值显示明显增大的趋势。阿尔泰3号伟晶岩最初形成的结构带中电气石的B同位素组成是目前所发现的最低值之一(-41.1l～39.01‰)，指示形成伟晶岩脉的初始岩浆可能由含非海相蒸发岩的泥质岩经变质深熔作用形成，或是伟晶岩岩浆在上侵定位过程中同化了含非海相蒸发岩地层的结果。本次研究利用电气石-白云母和电气石-四硼酸盐矿物间的同位索分馏以及熔体相-流体相间的同位索分馏，合理解释了阿尔泰3号伟晶岩脉电气石B同位素分馏过程，并首次获得伟晶岩形成、演化过程中B同位素组成演化的全程图谱。(4)伟晶岩岩浆形成和演化过程是否存在由过磷引起的液相不混溶现象未见确凿的岩石学和实验地球化学证据。阿尔泰3号伟晶岩脉糖粒状钠长石带(II带)明显由两种不同组构的岩性组成，而且该带是3号脉主要的Be矿化带，也是P、REE最重要的沉淀场所。阿尔泰3号伟晶岩脉梳状结构带和I带的碱性长石具较高P含量(平均值分别为0.42 wt％和0.22 wt％)，随着岩浆的演化进行，从III带到核部带，碱性长石中P含量逐渐增大(平均值由0.21 wt％增至0.50 wt％)，而II带碱性长石中异常低的P含量(平均值为0.08、wt％)是该带大量磷灰石矿物饱和结晶，导致残余熔体相中P极度亏损所造成的，而不是晚期出溶的岩浆热液交代形成的。根据Watson (1978)、Ryerson and Hess(1980)在液相线以上温度下实验研究获得的微量元素在不混溶的基性和酸性液相中分配特征，以及Webster et a1．(1997）对德国Ehrenfriedersdorf矿区伟晶岩石英中熔体包裹体的研究成果，我们推断在富磷岩浆体系中，在其演化的早期将出现由磷引起的液相不混溶作用，它对伟晶岩成岩和Be的成矿具有重大的影响。

中元古代昆阳群Fe-Cu-REE矿床地球化学研究-以武定迤纳厂矿床为例

稀土元素成矿与地壳的构造运动密切相关，稀土在中元古代具有大规模暴发性成矿特征。云南武定迤纳厂稀土铁铜矿床为昆阳群因民组出现稀土富集成矿的典型代表。本论文选择迤纳厂矿床为主要研究对象，系统研究矿床不同类型岩（矿）石和矿物的稀土元素地球化学特征，探讨富稀土的成矿流体、成矿物质来源和稀土元素成矿时代，揭示昆阳裂谷初期因民组稀土元素富集的地球化学机制。主要认识如下：1、迤纳厂矿床产于昆阳裂谷初期形成的禄丰一武定火山断陷盆地中。早中元古界昆阳群分布于绿汁江岩石圈断裂和小江一易门断裂的夹持地带，呈狭长状展布。迤纳厂矿床赋矿地层为昆阳群因民组上段的硅质白云岩和碱性火山岩（粗面安山岩）。矿体产出形态和矿石的结构构造等均显示矿体与赋矿地层同沉积特征；出现独立矿物氟碳饰矿、独居石及褐帘石，磷灰石、萤石、菱铁矿等矿物中也含有一定量的稀土，沿矿体走向和垂向稀土元素变化不大。2、矿体顶、底板围岩（石榴石黑云母片岩、钠长黑云母片岩等）的原岩为碱性火山岩（粗面安山岩），相对富集大离子亲石元素Ba、Cs、Rb、K、LRE日及贫Zr、Sr、Ti、Hf、HEE，为早元古代末期一中元古代早期交代富集地慢低程度部分熔融所形成的碱性火山岩。矿石稀土总量高（645-4443）×10-6，强烈富集轻稀土（（La/Tb）N＝17.3-81.1），稀土元素分布特征明显不同于矿区正常沉积的硅质白云岩和后期侵入的钠长石英斑岩及火山角砾岩，而与矿体顶、底板碱性火山岩中稀土元素配分特征基本一致，暗示稀土成矿物质来源与碱性火山岩有密切的关系；3、矿石中微量元素组合及变化特征与现代海底正在喷出的热液和热液沉积物中元素组合有较大的可比性，明显不同与火成碳酸岩型稀土矿床中的特征元素组合；在微量元素判别图解（Al-Fe-Mn、Fe／Ti-Al／（Al+Fe＋Mn）、U-Th、Y-P2O5等）中，逸纳厂矿石均投影在热水沉积区，矿石的Y／Ho值与黑烟囱值接近，表明成矿流体为高温、还原性质，稀土成矿可能以热水沉积作用方式为主；4、对矿石中主要矿物萤石、菱铁矿、磁铁矿、石英、方解石的稀土元素特征研究表明，矿石沉积时不同矿物中稀土元素分布特征基本相同，主要受成矿流体中稀土分布特征制约。而后期变质作用形成的矿物，其稀土元素分布主要受矿物晶体结构控制。同期成矿流体从早期到晚期（块状矿石→条带状矿石），轻重稀土分异变小，稀土总量增加，条带状矿石中稀土含量最高；矿石黄铜矿6345值变化在一任3％0到2g％。范围，显示慢源硫特征；菱铁矿6r3C（8％-9.1%）、δ18O（-11.17%-15.37）‰指示成矿流体具岩浆来源和有机质的脱梭酸分解作用参与；成矿流体中稀土元素可能主要以（RE（CO3）3F）4-、（既（CO3）3F2）、（RE（F，Cl万等形式迁移，当温度降低时沉淀出氟碳饰矿等稀土矿物；5、矿石和萤石单矿物 Sm-Nd等时线年龄分别为1621士110Ma和15：38士43Ma，与矿区碱性火山岩错石的U-Pb年龄1676Ma、因民组顶部石英正长斑岩的错石U-P1。年龄1685Ma基本一致，也与因民组地层年龄1765M。较为接近，反映成矿时代为早元古代晚期和中元古代早期：这一时间也与一早元古代晚期一中元古代早期昆阳裂谷初始裂陷阶段，大量来自于地幔的碱性火山岩喷发事件相吻合。矿石。Nd（t）:-2.87-3.60，萤石单矿物εNd（t）：-3.93-5.90，变化范围较窄并全为负值，接近0，指示源区为富集地幔。同时结合矿床形成的构造一地质环境及矿体产出的地质形态，认为逛纳厂稀土铁铜矿床可能是在昆阳裂谷初期，在碱性火山岩浆喷发的间歇期，来自地幔富稀土、挥发份的成矿流体由火山喷流一同生沉积方式形成的矿床。6、昆阳群因民组地层中出现的稀土富集、成矿与我国的白云鄂博稀土REE-Fe-Nb超大型矿一床和澳大利亚的olympic Dam Cu-U-Au-Ag-REE超大型矿床，在成矿时代、产出大地构造背景、成矿物质来源等方面具有较大的相似性，均体现成矿受控于中元古代1.5Ga超大陆聚合前或随后裂解初始阶段伴随的非造山型碱性岩浆或热液作用，稀土来源于超大陆拼合前因板块俯冲交代而形成的富集地幔。

氟、氯对热液钨、铜成矿的制约-以江西德兴铜矿、大吉山钨矿为例

矿化剂在热液矿床成矿过程中的重要作用一直为人们所关注，矿化剂地球化学行为直接影响成矿元素的富集成矿，不同的矿化剂元素可能对金属成矿具有一定的专属性。本文以著名的江西德兴铜厂超大型斑岩铜矿床和大吉山钨矿床作为研究对象，研究F、Cl与W、Cu成矿的关系。主要的认识如下：（1）F在花岗质岩浆中，可以降低岩浆的粘度、密度、固液相线温度、改变熔体结构，而Cl对熔体结构没有多大的影响。F在流体一花岗质熔体相间，绝大多数配分系数小于1.0，趋向于熔体相中配分，DF随体系中F浓度的升高而增加。Cl在流体一花岗质熔体相间的配分系数均大于1.0，且Dc1 随体系中Cl浓度的升高而增大·Cl强烈地趋向富集于流体相中。（2）Cu在流体一花岗质熔体作用过程中，铜总趋向于流体相中分布（DCu都大于1）。特别是在富Cl流体中Cu浓度较高，说明在富含Cl的热液流体能够从共存的熔体中活化迁移出大量的 Cu，S的加入DCu有降低的趋势。钨趋向于熔体相中富集，其配分系数大多小于1.0。（3）德兴铜厂花岗闪长斑岩属钙碱性系列岩石属I型花岗岩类，具有埃达克岩的特征。岩浆来源于深部，在结晶演化过程中发生了围岩物质的混染，这种高铜含量围岩的混染使成矿物质在岩浆中得到富集，有利于铜的活化、迁移。在铜厂岩体不同的蚀变带中，SiO2、K2O、Cu、Mo等从新鲜斑岩甚至弱蚀变带中带出，而在强蚀变带强烈富集，Cl同样有在强蚀变岩石中富集的趋势；而Na2O、Fe从斑岩体中带出，进入流体相中，流体中大量Fe的存在，有利于铜的沉淀、富集成矿。（4）德兴铜厂斑岩体微量元素和稀土元素地球化学特征表明，该岩体发生了流体一熔体作用，分异出来的流体是一种相对富氯的流体，同时成矿流体的流向是从岩体中心向接触带方向流动。（5）大吉山花岗岩具有高SiO2、A/CNK值，显示过铝质特点。黑云母花岗岩是壳源花岗岩但又受到慢源岩浆或慢源流体的影响。随着花岗岩的演化（从I→II→III）SiO2、K2O＋Na2O逐渐增加，ΣFe、Al2O3、CaO、F含量降低，为成矿提供了大量的矿化剂（F）和沉淀剂（Fe、Ca）。Eu负异常从I至III阶段花岗岩逐渐加强，表明该岩浆经历了高度的分异演化。（6）大吉山花岗岩类稀土元素具有“四重效应”配分的特点以及微量元素对玲Rb、Y/Ho、Zr/Hf以及Nb／Ta发生明显分异，暗示在花岗岩岩浆的演化过程中，经历了充分的流体一熔体作用，同时分异出大量富含F、W等矿化剂元素和成矿元素的热液流体，致使钨矿的形成。大吉山石英脉型钨矿的成矿年龄大约在155 Ma。（7）通过对成矿流体和花岗质岩石黑云母、白云母中卤素相对逸度的研究（log(H2O/fHCl）fluid、log（fHF/fHCl）fluid）发现，铜厂斑岩型铜矿床的成矿体系是相对富氯体系，而大吉山石英脉型钨矿床成矿体系相对富氟，同时氟可能主要迁移W、Sn、Nb、Ta等金属元素。（8）结合斑岩型铜矿床成矿流体特征，铜主要以C1的络合物形式存在和迁移，迁移形式主要是CuCl0、CuCl2等。石英脉型钨矿床中，钨主要以钨酸、钨酸盐及其离解形式存在和迁移，如WO42-、HWO4-、NaHWO4、Naw伍．等；在高度富氟的成矿流体中，钨的氟氧络合物（如WO3F-，WO2F42-等）对钨迁移也具有重要的作用。因此，不同矿化剂类型具有一定的成矿专属性，热液铜矿床主要与Cl、S有 关，而热液钨矿床大多与F有关。

地表水体中微量金属元素分布的水/胶体作用控制机理的实验研究

水体中轻重稀土元素之间的分异，特别是一些具有相同电价而又具有近似相同离子半径的元素对（如Y3＋/Ho3＋、Zr4+/Hf4+、Nb5+/Ta5+）之间的分异，Ce异常和REE四重效应存在及产生原因和不同因素的控制机理构成了水体稀土元素及其它微量金属元素地球化学研究的核心科学问题，是我们合理解释地表水体中REE及其它微量金属元素组成变化的重要理论基础。目前研究水I微粒界面作用的工作不少，但至今进行的胶体或其它微粒对REE和高价阳离子（如Zr、Hf、Nb和Ta）的吸附实验研究不多，已有的实验也未能对不同控制因素（如pH、溶液介质类型、无机和有机配位体等）的控制机理进行系统研究。本文通过系列批次实验，定量研究了水合氧化铁（日FO）在不同溶液介质条件下对二价（Cu2+）、三价（Ln3＋）、四价（Zr4+、Hf4+）以及五价（Nb5+、Ta5+）阳离子的吸附／去除作用，重点讨论了溶解配位体和pH影响下水l胶体作用对轻重稀土以及Y-Ho、Zr-Hf和Nb-Ta元素对之间分异行为的影响，并模拟了稀土元素在溶液中的形态分布。研究结果表明：微量金属元素在HFO上吸附的动力学特征受控于HFO生成的动力学，溶液介质条件（包括pH、电解质、溶解配位体、吸附剂及吸附质的浓度以及吸附质的形态分布等）是影响微量金属元素水l胶体作用的主要因素；稀土元素的分配系数在水胶体作用过程中受不同因素的影响而呈现不同的分布模式，但都存在丫的负异常和较低pH下Ce的正异常现象，在CO32-、腐殖酸和SO42-、PO43-的影响下，稀土元素的分配系数分别呈现轻稀土富集和重稀土富集的分布模式，REE在HFO上的作用机制是离子交换和特性吸附综合作用的结果；在天然水体p日范围内，Zr、Hf和Nb、Ta在吸附／共沉淀过程中发生了分异，但均显示相对惰性的行为并表现出较好的一致性，指示了其地球化学孪生对的行为。上述研究结果为合理解释地表水体中稀土和其它微量金属元素分布变化的多样性提供了实验依据。

Synthesis of a silica-bonded bovine serum albumin s-triazine chiral stationary phase for high-performance liquid chromatographic resolution of enantiomers

A novel method of synthesizing protein chiral stationary phase (protein-CSP) is proposed with 2,4,6-trichloro-1,3,5-triazine as the activator. The bovine serum albumin (BSA) based chiral columns (150x4.6 mm I.D.) were prepared successfully within 8 h. With tryptophan as the probe solute, it was observed that the BSA immobilized by this method had a better ability to distinguish enantiomers than that activated by glutaric dialdehyde. This may be due to the well-maintained BSA conformation and the larger amount of BSA immobilized on the silica gel. The BSA-CSP prepared by this method was relatively stable under experimental conditions, and the resolution of 13 chiral compounds was achieved. The coupling reaction in this method is mild, reliable and reproducible; it is also suitable for the immobilization of various biopolymers in the preparation of bioreactor, biosensor and affinity chromatography columns. (C) 2000 Elsevier Science B.V. All rights reserved.

Fractionation and analysis of Artemisia capillaris Thunb. by affinity chromatography with human serum albumin as stationary phase

A method for the screening and analysis of biologically active compounds in traditional Chinese medicine is proposed. Affinity chromatography using a human serum albumin (HSA) stationary phase was applied to separate and analyze the bioactive compounds from Artemisia capillaris Thunb. Five major peaks and several minor peaks were resolved based on their affinity to HSA, two of them were identified as scoparone (SCO, 6,7-dimethoxycoumarin) and capillarisin (CAP). CAP shows a much higher affinity to HSA than SCO. The effects of acetonitrile concentration, eluent pH, phosphate concentration and temperature on the retention behaviors of several major active components were also investigated, and it was found that hydrophobicity and eluent pH play major roles in changing retention values. The results demonstrate that the affinity chromatography with a HSA stationary phase is an effective way for analyzing and screening biologically active compounds in traditional Chinese medicine. (C) 2000 Elsevier Science B.V. All rights reserved.

Separation of acidic compounds by strong anion-exchange capillary electrochromatography

Separation of the acidic compounds in the ion-exchange capillary electrochromatograph (IE-CEC) with strong anion-exchange packing as the stationary phase was studied. It was observed that the electroosmotic flow (EOF) in strong anion-exchange CEC moderately changed with increase of the eluent ionic strength and decrease of the eluent pH, but the acetonitrile concentration in the eluent had almost no effect on the EOF. The EOF in Strong anion-exchange CEC with eluent of low pH value was much larger than that in RP-CEC with Spherisorb-ODS as the stationary phase. The retention of acidic compounds on the strong anion-exchange packing was relatively weak due to only partial ionization of them, and both chromatographic and electrophoretic processes contributed to separation. It was observed that the retention values of acidic compounds decreased with the increase of phosphate buffer and acetonitrile concentration in the eluent as well as the decrease of the applied voltage, and even the acidic compounds could elute before the void time. These factors also made an important contribution to the separation selectivity for tested acidic compounds, which could be separated rapidly with high column efficiency of more than 220 000 plates/m under the optimized separation conditions. (C) 2000 Elsevier Science BN. All rights reserved.

Separation of peptides by strong cation-exchange capillary electrochromatography

Separation of small peptides on ion-exchange capillary electrochromatography (IE-CEC) with strong cation-exchange packing (SCX) as stationary phase was investigated. It was observed that the number of theoretical plates for small peptides varied from 240 000 to 460 000/m, and the relative standard deviation for t(0) and the migration time of peptides were less than 0.57% and 0.27%, respectively for ten consecutive runs. Unusually high column efficiency has been explained by the capillary electrophoretic stacking and chromatofocusing phenomena during the injection and separation of positively charged peptides. The sample buffer concentration had a marked effect on the column efficiency and peak area of the retained peptides. The influences of the buffer concentration and pH value as well as the applied voltage on the separation were investigated. It has been shown that the electrostatic interaction between the positively charged peptides and the SCX stationary phase played a very important role in IE-CEC, which provided the different separation selectivity from those in the capillary electrophoresis and reversed-phase liquid chromatography. A fast separation of ten peptides in less than 3.5 min on IE-CEC by adoption of the highly applied voltage was demonstrated. (C) 2000 Elsevier Science B.V. All rights reserved.

Capillary electrochromatography using a strong cation-exchange column with a dynamically modified cationic surfactant

A novel mode of capillary electrochromatography (CEC), called dynamically modified strong cation-exchange CEC (DMSCX-CEC), is described in this paper. A column packed with a strong cation-exchange (SCX) packing material was dynamically modified with a long-chain quaternary ammonium salt, cetyltrimethylammonium bromide (CTAB), which was added to the mobile phase. CTAB ions were adsorbed onto the surface of the SCX packing material, and the resulting hydrophobic layer on this packing was used as the stationary phase. Using the dynamically modified SCX column, neutral solutes were separated with the CEC mode. The highest number of theoretical plates obtained was about 190 000/m, and the relative standard deviations (RSD's) for migration times and capacity factors of alkylbenzenes were less than 1.0% and 2.0% for five consecutive runs, respectively. The effects of CTAB and methanol concentrations and the pH value of the mobile phase on the electroosmotic flow and the separation mechanism were investigated. Excellent simultaneous separation of the basic and neutral solutes in DMSCX-CEC with a high-pH mobile phase was obtained, A mixture containing the acidic, basic, and neutral compounds was well separated in this mode with a low-pH mobile phase; however, peak tailing for basic compounds was observed in this mobile phase.

Alkaline treatment of the cellulose fiber affecting membrane column behaviour for high-performance immunoaffinity chromatography

The original cellulose fibers and those treated by alkaline solution were both used to prepare the acrylic membranes. The two kinds of membranes were packed into the columns for high-performance immunoaffinity chromatography by the immobilization of protein A on them. It was observed that the alkaline treatment of the cellulose fiber decreased the pressure resistance of the membrane to the mobile phases and greatly increased the accessible volume to the proteins, but affected the adsorption capacity of human IgG on the protein A membrane columns less. There is little difference between those two kinds of membranes on the adsorption capacities of HIgG, which means that the alkaline treatment of the cellulose fiber only significantly changes the void volume inter-membrane, and the porosity and surface area of membrane less. Alkaline treatment of the cellulose fiber reduced the membrane-column efficiency significantly. Some typical examples for the immunoaffinity analysis of IgG from human and dog plasma on the protein A membrane columns are illustrated. Copyright (C) 2000 John Wiley & Sons, Ltd.

Fast analysis of capillary electrochromatography with non-porous ODS as the stationary phase

High-speed capillary electrochromatography was developed on both short and long packed columns with 2 mu m non-porous ODS as the stationary phase. Factors that affect the analysis time of samples, such as voltage, electrolyte concentration, pH and organic modifier concentration in the mobile phase, were studied systematically. Fast analysis of aromatic compounds within 13 seconds was realized with column efficiency of 573,000 plates/m and a R.S.D.% of the retention times of all components in 8 consecutive injections below 1.0%. which demonstrated the high efficiency and high reproducibility of such a technique. In addition, DNPH derived aldehydes and ketones in both standards and environmental samples were separated with high speed.

Protein A tangential flow affinity membrane cartridge for extracorporeal immunoadsorption therapy

Tangential flow affinity membrane cartridge (TFAMC) fs a new model of immunoadsorption therapy for hemoperfusion. Recombinant Protein A was immobilized on the membrane cartridge through Schiff base formation for extracorporeal IgG and immune complex removal from blood. Flow characteristics, immunoadsorption capacity and biocompatibility of protein A TFAMC were studied. The results showed that the pressure drop increased with the increasing flow rate of water, plasma and blood, demonstrating reliable strength of membrane at high now rare. The adsorption capacities of protein A TFAMC for IgG from human plasma and blood were measured. The cartridge with 139 mg protein A immobilized on the matrix (6 mg protein A/g dry matrix) adsorbed 553 mg IgG (23.8 mg IgG/g dry matrix) from human plasma and 499.4 mg IgG (21.5 mg IgG/g dry matrix) from human blood, respectively. The circulation time had a major influence on IgG adsorption capacity, but the flow rate had little influence. Experiments in vitro and in vivo confirmed that protein A TFAMC mainly adsorbed Ige and Little of other plasma proteins, and that blood cell damage was negligible. The extracorporeal circulation system is safe and reliable. Copyright (C) 1999 John Wiley & Sons, Ltd.