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毛细管气相色谱用固定液的进展 总被引:4,自引:2,他引:2
一、前言 自从1979年弹性石英毛细管柱问世之后.毛细管气相色谱得到了迅速的发展。以毛细管柱代替填充柱的趋势日益明显.特别是1983年大内径厚液膜毛细管柱的发展和应用使这种趋势更加肯定了。当然目前在国内填充柱气相色谱仍在例行分析中占主导地位,但是随着毛细管色谱技术在国内的进一步发展,填充柱会逐步地被毛细管柱所取代。 相似文献
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针对目前毛细管色谱柱装柱效率低、不同批次装填的毛细管色谱柱之间性能差异大的问题,我们发展了一种多通道匀浆装填毛细管色谱柱的新装置。该装置以液相色谱泵提供压力、采用磁力搅拌保持匀浆液均匀分散,一次可装填多达6根毛细管色谱柱。以牛血清白蛋白(BSA)的胰蛋白酶酶切肽段混合物为样本,选择峰容量、蛋白覆盖率、3个特定离子的保留时间以及毛细管色谱柱柱压为指标,在毛细管液相色谱-质谱联用系统上对装填的反相毛细管色谱柱的性能进行了评价。分别考察了一次装填的6根毛细管色谱柱、两次装填的12根毛细管色谱柱以及一次装填1根与一次装填6根毛细管色谱柱的性能及稳定性。实验结果表明:同一批次装填的6根毛细管色谱柱的性能相近;不同批次装填的12根毛细管色谱柱的峰容量和覆盖率没有明显的区别,但保留时间和毛细管色谱柱柱压的稳定性较差;一次装填1根和一次装填6根毛细管色谱柱柱性能的稳定性与两次分别装填6根毛细管色谱柱的稳定性相近,即采用本装置可显著提高毛细管色谱柱的装填效率且每次装填毛细管色谱柱的数量不会对柱性能产生影响。 相似文献
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反相毛细管整体柱的制备及其在多肽混合物分离中的应用 总被引:3,自引:3,他引:0
采用甲基丙烯酸月桂酯为基础功能单体,乙二醇二甲基丙烯酸酯为交联剂,正十二醇、1,4-丁二醇及二甲基亚砜为致孔剂,在内径为75 μm的石英毛细管内制备了具有良好机械性能及化学稳定性的反相毛细管整体柱。考察了致孔剂的种类、比例以及交联剂在单体混合物中的比例对柱压和分离效果的影响;以单体15%、交联剂15%、致孔剂70%(均为质量分数)作为优化配方,在70 ℃条件下反应24 h;并对所合成的毛细管整体柱进行了电镜表征,测试了流速、柱长与柱压的关系。结果表明,毛细管整体柱的通透性良好,可通过延长柱长的方法提高分离效果。将所制备的毛细管整体柱装于纳升级高效液相色谱仪上进行牛血清白蛋白及血浆样本的胰蛋白酶酶切液的分离,获得了比较理想的分离效果。 相似文献
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本文发展了一种“一锅法”制备C18-硅胶杂化毛细管整体柱的方法。发展了一种“一锅法”制备有机-无机杂化毛细管整体柱的方法。首先将四甲氧基硅烷、乙烯基三甲氧基硅烷在弱酸条件下水解,然后加入有机单体(甲基丙烯酸-N,N-二甲基十八烷基溴化铵乙酯)及自由基聚合引发剂,同步原位完成硅羟基间的缩聚反应及双键间的自由基聚合反应,从而制成C18-硅胶杂化整体柱;同时用毛细管电色谱(CEC)和毛细管液相色谱(CLC)对其柱效和分离能力进行了初步评价,并将其应用到微柱液相色谱-串联质谱对牛血清白蛋白酶解液的分离分析。结果表明,该C18-硅胶杂化整体柱具有较高的柱效和较好的重现性,在分离分析复杂生物样品方面具有较大的应用前景。此外,本文所发展的方法在制备杂化整体柱的过程中不借助相应的硅烷试剂,为杂化整体柱的制备提供了一种新的思路。 相似文献
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毛细管电泳中的毛细管区段灌注及其相关技术 总被引:1,自引:0,他引:1
毛细管区段灌注是一种随手性毛细管电泳、亲和毛细管电泳和胶束电动力色谱-质谱发展而产生的实验技术。由于它能消除采用以上方法时遇到的缓冲溶液对检测的影响。因此引起人们的关注。本文对区段灌注技术的原理,区段灌注技术在手性毛细管电泳、亲和毛细管电泳和胶束电动力色谱中的应用,以及目前区段灌注技术存在的一些问题进行了评述。本文还对由区段灌注技术发展而来的逆流毛细管电泳、液相预柱毛细管电泳、多步配体进样等实验技术进行了简介。 相似文献
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采用液相沉积技术制备了纳米二氧化硅涂层毛细管,经十八烷基改性,将其作为开管毛细管电色谱(OTCEC)分离介质。研究了该涂层毛细管的电渗流行为,考察了烷基苯和多环芳烃的毛细管电色谱分离性能。结果表明,该涂层固定相对这些化合物表现出较强的疏水作用;增加液相沉积涂层次数有利于增加溶质的保留因子,四种多环芳烃和四种苯同系物在该柱上可实现基线分离。此外,该涂层制备简单、重现性好,并在应用中表现出较高的稳定性。 相似文献
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An overview and detailed analysis of the classical theory of capillarity is presented. A number of known equations of capillary rise dynamics are shown to be different limiting cases of one rather general equation. Some internal inconsistencies of the classical equations are pointed out. The role of nonlinear dissipation and flow pattern effects in the front zone of the liquid column and near the capillary entrance is discussed. Numerical simulations and experimental data demonstrating some characteristic types of dynamic behavior predicted by the theory are reported. Special attention is paid to the capillary rise of surfactant solutions. As applied to this special case, the existing theory is substantially elaborated by setting up a closed system of equations describing the surfactant transport and relaxation processes in the adsorption layer. A simplified relation for the capillary rise dynamics in the case of strong depletion of the interfacial region is obtained, which is in qualitative agreement with the experimental behavior. Copyright 2000 Academic Press. 相似文献
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Capillary impregnation into cylinder banks 总被引:3,自引:0,他引:3
Young WB 《Journal of colloid and interface science》2004,273(2):576-580
The capillary rise of liquid in a cylinder bank is examined in order to study the capillary pressure variation perpendicular to the direction of the cylinders. The calculations consider the local geometric variation of the flow channel and the position-dependent capillary pressure. The capillary flow around each cylinder is calculated by balancing the capillary pressure and the viscous drag along the flow path. The rate of filling for several layers of cylinders is used to estimate the equivalent capillary pressure. The method is also applied to the underfill of a flip chip system, which is modeled as a cylinder bank between parallel plates. 相似文献
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A short length of a sol‐gel monolith was initially prepared as the temporary frit in a 100 μm inner diameter fused‐silica capillary by an in situ photopolymerization. The packed 4 μm octadecylsilane particles were then immobilized within the identical sol‐gel solution through the same photopolymerization process. The prepared fritless capillary column was examined for the chromatographic performance by the self‐developed capillary liquid chromatography system. Baseline separation of the model analytes was achieved including thiourea, benzene, toluene and ethylbenzene with the lowest theoretical plate height about 66 μm for the retained component. A scanning electron micrograph was used to characterize the temporary frit and entrapped microspheres. The inorganic polymer matrix in the microsphere‐packed column functioned to link microspheres at specific sphere‐sphere and sphere‐capillary contact points. Furthermore, the stability and porosity of the fritless column were systematically investigated by a simple flow method. 相似文献
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María Paz San Andrs María Eugenia Len‐Gonzlez Luis Vicente Prez‐Arribas Luis María Polo‐Díez 《Journal of separation science》2000,23(5):367-372
This paper describes a liquid chromatographic method using a reversed phase capillary column coupled to an UV detector for the quantitation of thirteen pollutant phenols. Chromatographic separation was carried out with gradient elution at 25.0 ± 0.1°C. The two major anisocratic elution modes (gradient elution and temperature programming) were evaluated. The detection limit range was 10–81 pg (100 nL injected). The chromatographic method combined with liquid‐liquid extraction was applied to analysis of these compounds in river water. Recoveries of 75–103% were achieved for most of them. 相似文献
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The differential version of the method of capillary rise has been used to measure the capillary constant and calculate the surface tension of methane-nitrogen solutions. Experiments have been conducted in the temperature range from 95 to 170 K at pressures up to 4 MPa. Experimental data on surface tension have been compared with the results of calculations by thermodynamic models. Equations are given which describe the dependence of the capillary constant of a solution on its temperature and composition. 相似文献
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A. J. Berry D. E. Games I. C. Mylchreest J. R. Perkins S. Pleasance 《Journal of separation science》1988,11(1):61-64
A frit restrictor interface for capillary column supercritical fluid chromatography/mass spectrometry (SFC/MS) has been constructed and used for the analysis of high boiling point alkanes. Packed column SFC/MS is described using both a moving belt liquid chromatographic/mass spectrometric interface and a thermospray source in the filament-on mode. 相似文献