共查询到19条相似文献,搜索用时 125 毫秒
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毛细管电色谱是在毛细管中依靠电渗流来驱动流动相 ,同时溶质与固定相发生相互作用的一种色谱分离模式 ,它有高效液相色谱的高选择性 ,同时兼具毛细管电泳的高效性 [1] .传统电色谱柱是将HPLC填料装入毛细管 ,但由于装柱困难且易产生气泡而在一定程度上阻碍了电色谱的发展 [2~ 4 ] .通过柱内合成的方法直接在毛细管中制成连续床毛细管电色谱柱 ,可避免两端烧塞 . 1 995年 Svec等 [5,6]首次将连续床层色谱柱用于毛细管电色谱 ,此后 ,有关毛细管中原位合成连续床电色谱柱的方法得到了应用 [7~ 11] .为了使原位合成电色谱柱能产生电渗流 ,… 相似文献
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毛细管离子交换电色谱的分离行为 总被引:7,自引:0,他引:7
在离子交换毛细管色谱柱上实施电色谱,并对其分离行为进行了研究,采用75μm(i.d.)20cm的毛细管强阳离子交换柱(3μm)以NaH2PO4-H3PO4缓冲液为淋洗剂,紫外柱上检测(214nm)考察了流动相的pH值,有机改性剂及分离电压等因素对分离的影响,研究表明,不同的pH溶质的流出次序发生改变,随着有机改性剂含量增加,溶质的保留时间减小,而电渗流却增大,同时,对分离的柱效和方法的重现性进行了 相似文献
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在75μm×20cm的毛细管ODS填充柱上实现毛细管反相电色谱分离,考察种种分离因素,包括流动相的组成,有机相的种类和比例,电解质缓冲液的种类浓度和PH值,以及分离电压和分离温度等因素对填充毛细管电渗流的影响,系统研究了反相毛细管电色谱的电渗变化规律。 相似文献
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采用温和条件下的溶胶-凝胶技术,成功制备了阴离子交换-反相混合模式硅胶基质毛细管电色谱整体柱。通过调整反应液中不同前体的比例,优化了整体柱的制备条件。通过扫瞄电镜,对柱床进行了表征和分析。实验发现,所制备的整体柱电渗流的方向和大小可随流动相pH值的改变而改变,在酸性和中性条件下,具有从阴极流向阳极的电渗流;当流动相pH值升至约7.5时,电渗流方向发生了反转(由阳极流向阴极)。在优化的实验条件下,用所制备的整体柱对所考察的酸性(中性)化合物实现了快速分离,并获得了高达160,000N/m的柱效。 相似文献
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非电荷型毛细管电色谱原位柱的色谱行为研究──阴离子表面活性剂的动态改性 总被引:7,自引:5,他引:2
采用原位聚合的方法在毛细管中合成了非电荷型连续床电色谱原位柱 ,通过在电色谱流动相中加入阴离子表面活性剂十二烷基硫酸钠 (SDS)进行动态改性使其产生电渗流 ,考察了SDS浓度及有机改性剂浓度等因素对电渗流的影响。此类连续床柱制备容易 ,柱效可达 14万理论塔板 /m ,在不同的操作条件下有良好的稳定性 ,连续 10次运行 ,其死时间t0 与保留时间的精密度分别为 0 .2 2 %和 <0 .5 6 %。 相似文献
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以丙烯酸、2-丙烯酰胺-2-甲基丙磺酸为功能单体,N,N′-亚甲基双丙烯酰胺为交联剂,正十二醇、1,4-丁二醇及二甲基亚砜为致孔剂,偶氮二异丁腈为引发剂,原位聚合制备了丙烯酰胺类强阳离子交换整体柱。考察了驱动电压、有机调节剂、盐浓度、pH值等对电渗流的影响。结果表明,电渗流与驱动电压的线性关系良好,相关系数为0.9981;有机调节剂乙腈对电渗流的影响除与流动相的黏度有关外,还与固定相的溶胀有关,当浓度低时,电渗流随乙腈浓度的增加有反常的下降趋势;随着磷酸盐浓度逐渐增加,电渗流降低,与理论相符;在pH值为3~9范围内,电渗流基本上保持恒定,体现了整体柱使用酸碱范围宽的优越性。在优化的实验条件下,采用毛细管电色谱法在此整体柱上成功分离了5种多肽,体现了该类整体柱在多肽分离研究中的优势,为进一步将其应用于蛋白质分离研究打下了基础。 相似文献
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Behavior of neutral solutes in pressurized flow driven electrochromatography using a mixed stationary phase of ODS and anion-exchange 总被引:1,自引:0,他引:1
The behavior of neutral sample solutes in pressurized flow driven electrochromatography using a mixed stationary phase, which consisted of ODS and anion-exchange (ODS-SAX), was studied. Applications of both positive and negative voltage on a column induced increases in retention factors of sample solutes. The direction of an electroosmotic flow under applications of positive and negative voltage were the same, therefore, the sign of the surface charge density under positive and negative voltage was opposite. We proposed a new equation for the relationship between applied voltage and surface charge density, and the practical electroosmotic flow conformed to this equation. Studying the electroosmotic flow using our proposed equation revealed that the applied negative voltage accelerates the protonation of the quaternary ammonium group and dissociation of the silanol group on packing materials. The retention behavior of a neutral solute was affected by the existence of the charged functional groups. We propose that this phenomenon is applicable to the control of the retention behavior of a sample solute using an electric field. 相似文献
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采用简便易行的方法自制内径为100 μm的电色谱柱,并考察了其性能,同时研究了磷酸盐缓冲液浓度、乙腈体积分数、电压、柱温对中性化合物保留行为的影响。 相似文献
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The aim of this study was to evaluate the applicability of ODS-AQ packing material as a stationary phase in capillary electrochromatography (CEC). The electroosmotic flow created on an ODS-AQ stationary phase was measured at different mobile phase compositions and at different column temperatures. It was observed that the electroosmotic flow generated in the column increased by 50% when the temperature of the system was raised from 20 degrees C to 60 degrees C, while all other conditions were kept constant. The electroosmotic flow produced by the ODS-AQ stationary phase was found to be comparable to the flow generated in a column packed with Nucleosil bare-silica material. In addition, a set of polar compounds (D-lysergic acid diethylamide derivatives) was utilized to determine the influence of temperature and mobile phase composition on their chromatographic behavior on an ODS-AQ stationary phase in a CEC mode. A linear relationship between the solute retention factor and column temperatures was seen over the temperature range studied (20 degrees C to 60 degrees C). A quadratic function was used to describe the changes in the solute retention factors with variation of acetonitrile concentration in the mobile phase. 相似文献
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The effect of the superposition of electroosmotic flow and pressureinduced hydrodynamic counterflow on efficiency has been investigated for different capillary electrophoretic systems. Results are shown for 50 and 75 μm internal diameter capillaries at several voltage and counterpressure levels. Hydrodynamic counterflows were successfully applied in electrokinetic chromatography in order to delay the entry of a UV-active pseudostationary phase, tetraphenyl porphyrintetrasulfonate, into the detection zone allowing the separation of neutral nitroaromatics. The separations are based on the weak charge-transfer interactions between the porphyrin and the analytes. 相似文献
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建立了以硝酸钾作为背景电解质测定阿霉素脂质体药物中微量硫酸根离子的毛细管电泳分析法。考察了分离电压、背景电解质、电渗流改性剂浓度、pH值对分离测定的影响。结果表明,当毛细管长度为60 cm(有效长度51.5 cm)、分离电压为~15 kV、缓冲溶液采用20 mmol/L硝酸钾(pH 7.0)、电渗流改性剂采用0.4 mmol/L十六烷基三甲基氯化铵(CTAC)、检测波长为202 nm时,阿霉素脂质体破乳液中硫酸根离子和氯离子在3 min内得到了基线分离,硫酸根离子迁移时间和峰面积的相对标准偏差分别小于0.01%和1.0%,检出限为5 μg/L。用该方法对阿霉素脂质体样品中的微量硫酸根离子进行了分析测定,结果令人满意。 相似文献
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Separation and determination of 10-hydroxy-2-decenoic acid in royal jelly by capillary electrophoresis 总被引:1,自引:0,他引:1
Summary The application of capillary electrophoresis (CE) to the separation and determination of the active ingredient, 10-hydroxy-2-decenoic
acid, in royal jelly with direct on-column UV detection at 214 nm is described. Using a cathodic injection and anodic detection
scheme, 10-hydroxy-2-decenoic acid (10-HDA) was separated and detected in less than 10 min in a fused silica capillary column
with a phosphate buffer at pH 7.3 with an applied voltage of 20 KV followed by direct UV detection. The use of cetyltrimethylammonium
bromide (CTAB) as electroosmotic flow modifier allows the rapid separation of 10-HDA from other constituents in royal jelly
by reversing the direction of electroosmotic flow. The influence of organic solvents in the electrolyte on separation selectivity
is also discussed. 相似文献