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泽泻乙醇提取物的HPCE分离研究 总被引:2,自引:0,他引:2
采用高效毛细管电泳的胶束电动毛细管色谱的分离模式(MEKC),对泽泻的乙醇(95%)提取物进行分离研究。以十二烷基硫酸钠(SDS)胶束为准固定相.硼砂为缓冲体系,甲醇为有机添加剂,考察了SDS浓度、硼砂浓度、pH、甲醇用量、电泳电压、电泳温度等对分离的影响。结果表明:硼砂缓冲体系为运行缓冲溶液(pH:9.18~9.20)、硼砂浓度30mmoL/L、SDS浓度45mmol/L、甲醇体积分数30%,分离电压25kv、分离温度25℃时分离效果最好。在此条件下,得到分离度和重现性均较好的泽泻乙醇提取物的HPCE色谱图。 相似文献
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胶束电动毛细管色谱间接紫外光检测法分离胆汁酸 总被引:1,自引:0,他引:1
利用间接紫外光检测法在254 nm进行胆汁酸胶束电动毛细管色谱分离的研究.在对氨基苯磺酸为背景电解质和十二烷基硫酸钠作胶束的体系中,加入高浓度的尿素,有效地改善了两类胆汁酸5组份的分离度,在优化分离缓冲体系10 mmol/L对氨基苯磺酸-5 mmol/L硼砂-30 mmol/LSDS-7 mol/L尿素-10%乙醇(pH 7.5)中,13 min内获得基线分离,分离效率为8.4×104~1.1×105.所建立的方法无需衍生化处理,为胆汁酸的分离提供了新的通用的方法. 相似文献
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以阴离子表面活性剂十二烷基硫酸钠(SDS)、非离子表面活性剂吐温20( Tween 20)及两者组成的混合胶束体系作为毛细管胶束电动色谱(MECC)的分离介 质,进行4种结构相似的酸性化合物的MECC分离研究,考察了胶束的类型、表面活 性剂的浓度、缓冲溶液的pH值及有机改性剂乙醇对分离的影响。结果表明各因素对 酸性药物的MECC分离有不同的影响规律。SDS胶束体系对溶质的保留值最大, Tween 20体系的保留值最小,二者的分离选择性正好相反,混合胶束体系的分离行 为则介于两者之间;在SDS和Tween 20体系中,表面活性剂浓度增加,溶质的保留 时间均随之递增,混合胶束体系中,总浓度一定,随Tween 20配比的增加,溶质的 保留时间先减少后增加;缓冲溶液的pH值增大,使溶质的分离效果均能变差;有机 改性剂乙醇的加入对容量因子的影响主要与溶质的疏水性有关,并对分离作用机理 进行了探讨。在SDS和Tween 20 MECC体系下,分别进行了实样测定,取得了满意的 结果。 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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利用胶束电动毛细管色谱在柱样品电堆积的预富集方法,以十二烷基硫酸钠胶束作准固定相,对七种植物激素进行了富集和分离。研究了各种分离条件的影响,并分别在高电渗流和聚丙烯酰胺涂层抑制电渗流条件下对植物激素进行在柱电堆积富集,各种植物激素的检出限比文献报道降低1~2个数量级。在最佳条件下对植物样品中的脱落酸进行了测定,其相对标准偏差为2.4%;回收率为75%。 相似文献
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Miao WANG Jian Wei YAN Yan Fei LIN Jian De LU* Xiao Yun FU Department of Chemistry Yuquan Campus Zhejiang University Hangzhou Zhejiang College of Chinese Traditional Medicine Hangzhou 《中国化学快报》2002,13(12)
Micellar electrokinetic capillary chromatography (MECC) is a branch of capillary electrophoretic techniques, in which surfactant micelles are added to the electrolyte solution as pseudostationary phase. Separation in MECC is based on electrophoretic mobilities of the analytes when partitioned into micelles1. In this work, four acidic drugs similar in structure with aryl carboxylic acid were separated by MECC. The effects of type of surfactant, such as anionic surfactant SDS, nonionic … 相似文献
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Summary A method for the separation of a number of herbicides consisting of chlorophenoxy acids by micellar electrokinetic capillary chromatography (MECC) was developed. Sodium dodecyl sulphate (SDS), Brij 35, cetyltrimethylammonium bromide (CTAB) and methanol were introduced into the buffers to investigate their effects on the separation of the herbicides. SDS combined with Brij 35 as the micellar agent was found to provide the best overall separation of these components. 相似文献
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JunLI ZhuoBinYUAN 《中国化学快报》2004,15(8):947-950
A micellar electrokinetic capillary chromatography (MECC) was developed for the determination of aniline and 6 substituted anilines. The seven components were separated within 25min in the buffer solution of 40mmol/L sodium borate and 100mmol/L SDS. It was found that the separation was dependent on operating voltage, pH value, borate and SDS concentrations.The analytical performance was examined in terms of linear response and reproducibility.Wastewater was determined by the established method. 相似文献
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Tohru Saitoh Nobutoshi Ojima Hitoshi Hoshino Takao Yotsuyanagi 《Mikrochimica acta》1992,106(1-2):91-99
The partition constants (K
d) have been estimated for nitrophenols, thiazolylazo dyestuffs and metal chelate compounds into the sodium dodecyl sulfate (SDS) micellar phase at an ionic strength of 0.10M [(H+, Na+)Cl–] and at 20 °C. The equilibrium partition data obtained by batch-wise solution spectrophotometry (equilibrium shift method) agree well with those by the micellar electrokinetic capillary chromatography (MECC) with the SDS micellar pseudo-stationary phase. The MECC clearly discriminates a very small difference (0.03) in the logK
d values of some metal chelates. The plot of theK
d values with the van der Waals volume of the solute molecules obviously shows the leveling-off of theK
d values over solute size near 110 ml/mol, which seems to be consistent with the results obtained in the Triton X-100 micellar system. This phenomenon arises most probably from the rigidity of the micellar pseudo-phase (a micellar volume-constraint effect) in sharp contrast with true two-phase partitioning such as solvent extraction systems. 相似文献
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Analysis of differential detergent fractions of an AtT-20 cellular homogenate using one- and two-dimensional capillary electrophoresis 总被引:2,自引:0,他引:2
Differential detergent fractionation was used to sequentially extract cytosolic, membrane, nuclear, and cytoskeletal fractions from AtT-20 cells. Extracted components were denatured by sodium dodecyl sulfate (SDS) and then labeled with the fluorogenic reagent 3-(2-furoyl) quinoline-1-carboxaldehyde. Both capillary sieving electrophoresis (CSE) and micellar electrokinetic capillary chromatography (MECC) were used to separate labeled components by one-dimensional (1D) electrophoresis. Labeled components were also separated by two-dimensional (2D) capillary electrophoresis; CSE was employed in the first dimension and MECC in the second dimension. Roughly 150 fractions were transferred from the first to the second capillary for this comprehensive analysis in 2.5 h. 相似文献
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寡糖的毛细管电泳分析 总被引:10,自引:0,他引:10
多种寡糖经α-萘胺衍生化后,用硼砂作为电泳介质,实现了高效毛细管电泳分离。比较了毛细管区带电泳和胶束毛细管电动色谱分离寡糖α-萘胺衍生物的电泳行为,对影响分离度的诸因素进行了考察,选择了最佳分离条件。 相似文献
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苯胺及其衍生物的毛细管电泳行为研究 总被引:3,自引:1,他引:3
黄甫 《理化检验(化学分册)》2003,39(12):696-699
采用紫外吸收检测,毛细管电泳分离,研究了九种苯胺及其衍生物在毛细管区带电泳(CZE)体系和胶束电动毛细管色谱(MECC)体系中的行为特征。讨论了缓冲溶液的浓度与pH、胶束浓度及混合胶束等在不同体系中对分离组分的影响,发现在CZE体系中,控制分离的主要因素是pKb值;在MECC体系中,控制分离的主要因素是溶质分子中碳原子数。建立了一种分离测定九种苯胺及其衍生物的高效毛细管电泳方法。 相似文献
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以十二烷基硫酸钠(SDS)胶束为准固定相,考察了头孢哌酮、头孢哌酮S-异构体、头孢哌酮杂质A及其他未知杂质在胶束电动毛细管色谱(MECC)分离模式下的分离行为。研究了运行缓冲液的pH值、磷酸盐浓度、SDS浓度、甲醇体积分数、分离电压、分离温度等因素对头孢哌酮、S-异构体、头孢哌酮杂质A及其他杂质的迁移时间、分离度以及可分离出的杂质个数的影响。结果发现,这些因素对头孢哌酮与诸杂质间的分离及检测有显著的影响,尤以pH值为最。它不仅影响它们的迁移时间和分离效率,还直接影响头孢哌酮及其杂质峰的检测。优化后的分离条件:运行缓冲液为70 mmol/L磷酸盐-100 mmol/L SDS (pH 6.5),分离电压为15 kV,分离温度为25 ℃。在此条件下,用非涂渍石英毛细管51.0 cm×75 μm(有效长度42.5 cm),压力进样5 kPa×5 s,在254 nm波长下进行检测,可分离出28个杂质,诸杂质彼此间及与头孢哌酮间可得到有效分离。并将该方法成功地用于测定注射用头孢哌酮钠的含量和有关物质,结果令人满意。 相似文献