高效毛细管电泳的电导检测和紫外光度检测研究

本文自制商效毛细管电泳装置.研究了毛细管区带电泳电导检测和毛细管胶束电动色谱紫外光度检测。在电导检测中,制作铂丝微电导池,并由用电池隔膜制作的导电接口连接电泳毛细管和电导池,高压被有效隔离,实现柱后电导检测,用内径200μm、长70cm(到接口)石英毛细管在10kV电压下分离检测Li~-、Na~-、K~-。在电动色谱中将高效液相色谱仪与高压电源组成电泳装置,用内径100μm,长50cm(到检测器)石英毛细管和SDS胶束溶液在14kV电压下分离检测电中性化合物。     

用毛细管电泳法对某些药物的分离试验

本文采用毛细管电泳法,以50μm内径,45cm长的弹性石英毛细管作为分离管,选用磷酸盐-硼酸盐-十二烷基硫酸钠缓冲溶液体系,在柱254nm紫外检测器,在不同的电泳电压下,对水溶性维生素,磺胺类药物、头孢菌素抗生素,解热镇痛药物有效成份进行了分析,取得较满意的结果。     

毛细管凝胶电泳的激光光热在线检测

近年来,毛细管电泳已成为一种高效快速的微化学分离分析新技术,在无机、有机及生物化学分析中得到了广泛的应用.但毛细管的内径小,进样量在pg～ng级,给样品的检测带来新的困难.因此,发展高灵敏度的显微在线检测器,已成为毛细管电泳技术发展中的重要环节.基于各种原理的检测器研究已有报道~[1].Dovichi等曾用热透镜技术在线检测了乙腈/     

毛细管电泳安培检测扑热息痛及其水解物

研究了各种电化学预处理条件下碳纤维电极对扑热息痛及水解物的电化学行为。确定该体系最佳预处理条件为０．２Ｖ电位下阳极化１ｍｉｎ，再于－２．０Ｖ下阴极化１０ｓ。预处理后的碳纤维伏安响应得到明显提高。运用最佳条件并在支持电解中加入添加剂后，扑热息痛及其水解物在毛细管电泳上获得很好的分离和检测。其中扑热息痛的检测下限为２．７８ｐｇ；对氨基酚为１．８４ｐｇ。     

长光路光度法测定中药材中痕量硒

本文研究了用长光路光度法测定痕量硒。在酸性溶液中，Ｓｅ（Ⅳ）催化ＫＣｌＯ３氧化苯肼成偶氮离子，继而与变色酸生成红色偶氮化合物。硒含量在１．０×１０－９～２．０×１０－７ｇ／ｍＬ范围内遵守比尔定律。巯基棉分离后，测定中药材中总硒，获得满意结果。     

区带毛细管电泳分离测定大黄提取液中游离蒽醌化合物

采用区带毛细管电泳法分离和同时测定大黄提取液中五种蒽醌化合物的含量。毛细管电泳的分离条件为:50 cm×75μm i.d.未涂层石英分光毛细管,分离电压20kV,0.05 mol/L KH2PO4-Na2HPO4(pH=8.2)缓冲溶液,紫外检测波长为254 nm,以氨基苯磺酸为内标。该法简便,快速,分辨率高,重现性好。     

毛细管电泳免疫分析的发展及动向

毛细管电泳免疫分析是一种新兴的免疫分析技术，较常规免疫分析方法具有很多的优越性。本文对毛细管电泳免疫分析近几年的发展情况作了总结，并对其发展的动向作了评述。     

Extending the scope of enantiomer separation by capillary supercritical fluid chromatography on immobilized polysiloxane-anchored permethyl-β-cyclodextrin (Chirasil-Dex)

Immobilized polysiloxane-anchored permethyl-β-cyclodextrin (Chirasil-Dex) with a cyclodextrin content of approximately 30 % by weight, previously employed as a versatile chiral stationary phase for the separation of enantiomers by GC, has been used for the separation of enantiomers by capillary supercritical fluid chromatography (SFC). A considerable number of racemates could be resolved, e.g. aromatic alcohols, amino alcohols (TFA derivatives), and underivatized acids. Many pharmaceutical compounds were among those analyzed, including several NSAIDs (e.g. ibuprofen and ketoprofen), a steroidal drug (nor-gestrel), a barbiturate (hexobarbital), and others. Among the racemates resolved were many which cannot be analyzed by GC owing to low volatility or decomposition at elevated temperatures. For two racemates, analysis temperature and mobile phase density were systematically varied to give constant analysis times or capacity factors k. Low temperatures (ca 60 °C) yielded the best separation in term of separation factor, α, or resolution, R_s, even though higher densities had to be used. In comparison with GC, capillary SFC was able to furnish higher separation factors and similar resolution. The applicability of capillary SFC for the analysis of mixtures of cyclodextrin derivatives, e.g. those used in the synthesis of Chirasil-Dex, was, furthermore, demonstrated.     

石英芯片电泳分离检测尿中蛋白的研究

通过对缓冲体系、缓冲液浓度、酸度、乳酸钙浓度、乙胺浓度、电泳电压和进样时间的优化选择，用石英芯片电泳一紫外检测法分离了纯人白蛋白和人运铁蛋白；在75mmol／L硼酸盐（pH10．55）（含0．8mmol／L乳酸钙、1％（φ）乙胺）运行缓冲液中，上述两组分在3min内完全分离；纯人白蛋白和人运铁蛋白的线性范围分别为1．0～15．0g/L和1．0～10．0g／L；检出限（S／N=3）均为0．5g／L，应用于临床尿蛋白分离测定，并与Helena琼脂糖凝胶电泳仪电泳结果进行比较，获得一致结果。     

On-chip potential gradient detection with a portable capillary electrophoresis system

A portable chip-CE system with potential gradient detection (PGD) was developed and applied to the determinations of alkali metals and alkaloids. The separation efficiency appeared to be satisfactory and nonaqueous capillary electrophoresis (NACE) proved to be applicable to PGD or conductivity detection. The power supplies, separation and detection were built on a device of 3 kg in weight. A branch channel near the end of the separation channel was designed to perform PGD and make the application of relatively high field strength possible. The study is the first report on the application of PGD on the microchip platform. The design of the chip-CE system shows several advantages, such as simplicity, miniaturization and wide applicability.