毛细管电泳在低分子量有机酸分析中的应用

本文介绍了低分子量有机酸的毛细管电泳研究方法。着重总结了各种分离模式和检测方法,并评述了近五年来,毛细管电泳在食品和环境中有机酸分析的应用进展。引用文献70篇。     

Simultaneous Determination of Inorganic Anions and Organic Acids in Environmental Samples by Capillary Zone Electrophoresis with Indirect UV Detection

Capillary zone electrophoresis (CZE) with indirect UV detection was developed for the simultaneous determination of inorganic anions and organic acids in environmental samples. Various aromatic acids (benzoic, phthalic, trimellitic, and pyromellitic acids) were evaluated as background electrolytes (BGEs) to give high resolution and detection sensitivity. Co-electroosmotic conditions such as the concentration of BGE, electrolyte pH, and EOF modifier were systematically investigated. Three inorganic anions and ten organic acids were determined simultaneously in 10 min using an electrolyte containing 10 mM phthalic acid, 0.5 mM myristyltrimethylammonium bromide (MTAB), and 5% methanol (MeOH) (v/v) at pH 5.60. Linear plots for the test solutes were obtained in the concentration range 0.01–1.0 mM with detection limits in the range 5–30 μM. The proposed method was successfully demonstrated for the determination of inorganic anions and organic acids in natural water, soil, and plant extracts after direct sample injection.     

毛细管区带电泳电化学检测器

本文阐述了毛细管区带电泳探针式安培检测器的构造、工作原理、理论及其与电泳系统的联结技术;介绍了该检测器的应用情况。     

毛细管区带电泳法对柱前衍生胆汁酸的高效分离研究

以7-氨基-1,3-萘二磺酸作为柱前衍生试剂,采用毛细管区带电泳-光二极管阵列检测器分离测定6种胆汁酸。实验综合考察了缓冲溶液浓度、pH值、温度及添加剂对胆汁酸衍生化产物分离效果的影响。在不加其它添加剂情况下,于25mmol/L的pH为9.5的硼酸盐缓冲溶液中,20℃,5kPa压力下进样,进样时间8s,13min可实现6种胆汁酸的快速高效基线分离。该方法检出限(3σ)为0.022～0.046μmol/L,线性范围为0.07～5μmol/L。     

毛细管区带电泳在氧氟沙星含量分析中的应用

氧氟沙星（ＯＦ）是第三代喹诺酮类药物中效果最好的广谱抗菌素之一。由于它在ｐＨ２～１１范围内难溶于水与醇，给用ＨＰＬＣ法检测其含量带来一定困难。本文报告了用毛细管区带电泳（ＣＺＦ）分离检测该药的方法。由于使用ｐＨ调制样品引入技术，克服了其溶解性不好给ＨＰＬＣ法所带来的困难。其实验条件为：５０ｍｍｏｌ／Ｌ硼砂（ｐＨ１．５）为电泳缓冲液，２８０ｎｍ为紫外检测波长，２５ｋＶ为电泳电压。样品由高差进样方式引入分离毛细管（５．１２ｃｍ×５０μｍｉ．ｄ．，有效分离长度为３８．５ｃｍ）。用磺胺作内标，ＯＦ在４８～５３０ｍｇ／Ｌ及５８０～９７０ｍｇ／Ｌ范围内可进行定量分析。保留时间（ｔｒ）及相对紫外吸收（Ａ（样品）／Ａ（内标））的日内－ＲＳＤ值分别小于１．０％和２．４％（ｎ＝６）。     

Separation and Determination of Bases by Capillary Zone Electrophoresis

ＳｅｐａｒａｔｉｏｎａｎｄＤｅｔｅｒｍｉｎａｔｉｏｎｏｆＢａｓｅｓｂｙＣａｐｉｌｌａｒｙＺｏｎｅＥｌｅｃｔｒｏｐｈｏｒｅｓｉｓＺＨＡＯＴａｏ,ＬＩＵＱｉ－ｐｉｎｇ,ＣＨＥＮＧＪｉｅ－ｋｅ（ＤｅｐａｒｔｍｅｎｔｏｆＣｈｅｍｉｓｔｒｙ,ＷｕｈａｎＵｎｉｖ...     

毛细管区带电泳的离子交换在柱预富集技术研究

提出了离子交换固相萃取的毛细管区带电泳在柱预富集技术。预富集毛细管和分离毛细管的端面靠紧,二者通过一段带侧孔的聚四氟乙烯（PTFE）套管固定。预富集毛细管内壁键合羧基阳离子交换基团,进样时分析离子被保留在预富集管的固定相上,用2mol／L的氯化铵溶液洗脱,再进行毛细管区带电泳分离。方法成功富集和分离了两种低浓度的药物阳离子,普萘洛尔和美托洛尔的灵敏度比常规电动进样分别提高4200和3400倍,其浓度检出限分别为0．02μg/L和0．14μg/L。     

毛细管区带电泳定量分析SD大鼠前列腺素

前列腺素具有多种生理和病理作用．本文研究了两种重要的前列腺素类物质PGE。与TXB。'的毛细管区带电泳（CZE）的分离与间接紫外吸收检测条件．发现少量磷铅酸使铬酸钾在254urn处吸收强度增加，有效地改善PGE。与TXB。的分辨率，并使间接光度检测PGE。与TXB。的灵敏度提高约5倍，适用于SD大鼠肺组织中PGE。与TXB。的测定．且实验部分1．1电泳操作所有溶液在进人毛细管分离柱之前，均用0·3Pm微孔滤膜过滤．进样在阳极端，手动高差进样，进样高度10cm，进样时间15min．l·2样品处理取SD大鼠肺组织0·500g（干样）．剪碎后加人…     

毛细管区带电泳分离硝基苯胺位置异构体的研究

采用毛细管区带电泳(CZE)技术,在极端pH值条件下分离了邻、间、对硝基苯胺位置异构体;研究了背景缓冲溶液、pH值、分离电压、温度及进样时间等因素对分离的影响,得出了3种样品的标准曲线、线性范围及加样回收率。在选定的实验条件下15min内实现了上述3种苯胺类化合物的分离。该方法快速,准确,重现性好。     

Determination of the pKa of Benzophenones by Capillary Zone Electrophoresis

Electrophoretic behavior of seven benzophenones as a function of the buffer pH was investigated, and their pK_a values were determined by capillary zone electrophoresis. The determination of pK_a allows us to rationalize the influence of the buffer pH on the migration behavior of benzophenones. The results reveal that both the presence of intramolecular hydrogen bond and the favorable π‐electronic delocalization decrease the degree of the acid dissociation of the hydroxyl groups of hydroxybenzophenones. However, the introduction of a hydroxyl group at the 4‐position or at the 2′‐position of the aromatic ring of hydroxybenzophenones would decrease greatly their pK_a1 values. Thus the presence of this type of hydrogen bonding also plays an important role in the acid dissociation of these hydroxybenzophenones.     

毛细管电泳在环境分析中的应用

以国内外近年来公开发表的科技文献为信息来源,从现状、发展优势和实际应用等方面就毛细管电泳在环境分析中的应用和发展前景予以综述。     

Separation and Migration Behavior of Benzophenones in Capillary Zone Electrophoresis

The migration behavior and separation of eight benzophenones selected were investigated by capillary zone electrophoresis in the range of pH 7.5–11.5. The effect of buffer pH, the types of buffer electrolyte, and the concentration of phosphate‐borate buffer on the separation and selectivity of benzophenones selected were examined. Better separability can be obtained with phosphate‐borate buffer than with phosphate buffer or borate buffer at around pH 9.2. Baseline separation of eight benzophenones could be simultaneously and successfully achieved with an appropriate choice of buffer pH and the concentration of phosphate‐borate buffer in capillary zone electrophoresis. The migration order of benzophenones selected could be explained on the basis of the degree of ionization and molecular mass.     

毛细管电泳柱端盘状电极安培检测区带展宽的定量分析

从理论上分析了影响毛细管电泳法端盘状电极安培区检测区带展宽的诸因素，给出了区带展宽的模拟公式，通过实验考察了进样量，分离电压，检测器体体积对区带展宽的影响并验证了模拟公式。     

毛细管区带电泳用于分离分析砷化合物的研究

采用毛细管区带电泳，以磷酸盐为缓冲溶液分离了5种砷的化合物：As（Ⅲ）、DMA、ANA、MMA和As（Ⅴ）．用紫外吸收法在191nm波长下，对实验条件进行了优化；使用扩展光程毛细管研究了实验方法的重现性；测定了各种砷化合物的峰面积与浓度的关系，在最大进样量时测定了检出限，并将该方法用于合成样品的分析．     

Simultaneous Determination of Organic Acids in Wine Samples by Capillary Electrophoresis and UV Detection: Optimization with Five Different Background Electrolytes

A simple technique is described for the routine capillary electrophoretic determination of organic acids in wine samples. Several aromatic and non‐aromatic compounds, including phthalic acid, benzoic acid, sorbic acid, boric acid, and phosphate, were evaluated as background electrolytes in order to obtain the highest resolution and detection sensivity. Factors that affect capillary electrophoretic separation such as the concentration and pH of the background electrolyte (BGE), the concentration of the electroosmotic flow modifier (EOF), and methanol addition to the electrolyte were investigated systematically. Tartaric, malic, succinic, acetic, and lactic acids were determined simultaneously in approximately six minutes using an electrolyte containing 3 mM phosphate and 0.5 mM myristyltrimethylammonium bromide (MTAB) as electroosmotic flow modifier at pH 6.5. This method is quantitative, with recoveries in the 90–102% range and linear up to 50 mg L^–1. The precision is better than 1% and the procedure shows the appropriate sensibility, with detection limits between 0.015 and 0.054 mg L^–1. The proposed method was successfully employed for the determination of organic acids in wine samples by direct sample injection after appropriate dilution and filtration.     

Optimization,Validation and Application of a Capillary Zone Electrophoresis Method for the Assay of Sparfloxacin in Pharmaceutical Formulation

Abstract

A capillary zone electrophoresis (CZE) method has been developed for the determination of the antibiotic sparfloxacin in tablets. The CZE separation was performed using 75 µm×35 cm fused-silica capillary under the following conditions: 25°C; applied voltage, 12 kV; 25 mM H₃PO₄-NaOH running buffer (pH 8.5). The detection wavelength was 254 nm. Flumequine was used as internal standard (IS). The method was suitably validated with respect to linearity, limit of detection and quantification, accuracy, precision, specificity, and robustness. The calibration was linear from 10 to 60 µg mL^?1 and the limit of detection and quantification were 5.38 and 9.46 µg mL^?1, respectively. Recoveries ranging from 95.68%–102.4% were obtained in the determination of sparfloxacin that were spiked to placebos. Excipients in the commercial tablets and degraded products from different stress conditions did not interfere in the assay. The method was successfully applied to the determination of sparfloxacin in pharmaceutical tablets.     

九种嘌呤碱的毛细管区带电泳分离

用毛细管区带电泳法分离和测定咖啡碱，９－Ｎ二羟丙基茶碱，可可碱，腺嘌呤，鸟嘌呤、茶碱、黄嘌呤、尿酸和６－巯基嘌呤，在熔硅毛细管（７０ｃｍ×７５μｍｉ．ｄ，有效长度６３ｃｍ）内，使用０．０１ｍｏｌ／Ｌ（ｐＨ＝１０）硼砂缓冲溶液，电压为２５ｋＶ温度为３０℃，真空进样１ｓ，于２６０ｎｍ处检测，可在７ｍｉｎ内分离上述到９种嘌呤碱，理论塔板数达到３．０×１０＾５，检测限达ｆｍｏｌ级，方法用于人尿分析，结果令     

16通道毛细管阵列电泳对手性氨基酸分离条件的快速筛选

利用自行研制的16通道旋转激光扫描共焦荧光检测式毛细管阵列电泳仪,我们采用了不同浓度的十二烷基硫酸钠、β-环糊精、γ-环糊精对荧光素标记丙氨酸、甲硫氨酸、色氨酸和谷氨酸4种手性氨基酸进行了手性拆分条件研究,快速地获得了这4种手性氨基酸对映体最佳的拆分条件:分离缓冲液为10 mmol/L硼酸缓冲液(pH=10),5 mmol/Lγ-环糊精为添加剂时,4种手性氨基酸全部达到了基线分离。     

Simultaneous Determination of Carbohydrates and Amino Acids by Capillary Zone Electrophoresis with Constant Potential Amperometric Detection at a Copper Electrode

Capillary zone electrophoresis with end-column amperometric detection at a copper microdisk electrode (100 μm in diameter) was successfully applied for simultaneous determination of carbohydrates and amino acids. Under the separation voltage of 27 kV and the separation electrolyte of 80 mM NaOH in a 75 cm fused silica capillary (10 μm i.d. × 375 μmU o.d.), complete separation of a standard mixture containing 9 carbohydrates and 12 amino acids was achieved in less than 25 min. With the electrokinetical injection of 5.4 s at 27 kV and the detection potential of 0.62 V vs. Ag/AgCl, the detection limits (S/N = 3) were 0.22–0.65 ppm (1.2–1.9 μM) for carbohydrates and 0.31–6.5 ppm (2.3–39 μM) for amino acids, respectively. The calculated numbers of theoretical plates were between 41,000 and 190,000. The use of this method for analysis of carbohydrates and amino acids in a urine sample was demonstrated.     

毛细管区带电泳中场增强进样柱内富集的非线性特征

直接柱头场效应进样是一种毛细管区带电泳柱内富集,其进样过程中样品在柱内的分布可分为两部分,即在运行缓冲溶液中的堆积区段和由电渗流引入的样品溶液区段.通过对溶质输运行为的研究表明:两区段长度与进样时间之间并非简单的线性关系,因此进样量与进样时间的关系也非线性,且与溶质淌度有关;进样量的增加并不能导致富集倍数的同步增加,由于层流的作用使得场效应进样柱内富集效果降低.为了在保持柱效基本不变情况下得到好的富集效果,除需使溶质在运行缓冲溶液和样品溶液中的电导率比极大外,进样时间也应与之匹配.