基于适配体-金纳米粒子和光热-激光背向散射干涉技术的水中As(Ⅲ)的定量检测

针对As(Ⅲ)的检测问题,提出了一种基于适配体-金纳米粒子探针和光热-激光背向散射干涉原理的水中As(Ⅲ)的定量检测技术.结合了As(Ⅲ)适配体的金纳米粒子溶液呈现稳定的酒红色,对绿光有较强的吸收作用.采用532 nm的激光照射毛细管内的金纳米粒子溶液,由于光热效应溶液折射率发生变化,激光背向散射干涉(Back-Sca...     

高效毛细管电泳—激光干涉折射法测定多元醇的研究

本文应用高效毛细管电泳、激光干涉折射检测法研究了多元醇在四硼酸钠溶液中电泳行为。详细探讨了溶液ｐＨ值，四硼酸钠浓度及多元醇的结构对多元醇－硼酸配位离子淌度的影响。确定了高效毛细管电泳直接分离、激光干涉检测多元醇的新方法。     

激光回射束干涉相移效应的研究

激光回射束干涉相移效应的研究邓延倬，何金兰（武汉大学分析测试科学系，武汉，４３００７２）关键词激光，折射指数，干涉相移效应，毛细管电泳基于激光回射束干涉相移效应，曾首次用于光热测量［１］和微体积样品检测［２］．本文讨论这种效应的基本原理及其用于分析化...     

高效毛细管电泳中的激光光热检测技术

集中介绍了激光光热分析在高效毛细管电泳检测上的应用；分析了各种光热检测构型的特点，阐述了影响光热信号的各种因素；指出了激光光热检测技术在高效毛细管电泳中的应用前景。     

高效毛细管电泳,激光干涉检测快速分离二糖研究

首次报道一种高效毛细管电泳、激光干涉折射检测快速分离二糖的新方法。详细研究了四硼酸钠溶液中，ｐＨ值、四硼酸钠浓度及有机添加剂对二糖－硼酸络离子迁移行为的影响，发现在ｐＨ为９．７的０．１ｍｏｌ／Ｌ四硼酸钠溶液中，１０ｍｉｎ内４种二糖得到基线分离。采用自制激光干涉型折射指数检测器，不需对二糖衍生化处理，可直接进行在柱检测。     

单糖、多元醇亚砷酸络合物毛细管电泳分离研究

采用激光干涉检测方法系统研究了单糖、多元醇亚砷酸络合物的电泳行为;并考察了溶液中ｐＨ值、亚砷酸盐浓度对单糖、多元醇亚砷酸络合物淌度的影响。实验结果表明,在亚砷酸溶液中,单糖和多元醇的选择性好,峰形尖锐;从而建立了一种单糖、多元醇毛细管电泳分离及直接检测的新方法。     

激光光热干涉光谱分析方法研究

本工作设计了一种新的激光光热干涉光谱装置,类似于Mach-Zehnder干涉仪的光路构型,采用探测束聚焦和泵浦束与探测束相交的光学结构,光路容易调整稳定性较好.文章讨论了方法的原理,详细研究了影响光热干涉信号的实验参数,获得结晶紫的检测下限为8.0×10~(-8)mol/L,相应的最小吸光度为3.6×10~(-6)。     

毛细管电泳-激光干涉检测法测定饮料中蔗糖含量

本文将毛细管电泳-激光干涉检测法用于饮料中蔗糖的定量测定.结果表明,在样品浓度低于10mg/mL时,检测信号与样品浓度成正比.样品不需衍生化处理直接进行测定,分析结果较为满意.     

毛细管电泳-间接紫外法测定饮用水中草甘膦、草铵膦及其代谢产物

提出了毛细管电泳-间接紫外分析方法测定饮用水中草甘膦及其代谢产物氨甲基膦酸、草铵膦及其代谢产物3-甲基磷酸亚基丙酸。样品与25mmol·L-1乙酸铵溶液混匀后,采用SAX型固相萃取小柱提取待测物。洗脱液经毛细管电泳分离,以o-磷酸基-DL-苏氨酸为内标物,紫外检测波长为214nm。草甘膦、草铵膦、氨甲基膦酸和3-甲基磷酸亚基丙酸的线性范围为0.10~20.0mg·L-1,检出限(3S/N)分别为0.22,0.30,0.18,0.03mg·L-1,加标回收率在82.1%~108%之间。     

根际土壤溶液中磷的毛细管电泳分析

应用毛细管区带电泳间接紫外吸收法,对测定根际土壤溶液中PO43-的检测波长、电泳温度、分离电压和电解液组成等参数进行了选择,发展了根际土壤溶液中PO34-浓度的毛细管电泳分析法。选择后的电泳条件为:电解液为32mmol/L三羟甲基氨基甲烷+4mmol/L1,2,4-苯三酸+0.3mmol/L十六烷基三甲基溴化铵(pH=8.5);检测波长为205nm,分离电压为-20kV,温度为25℃。本方法有效地屏蔽了土壤溶液中Cl-,SO42-和NO3-等离子对PO43-测定的影响,对根际土壤溶液中PO43-的检出限为0.68mg/L(S/N=3);回收率为87.2%～99.4%,适于测定微量根际土壤溶液样品中PO34-的浓度。     

Indirect thermo-optical detection for capillary electrophoresis

Indirect thermo-optical detection for capillary electrophoresis is described first. A 20 mW helium-neon laser (632.8 nm) was used to provide the pumping beam and a 2 mW helium-neon laser (632.8 nm) supplied as the probe beam; Methylene Blue dye was used as a background absorber. The addition of ethanol to the background electrolyte solution can be performed to reduce adsorption of Methylene Blue onto the capillary wall. The detection method was applied to the detection of amino acids separated by capillary electrophoresis. The detection limit for lysine was 5 × 10⁻⁶ mol l⁻¹ (signal-to-noise ratio, 2).     

Assay of protein drug substances present in solution mixtures by fluorescamine derivatization and capillary electrophoresis.

A method is described to enhance the resolution and detection sensitivity of proteins, peptides, and amino acids in capillary electrophoretic analysis of solution mixtures. The method consists of derivatizing the analytes with fluorescamine, which is normally used as a fluorogenic reagent for compounds containing a reactive primary amine functional group, and then using the derivative as an ultraviolet chromophore to enhance detection sensitivity (measured at 280 nm) in capillary electrophoresis. The results demonstrated a significant improvement in the separation and detection sensitivity of the derivatized analytes as compared to their underivatized counterparts. The use of chromophores, such as fluorescamine, in capillary electrophoresis facilitates the analysis of components of solution mixtures, such as pharmaceutical formulations, that could not be resolved and/or detected by conventional capillary electrophoresis procedures.     

Sub-femtomole determination of DABSYL-amino acids with capillary zone electrophoresis separation and laser-induced thermo-optical absorbance detection

Fifteen amino acids are determined as the DABSYL (4-4-dimethylaminoazobenzene-4'-sulfonyl chloride) derivative with capillary zone electrophoresis separation and low-power laser-induced thermo-optical detection. Separation efficiencies are on the order of 200 000 theoretical plates and the detection limit, 3 s, is 200 attomole of glycine injected onto the column. At the detection limit, 0.7 attomole of glycine is present within the 40 picoliter detection volume.     

毛细管区带电泳法测定复方磷酸可待因溶液有效成份

应用毛细管电泳法测定了复方磷酸可待因溶液中磷酸可待因、盐酸麻黄碱、扑尔敏的含量。毛细管电泳的条件为 :37cm× 5 0 μm i.d(有效长度 30 cm)未涂层石英毛细管柱 ;分离电压 :1 5 k V;缓冲溶液 1 5 0 mmol/L NH4 Ac- H3PO4 ( p H2 .0 )。研究了方法的线性范围、精密度、回收率等 ,测定了三批样品。实验证明方法简便、快速、准确     

毛细管电泳法进行化妆品中砷的形态分析

从样品前处理、毛细管电泳修饰、进样方式、分离模式和检测条件等方面对毛细管电泳法研究化妆品中砷的形态进行讨论。在不同pH值的缓冲溶液中,用毛细管电泳法进行化妆品中砷的形态分析,测定波长为197nm。采用磷酸盐缓冲溶液,化妆品中As(Ⅲ)、二甲基胂(DMA)、对氨苯基胂酸(ANA)、一甲基胂(MMA)和As(V)等5种形态的砷可通过毛细管电泳法得到有效分离。     

高效毛细管电泳技术测定肌苷口服液的含量

介绍了应用高效毛细管电泳技术测定肌苷口服液含量的方法。实验是将肌苷口服液直接进样,以硼酸－硼酸盐为缓冲溶液。实验的回收率为９５．０％～９９．８％,相关系数０．９９８５,精密度的变异系数小于５％。方法简便、快速、准确、灵敏度高。     

Capillary zone electrophoresis separations of enantiomers present in complex ionic matrices with on-line isotachophoretic sample pretreatment.

Analytical capabilities of capillary zone electrophoresis (CZE) with on-line coupled capillary isotachophoresis (ITP) sample pretreatment in the column-coupling capillary electrophoresis equipment to separate and determine enantiomers present in multicomponent ionic matrices were studied. Tryptophan was used as a model analyte in the ITP-capillary zone electrophoresis experiments performed in this context while a 90-component model mixture of UV-light absorbing organic anions and urine served as multicomponent sample matrices. Various working modes in which the on-line coupled capillary isotachophoresis-capillary zone electrophoresis combination in the column-coupling separation system can operate were employed in the anionic regime of the separation with direct injections of the samples. Advantages and limitations of these working modes in the separations of enantiomers present in model and urine matrices were assessed. Experiments with model mixtures of tryptophan enantiomers revealed that the two were resolved in the capillary zone electrophoresis stage with the aid of alpha-cyclodextrin also when their concentration ratio in the sample was 1:200 while the concentration of L(-)-tryptophan was 25 nmol/l. The limits of detection for the enantiomers were at approximately 10 nmol/l (approximately 1.5 ng/ml) concentrations for a 220 nm detection wavelength of the UV detector employed in the capillary zone electrophoresis stage and for a 30 microliters sample load. A high sample load capacity of the on-line coupled capillary isotachophoresis stage was effective in separating the samples corresponding to 3-6 microliters volumes of undiluted urine. The results from the runs with urine samples showed that only the capillary isotachophoresis-capillary zone electrophoresis combination with a post-column on-line coupled capillary isotachophoresis sample clean-up (responsible for a removal of more than 99% of the sample anionic constituents migrating in the on-line coupled capillary isotachophoresis stack and detectable in the capillary zone electrophoresis stage) provided a universal alternative for the detection and quantitation of the model analyte (L(-)-tryptophan).     

Analysis of a biopolymer by capillary electrophoresis with a chemiluminescence detector using a polymer solution as the separation medium.

We developed capillary electrophoresis with a chemiluminescence detector using a polymer solution as the separation medium for the analysis of biopolymers, such as DNA and protein. A peroxyoxalate chemiluminescence reagent of bis(2,4,6-trichlorophenyl)oxalate was used together with fluorescein-labeling reagent. When a migration buffer solution containing carboxylmethylcellulose was used, the flow-type chemiluminescence detection cell was found to give a better resolution than the batch-type one. Fluorescein-labeled adenosine triphosphate of 1.0 x 10(-4) M was examined by means of capillary electrophoresis with absorption (260 nm), fluorescence (ex. 496 nm and em. 517 nm), and chemiluminescence detectors. The chemiluminescence detection showed the highest sensitivity among them; the S/N ratios obtained by absorption, fluorescence, and chemiluminescence detections were 4, 38, and 130, respectively. Fluorescein-labeled DNA was prepared through a polymerase chain reaction using fluorescein-labeled deoxyadenosine triphosphate. A mixture of the labeled DNA fragments (500, 600, 700, 800, 900, and 993 bp) was successfully separated and detected by the present system. A mixture of proteins (lysozyme, cytochrome C, and ribonuclease A) which were labeled with fluorescein isothiocyanate was also separated and detected.     

Determination of trace RA by capillary electrophoresis-solid-phase microextraction with direct UV detection

A new method of offline solid-phase microextraction coupled with capillary electrophoresis (CE) [in an uncoated capillary using borax and boric acid in acetonitrile-water (40:60) as the running buffer] with UV detection at 254 nm is presented and used for direct determination of trace biomedically important retinoic acid (RA) without any derivation. As low as 138 ng/mL RA in aqueous solution can be determined using CE with UV detection with a concentration factor of 19.6 times.     

毛细管区带电泳法测定尿中甲酸含量

采用高效毛细管区带电泳法测定人体尿中甲酸含量,尿样经过滤后直接进样,方法简单、快速,测定结果令人满意。电泳电解质体系采用５ｍｍｏｌ／Ｌ邻苯二甲酸氢钾,０．５ｍｍｏｌ／Ｌ十六烷基三甲基溴化铵,ｐＨ６,５０ｃｍ×５０μｍｉ．ｄ．熔融石英毛细管（有效长度４８．５ｃｍ）,检测波长２１０ｎｍ,负电源,分离电压３０ｋＶ,压力进样,恒温２５℃,每次电泳前用０．１ｍｏｌ／ＬＮａＯＨ及缓冲溶液对毛细管各冲洗５ｍｉｎ。同时,采用检测波长与参比波长对调的方法使负峰转变为正峰。