高效毛细管电泳－电荷耦合器件检测器联用技术研究Ⅰ．多波长荧光检测装置

报道了用电荷耦合检测器等设备组成的高效毛细管电泳多波长荧光检测装置。以荧光素和罗丹明Ｂ对其性能进行了评价,得到了具有光谱和时间分辨的三维电泳图,与被测物标准荧光光谱对照,可以直接鉴定被分离的化合物。     

反相高效液相色谱法的多波长同时测定预混合饲料中的脂溶性维生素A，α－E，D_3，K_3

反相高效液相色谱法的多波长同时测定预混合饲料中的脂溶性维生素Ａ，α－Ｅ，Ｄ＿３，Ｋ＿３李桂凤，李缙扬，郝征红，聂燕，孟兆宏，李学春（山东省农业科学院中心实验室济南２５０１００）１前言对脂溶性维生素的分析，被许多国内外分析专家认为是高难度的分析项目。本...     

寡糖—8—氨基芘—1,3,6—三磺酸衍生物的毛细管电泳—激光诱？…

利用自组装的毛细管电泳－激光诱导荧光装置,研究了多种寡糖－８－氨基芘－１,３,６－三磺酸（寡糖ＡＰＴＳ）衍生物的分离。考察了电泳介质、浓度及pＨ对寡糖－ＡＰＴＳ 衍生物分离的影响,在酸性和碱性条件下,分别实现了痕量寡糖标准品及葡聚糖水解产物的高效分离。     

磷脂酰胆碱LB单分子膜诱导下KDP晶体取向生长的研究

有机超薄膜诱导晶体生长是在化学、物理与生物多门学科相互交融的基础上发展起来的新兴学科 ,并逐渐成为仿生合成的重要分支 [1] .目前的研究重点主要集中于以有机化合物 LB膜作为模板剂诱导生物矿化材料上 [2～ 5] .磷脂 LB膜是生物膜的简化模型体系 [6 ] ,用它作模板剂将使该领域的研究进一步接近生物体系 .对晶体而言 ,修饰晶体材料的特征对于改善和测定材料的光学性能至关重要 [2 ] ,但目前有关上述领域的研究几乎均是空白 .KH2 PO4 ( KDP)晶体是性能优良的非线性光学材料 [7] ,本文首次以磷脂分子 LB膜作为模板剂诱导 KDP的晶化…     

Amperometric Determination of Cr(III) and Cr(VI) by Flow Injection Analysis

Speciation of Cr(III) and Cr(VI) can be attained by flow injection analysis with amperometric detection. Cr(VI) is reduced in an acidic medium to Cr(III) with a glassy carbon electrode at —0.1 V vs. Ag/AgCl and the current is recorded. Cr(III) is oxidised on-line to Cr(VI) with alkaline hydrogen peroxide solution. From the difference of the total chromium and Cr(VI), the amount of Cr(III) was obtained. A linear calibration curve for Cr(VI) was obtained for the concentration ranges 0.01-5.0ppm of Cr(VI) and we have calculated the limit of determination to be about 0.5ppb. We have studied the degree of reproducibility obtained using the solid electrodes under various conditions. The influence of flow rate, coil length, interfenences and the extent of reaction were studied.     

A Rapid and Efficient Way to Dynamic Creation of Cross‐Reactive Sensor Arrays Based on Ionic Liquids

Based on the simple counterion exchange of ionic liquids, a rapid, facile, and efficient strategy to create a cross‐reactive sensor array with a dynamic tunable feature was developed, and exemplified by the construction of a sensor array for the identification and classification of nitroaromatics and explosives mimics. To achieve a good sensing system with fast response, good sensitivity, and low detection limit, the synthesized ionic liquid receptors were tethered onto a silica matrix with a macro‐mesoporous hierarchical structure. Through the facile anion exchange approach, abundant ionic‐liquid‐based individual receptors with diversiform properties, such as different micro‐environments, diverse molecular interactions, and distinctive physico‐chemical properties, were easily and quickly synthesized to generate a distinct fingerprint of explosives for pattern recognition. The reversible anion exchange ability further endowed the sensor array with a dynamic tunable feature as well as good controllability and practicality for real‐world application. With the assistance of statistical analysis, such as principal component analysis (PCA) and linear discrimination analysis (LDA), an optimized‐size array with a good resolution was rationally established from a large number of IL‐based receptors. The performed experiments suggested that the ionic‐liquid‐based sensing protocol is a general and powerful strategy for creating a cross‐reactive sensor array that could find a wide range of applications for sensing various analytes or complex mixtures.     

Application of hot platinum microelectrodes for determination of flavonoids in flow injection analysis and capillary electrophoresis

The determination of quercetin and rutin by flow injection analysis (FIA) and capillary electrophoresis (CE) using electrochemical detection was described. These flavonoids were determined at normal (unheated) and hot platinum microelectrodes using cyclic voltammetry. When quercetin or rutin is reaching the platinum electrode, a change of the current in the region of the platinum oxide formation is observed. Integration of the current changes in this in this region creates analytical signals in the form of peaks. An increase of temperature to about 76 ?C in a small zone adjacent to the microelectrode causes an increase of the analytical signal by more than 6 times under FIA conditions. This method enables the use of hot microelectrodes as detectors in HPLC or CE. In CE the improvement of the analytical signal at hot microelectrodes is smaller than in FIA and increase only 1.3–3.4 times. Heated microelectrodes were used for analysis of the flavonoids in natural samples of the plant (extract of sea buckthorn) and a pharmaceutical preparation (Cerutin).     

Biparametric potentiometric analytical microsystem for nitrate and potassium monitoring in water recycling processes for manned space missions

The construction and evaluation of a Low Temperature Co-fired Ceramics (LTCC)-based continuous flow potentiometric microanalyzer prototype to simultaneously monitor the presence of two ions (potassium and nitrate) in samples from the water recycling process for future manned space missions is presented. The microsystem integrates microfluidics and the detection system in a single substrate and it is smaller than a credit card. The detection system is based on two ion-selective electrodes (ISEs), which are built using all-solid state nitrate and potassium polymeric membranes, and a screen-printed Ag/AgCl reference electrode. The obtained analytical features after the optimization of the microfluidic design and hydrodynamics are a linear range from 10 to 1000 mg L⁻¹ and from 1.9 to 155 mg L⁻¹ and a detection limit of 9.56 mg L⁻¹ and 0.81 mg L⁻¹ for nitrate and potassium ions respectively.     

CZE study on adsorption processes of aliphatic and aromatic amines on PMMA chip

Adsorption processes on a PMMA chip linked with CZE separations of a group of 13 aliphatic and aromatic mono‐ and di‐amines were studied. Due to the lack of chromophores within aliphatic amines, contact conductivity detection implemented directly onto the chip was used for monitoring of cationic CZE separations. To prevent an adsorption of studied amines to the chip channels, the surface of PMMA chip was modified by dynamic coating. Different surface modifiers, such as aliphatic oligoamines (diethylenetriamine and triethylenetetramine), were added to the BGE solutions filling the chip channels. The effect of various concentrations of surface modifiers on peak profiles and separation parameters of amines was monitored. Of these, mainly, aliphatic di‐amines and aromatic mono‐amines adversely affected the CZE resolution of a whole group of analytes by their strong adsorption to the chip channels. A propionate BGE with pH 3.2 containing 100 μM triethylenetetramine and 25 mM 18‐crown‐6‐ether was found suitable for CZE resolution of 12 from a total of 13 amines studied. Simple dynamic modification of the surface of PMMA chip enabled fast (analysis time lasted 9 min), sensitive (sub‐μM LODs reached) and reproducible (1–3% RSD of the peak areas) CZE analysis of the aliphatic and aromatic amines.     

Electrolyte system strategies for anionic isotachophoresis with electrospray‐ionization mass‐spectrometric detection. 1. Regular isotachophoresis and free‐acid isotachophoresis

The subject of this work is the definition of a simple model based on general ITP theory that allows describing and predicting the behavior of ITP systems compatible with ESI‐MS detection. The model is exemplified by anionic ITP of weak acids that represent an interesting potential application field of ITP‐ESI‐MS. Suitable ESI‐compatible electrolyte systems of very simple composition are proposed including a special free‐acid ITP arrangement. The properties of these systems are discussed using illustrative diagrams of their stacking windows. The use of anionic ITP‐ESI‐MS in negative‐ion ESI mode is reported for the first time and its suitability for sensitive trace analysis is demonstrated. The presented ITP‐ESI‐MS application example comprises a free‐acid ITP system formed of formic and propionic acids and direct injection analysis of ibuprofen and diclofenac in waters with quantitation limits of the order 10^?10 M.