一种新型毛细管电泳—电感耦合等离子体光谱法接口装置

毛细管电泳是一种高效、简便的分离方法，已被用于生物、环境及临床等试样的分离及分析[1]．检测技术在毛细管电泳中占有重要的地位，目前，在柱紫外可见及荧光检测是两种广为接受的检测方法，但其检测灵敏度仅为10－5～10－6mol／L[2]．电感耦合等离子体光谱（ICP－AES／MS）是一种灵敏的元素选择性的分析方法，已被广泛地用于各种试样中元素分析．近年来，该方法作为色谱及毛细管电泳的检测器，被用于元素的形态分析[3]．在毛细管电泳（CE）与ICP光谱连用技术中，挑战性的工作是设计一种能把CE与ICP相连的接口．目前已有几种接口…     

复方新诺明片剂中有效成分的毛细管区带电泳快速测定法

研究了用毛细管区带电泳法快速测定复方新诺明片中磺胺甲恶唑（ＳＭＺ）和甲氧苄氨嘧啶（ＴＭＰ）的含量。使用长２７ｃｍ（有效长度２０ｃｍ）内径５０μｍ的石英毛细管,２５ｋＶ分离电压,在０．０５ｍｏｌ／Ｌ的乙酸盐缓冲液（ｐＨ５．５）中,上述两组分可在１．５ｍｉｎ内完全分离。用紫外检测器在２１４ｎｍ处检测,外标法定量。１０次检测含有１４１．７ｍｇ／ＬＳＭＺ和２５．６ｍｇ／ＬＴＭＰ的试样溶液,相对标准偏差为１     

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）。     

毛细管电泳法同时测定血浆中的美西律、利多卡因和布比卡因的浓度

采用毛细管电泳法同时测定血浆中关西律、利多卡因和布比卡因的浓度。取0．5mL血浆，用乙醚提取后吹干，重组后进样于毛细管电泳仪进行分离测定。电泳条件：分离用缓冲液为75mmol／L NaH2PO4溶液（pH3．0），温度30℃，运行电压26kV，紫外检测，波长200nm，压力进样5S。本法在0．1～4．0μg／mL范围内线性关系和精密度良好，方法回收率在96％～105％之间，检出限均为0．02μg／mL，可满足临床监测需要。     

毛细管电泳在拮抗药物对氨基苯甲酸，对羟基苯甲酸和磺胺分析测…

本报道了一种用毛细管区带电泳法分离与测定对氨基苯甲酸、对羟基苯甲酸及磺胺类药物的新方法。电泳条件为：用２０ｍｍｏｌ／Ｌ硼砂－２０ｍｍｏｌ／ＬＨ３ＰＯ４－２０ｍｍｏｌ／Ｌβ－环糊精－４％乙醇作电泳液，Ｌ－抗坏血酸为内标，２８０ｎｍ为检测波长，样品由电进样方式１０ｋＶ／１０ｓ）引入毛细管（５１．２ｃｍ×５０μｍｉ．ｄ．，有效分离长度为３８．５ｃｍ）．在２４．５℃下，６ｍｉｎ内三可达基线分离（电泳电     

毛细管区带电泳法快速测定复方布洛芬片的有效成分

 研究了用毛细管区带电泳法快速测定复方布洛芬片中布洛芬和伪麻黄碱含量的方法。在０．０２５ｍｏｌ／Ｌ的磷酸盐缓冲液（ｐＨ８．１）中，上述两组分可在３ｍｉｎ内得以完全分离，用紫外检测器在２１０ｎｍ处检测，并以外标法定量。１１次测定含有９．５ｍｇ／Ｌ盐酸伪麻黄碱和６６．７ｍｇ／Ｌ布洛芬的试样溶液，相对标准偏差为２．９％（伪麻黄碱）和１．９％（布洛芬），回收率为１０３．１％（伪麻黄碱）和９７．６％（布洛芬）。应用毛细管区带电泳法测定复方布洛芬片剂的含量，所得结果与ＨＰＬＣ法一致。     

毛细管区带电泳法快速测定复方布洛芬片的有效成分

研究了用毛细管区带电泳法快速测定复方布洛芬片中布洛芬和伪麻黄碱含量的方法。在０．０２５ｍｏｌ／Ｌ的磷酸盐缓冲液（ｐＨ８．１）中，上述两组分可在３ｍｉｎ内得以完全分离，用紫外检测器在２１０ｎｍ处检测，并以外标法定量。１１次测定含有９．５ｍｇ／Ｌ盐酸伪麻黄碱和６６．７ｍｇ／Ｌ布洛芬的试样溶液，相对标准偏差为２．９％（伪麻黄碱）和１．９％（布洛芬），回收率为１０３．１％（伪麻黄碱）和９７．６％（布洛芬）。应用毛细管区带电泳法测定复方布洛芬片剂的含量，所得结果与ＨＰＬＣ法一致。     

毛细管区带电泳法测定十全大补丸中的川芎嗪和芍药甙

川芎嗪和芍药甙是十全大补丸中的主要有效成分。本文用毛细管区带电泳法分离测定了这两种成分。以40mmol/L硼砂（含3％乙醇,V／V）、pH10．88为电泳介质,未涂层熔融硅毛细管,压力进样（69kPa·s）,15kV恒压电泳（23℃）,检测波长232nm。在20～700mg/L和15～55mg／L范围内,川芎嗪与芍药甙可分别定量分析。加样回收率川芎嗪为101．0％±1．8％,芍药甙为99．3％±2．0％。     

毛细管电泳安培法检测中的在柱场放大效应

本文首次报道用安培电化学检测器探讨毛细管电泳分离的场放大进样效应，分析了系统峰的形成以及场放大进样对电泳分离检测的影响。采用２５μｍ内径毛细管电泳分离，对去甲肾上腺素（ＮＥ）和儿茶酚（ＣＡＴ）分别可达０．４ｎｍｏｌ／Ｌ和１．５ｎｍｏｌ／Ｌ的浓度检测限，有效提高了毛细管电泳安培法检测的灵敏度。     

稀土离子及胺和氨基酸的高效毛细管区带电泳电导检测

用自制高效毛细管电泳装置研究毛细管电泳电导检测，由用阴离子交换膜管制作的导电接口连接电泳毛细管和电导池，高电压被有效隔离，实现柱后电导检测，用长６０ｃｍ、内径５０μｍ石英毛细管，以ｐＨ４．０的７×１０￣（－３）ｍｏｌ／ＬＮａＡｃ￣（－２）×１０￣（－３）ｍｏｌ／ＬＨＩＢＡ－ＨＡＣ溶液为载体，在１８ｋＶ电压下，轻重三种稀土Ｎｄ、Ｇｄ、Ｙｂ的混合物８ｍｉｎ内完成分离检测。用上述毛细管，以ｐＨ为５．８的５×１０￣（－３）ｍｏｌ／ＬＮａＡｃ－ＨＡＣ溶液为载体，在２０ｋＶ电压下乙二胺、三乙胺、组氨酸、谷氨酸混合有机物７．５ｍｉｎ内完成分离检测。     

System Suitability in an Optimized HPLC System

Abstract

The relationship between calibration, validation and system suitability is demonstrated within the chemometric framework. The importance of system suitability is stressed and its interrelationship with mobile phase optimization is discussed. In addition, it is shown that sensitivity data generated in a mobile phase optimization study can be used to effectively set system suitability criteria and make improvements to an unacceptable chromatographic system.     

光致变色高分子体系

对光致变色功能高分子作了概括性综述，介绍了各类体系的光致变色机理，制备方法，应用研究等方面的进展情况。     

The NCI Drug Information System. 1. System overview

An interactive computer system has been designed to handle all the data associated with the National Cancer Institute's (NCI) drug screening program. The system resides on the NIH DEC System 10 computers and allows interactive access to the entire NCI screening data system. This contains over 20 separate databases, including a chemistry file of about 400,000 structures and a biology file of approximately 1.5 million test records. New compounds and test data are added daily to the files, and the system also controls and records all the daily operations of the screening program, such as acquisition, shipping, and biological testing of chemicals.     

The NCI Drug Information System. 6. System maintenance

The NCI Drug Information System (DIS) is a collection of 24 interactively searchable databases which contain all the data associated with NCI's drug screening program. Data flow into all of these databases upon a daily basis, and maintenance procedures have been developed which provide a high degree of currency to the files. An extensive security system controls both write access and read access to the DIS and matches both to the authorization possessed by each specific user. Detailed usage statistics are collected automatically. The cost of the overall system in terms of both manpower and machine time is discussed briefly.     

Cyclohexane-Dodecane Binary System

Russian Journal of General Chemistry -     

The Allylcobalt System

The following report describes the preparation and reactions of organocobalt compounds, especially the thermally unstable tris(π-allyl)cobalt and cyclooctenylcobalt compounds. The stoichiometric and catalytic transformations of these highly reactive organocobalt systems give an insight into the rôle of cobalt in homogeneous catalysis involving alkenes and alkynes.     

Metal Vector Manipulated Molecular Self-Assembly from Werner System to Cotton System

A definition of metal vector was given to coordinatively unsaturated metals or asymmetrically coordinated metal complexes in which the metal center is partly blocked by inert chelating ligand(s), thus possess specific reactivity and directionality, such as cis-coordinated square Pd(Ⅱ) or Pt(Ⅱ) complexes. Metal vectors have been extensively used in coordination catalysis and molecular assembly. In 1990, Fujita [ 1 ] first demonstrated the utility of cis-coordinated square Pd(Ⅱ)or Pt(Ⅱ) complexes as a right angular 2D metal vector in the formation of molecular square, a cyclic tetramer with nano-cavity and unique molecular recognition. So far, much attention has been paid to the use of the mononuclear coordination centers (Werner-type metal vectors) in molecular assembly.As late as 1999, Cotton et al. [2] reported the use of cis-coordinated metal-metal bonded dimetal units (Cotton-type metal vectors) to direct assembly of molecular squares.This presentation includes two parts: 1) Werner-type metal vector directed molecular assembly; [3]2) Cotton-type metal vector directed molecular assembly.[4]Firstly, the Werner-type metal vector, cis-coordinated Pd(Ⅱ) nitrate, was used to direct a 6-component self-assembly. This leads to the formation of a molecular bowl or crown with syn,syn,syn conformation. These structures are analogues of calix[3]arenes and can function as anion receptors. Interestingly, an nitrate is found to distort from a trigonal plane into a trigonal pyramid when binding to the bottom of the molecular bowl.Secondly, the Cotton-type metal vector, cis-diRh(Ⅱ, Ⅱ), was used to assemble di- or poly-carboxylate anions into neutral supermolecules. Most interestingly, a calixarene-based carceplex with four cis-diRh(Ⅱ, Ⅱ) fastners was obtained[5].All self-assembling entities were studied by both X-ray crystallographic analysis and solution NMR spectra, which are consistent with the presence of assembling structures even in solution.     

环糊精-石墨烯超分子体系

环糊精是由D型吡喃葡萄糖通过α-1,4-糖苷键连接而成的环状超分子主体化合物,其特殊的结构赋予了其良好的分子识别性能;石墨烯是仅由单层sp杂化的碳原子构筑的具有良好的电化学性能的材料.作为著名的"明星分子",石墨烯类材料无疑是近5年来研究热点之一.在各种各样的石墨烯材料中,由环糊精-石墨烯联合构筑的超分子体系在保留二者优良性能的同时又引入了新的功能特点.综述了近些年来新发展起来的环糊精-石墨烯超分子体系:通过二者作用方式进行了分类,分为共价键连接和非共价键连接;综述了该超分子体系在药物运输及释放、电化学检测(包括对药物分子、污染物和生物分子的检测)等领域的应用;最后对该体系在药物负载及释放、模拟生物固氮、燃料电池、研究电子传导等应用前景进行了展望.