农业样品分析

本文是《分析试验室》定期评述栏目中“农业试样分析”的第２篇评述，它评述１９９２年３月至１９９４年６月国内农业测试分析的进展，包括分子光谱、原子光谱、色谱、电化学、电泳等方法，共引用文献２８０篇。     

农业样品分析

本文是本刊“农业样品分析”第三篇定期评述，对１９９４年４月至１９９８年６月（着重于近两年）国内农业测试分析的进展作了评述，包括分子光谱、原子光谱、色谱、电化学、电泳分析，共引用文献６７５篇。     

环境中锑的形态分析研究进展

评述了环境样品中痕量锑的形态分析概况及近年来的发展趋势，主要包括分光光度法、电化学方法、原子光谱法和色谱法等。     

气相富集原子光谱分析技术研究进展

作为一种简单、高效、低耗的预富集方法,气相富集技术(GPE)可作为原子光谱仪器的关键部件用以提高分析灵敏度、消除基体干扰,在原子光谱的小型化、现场化研究领域已得到广泛应用。GPE是通过氢化物发生、紫外蒸气发生、电热蒸发等进样方式使样品转换为气态分析物,被石英、碳、金属等材料捕获在富集装置中,其中捕获/释放条件也是决定元素预富集的关键因素,主要包括冷捕获、合金捕获、热捕获、介质阻挡放电等富集/释放方式。该文综述了GPE技术在原子光谱领域的研究进展,从进样方式、捕获材料、捕获/释放方式等方面进行了分析与探讨,并对其研究和应用前景进行了展望。     

环境样品分析

本文是“分析试验室”定期评述“环境试样分析”的第７篇评述。它全面评述了１９９８年１对１９９９年１２月间我国环境分析的进展,内容包括：概述,大气样品分析,水样品分析,土壤和沉积物样品分析,生物样品分析,放射性监测,标准、质量控制和质量保证,展望。     

环境中无机铬形态分析研究进展

本文对近年来环境分析化学中的一个重要分支－环境中无机铬的形态分析进展及有关分析方法的现况和发展趋势进行了概述。     

原子发射光谱分析

本文是《分析试验室》期刊定期评述中“原子发射光谱分析”课题的第一篇评述文章。文中对1987～1990年期间我国原子发射光谱分析(AES)领域所取得的进展作了全面评述。内容包括概述、火焰发射光谱法、电弧发射光谱法、火花发射光谱法、电感耦合等离子体原子发射光谱法、直流等离子体原子发射光谱法、微波等离子体原子发射光谱法、亚稳态能量转移发射光谱法、激光显微发射光谱法、空心阴极灯和Grimm灯发射光谱法等方面。     

原子光谱法测定润滑油中金属

评述了近年来原子光谱法测定润滑油中金属含量技术的沿革、方法及进展。着重介绍了原子光谱法测定润滑油中金属含量的样品前处理方法及原子光谱法测定技术。     

固相微萃取技术在农药残留分析中的应用

固相微萃取技术是一种崭新的无溶剂萃取分离技术。文中对影响萃取效果的因素进行了综述,并对固相微萃取技术在农药残留分析中的应用作出概述,引用文献56篇。     

环境水样及食品中亚硝酸根的分析进展

评述了自1997年至2002年国内外环境水样及食品中亚硝酸根(NO2^-)的分析进展。包括分子光谱法、电化学分析法和色谱分析法，引用文献96篇。     

农产品中多种残留农药的气相色谱质谱快速检测

运用气相色谱质谱联用技术实现农产品中多种残留农药的快速检测。采用改进的基质固相分散(MSPD)技术,减少了基体杂质的干扰;对土豆、白菜、胡萝卜、苹果、橘子、黄瓜以及大米进行了97种农药的加标回收检测。对于每个样品,实现包括前处理的整个分析过程只需要90 m in。大部分的农药回收率都在70%~120%之间;相对标准偏差也一般都小于10%。结果表明,该方法可以成功地应用于农产品中大范围农药的分析。     

Automation of sample pretreatment for liquid chromatography

The purpose of this review is to discuss the strategic problems of automating sample preparation (SP) for high performance liquid chromatography (HPLC). There is a general feeling that SP is the bottleneck of many HPLC procedures. Despite numerous reports of successful automation of SP, there are still many laboratories using manual or semiautomated SP procedures. This calls for a reevaluation of the present situation.     

填充吸附剂微萃取技术及其在微小体积样品萃取应用中的研究进展

微萃取技术是分析化学领域发展迅速,且已经得到广泛应用的样品前处理技术.填充吸附剂微萃取(MEPS)是一种微量固相萃取技术,使用微量的吸附剂填充于微量注射器,通过反复抽推方式使样品多次流经吸附剂以完成样品吸附萃取过程,萃取后的样品可直接用于色谱分析.典型的MEPS萃取设备包括MEPS注射器和MEPS吸附床(BIN).ME...     

微乳液毛细管电动色谱-场放大富集法灵敏分析尿液中的9种麻醉剂类药物

建立了一种微乳液毛细管电动色谱(MEEKC)-场放大富集(FASI)分析尿液中多种麻醉剂(吗啡、可待因、纳洛酮、海洛因、蒂巴因、可卡因、哌替啶、芬太尼、美沙酮)的方法。考察了微乳液组成、分离电压等因素的影响,得到的最佳微乳液组成(质量分数)为0.6%十二烷基硫酸钠、1.2%正丁醇、0.6%乙酸乙酯和97.6% 10 mmol/L硼砂缓冲液(pH 9.5);分离电压为25 kV。在上述微乳体系中,9种化合物在15 min内得到了基线分离。采用场放大在线富集技术提高了分析灵敏度,检出限(S/N=3)低至0.3 μg/L。模拟尿样样品中9种麻醉剂的加标回收率介于79.4%～119.9%之间,日内相对标准偏差小于5.5%。将该方法应用于美沙酮大鼠体外代谢样品的测定,结果令人满意。     

微流控高通量试样引入技术的研究进展

如何实现外部宏观系统与芯片微观系统之间的衔接一直是微流控芯片分析领域中一个重要的研究课题。本文结合作者所在研究组的工作及成果,介绍了当前微流控高通量试样引入技术的研究进展。其中分别介绍了基于固定储液池、流通池和取样探针3种模式的微流控芯片系统试样引入系统,以及基于毛细管的微流控高通量试样引入系统。此外,还对该领域研究发展的前景进行了展望。     

柱头场放大样品富集技术测定镍

利用毛细管电泳在线化学发光检测技术,研究了镍离子场放大样品富集过程。结果表明,利用该技术可使灵敏度显著改善,浓缩因子达5 8×104,镍离子检出限为1 2×10-10mol/L。预进一段水柱可使检出限达到7 0×10-11mol L。还考察了进样方式、样品基体浓度、进样时间、进样电压对检测灵敏度的影响。     

Effects of sample preservation and storage on mercury speciation in natural stream water

Despite an increasing focus on low level methods for determination of mercury species in water over the last decades, few studies have paid attention to direct effects of different sample preparation methods (i.e. preservation techniques) on natural freshwater samples. In this study we show how different preservation techniques give significantly different concentrations of total and methylmercury in freshwaters (9 and 14% on average, respectively). Natural stream samples from a forested lake catchment were studied. Mean stream sample concentrations of total (3.6 ng/L) and methylmercury (0.06 ng/L) reflect levels typical for pristine humic boreal catchments. The main reason for the observed average differences in total and methylmercury concentrations is the use of one instead of two sample bottles and timing of sample acidification, respectively.     

Isoelectric focusing sample injection for capillary electrophoresis of proteins

Carrier ampholyte-free isoelectric focusing (IEF) sample injection (concentration) for capillary electrophoresis (CE) is realized in a single capillary. A short section of porous capillary wall was made near the injection end of a capillary by HF etching. In the etching process, an electric voltage was applied across the etching capillary wall and electric current was monitored. When an electric current through the etching capillary was observed, the capillary wall became porous. The etched part was fixed in a vial, where NaOH solution with a certain concentration was added during the sample injection. The whole capillary was filled with pH 3.0 running buffer. The inlet end vial was filled with protein sample dissolved in the running buffer. An electric voltage was applied across the inlet end vial and etched porous wall. A neutralization reaction occurs at the boundary (interface) of the fronts of H+ and OH-. A pH step or sharp pH gradient exists across the boundary. When positive protein ions electromigrate to the boundary from the sample vial, they are isoelectricelly focused at points corresponding to their pH. After a certain period of concentration, a high voltage is applied across the whole capillary and a conventional CE is followed. An over 100-fold concentration factor has been easily obtained for three model proteins (bovine serum albumin, lysozyme, ribonuclease A). Furthermore, the IEF sample concentration and its dynamics have been visually observed with the whole-column imaging technique. Its merits and remaining problem have been discussed, too.     

Using sample qualification techniques to classify dsc records

The Similarity Match, Distance Match, Discriminant Analysis, Search Standards, and QC Compare Search techniques of statistical analysis are applied to DSC records in order to distinguish between two forms or classes of a new pharmaceutical active component. The classes are defined according to its therapeutic activity as 'positive' and 'negative'. Excellent results are obtained using the QC Compare Search Method. This revised version was published online in July 2006 with corrections to the Cover Date.