氰化物检测方法研究进展

对应用于氰化物的检测方法如色谱法、光谱法、电化学法、硝酸银滴定法及快速检测试纸条法等的现状（主要在1992～2011年间发表的文献）及相关的原理和方法的特点之处作了综述（引用文献38篇）。     

荧光探针在氰化物分析中的研究进展

氰化物极易与细胞色素氧化酶键合,抑制电子转移、导致组织缺氧,从而显示较强的毒性。荧光化学传感器作为简易、灵敏且可视化的方法广泛应用于氰化物的检测。本文对荧光探针在氰化物检测中的应用进行综述,概述了氰化物的毒性机制和荧光探针对氰化物的响应机理。同时,本文总结了荧光探针在水体、食品和生物组织中对氰化物的检测及生物成像中的应用,并对荧光探针在结构设计中如何提高生物兼容性和靶向性等进行了展望,以期为光化学探针分子的设计及应用提供理论与研究依据。     

数码比色法测定环境及生物样品中的氰化物浓度

在传统氰化物检测方法的基础上,提出了一种新的方法—数码比色法。在一定条件下,苦味酸与氰化物生成黄色化合物,用数码相机对显色溶液拍照,通过数码比色,进行灰度处理,照片的三原色值与氰化物的浓度成线性关系,可以直接分析出其氰化物的浓度。对唾液样品测定,其回收率为98.18%,对照品测定的相对标准偏差RSD为1.5%。研究结果表明,数码比色法具有准确度和精密度都比较理想,方便快速、环境友好等特点。     

流动注射光度法测定水中氰化物

基于氯化氰与1,3 二甲基巴比妥酸和吡啶 4碳酸在缓冲条件下反应,产生红色络合物的原理,提出了用流动注射光度法(CFA)测定自来水中氰化物。该方法线性范围为0～40.0μg·L-1,精密度和准确度高,检出限为0.002mg·L-1,适用于自来水中微量氰化物的检测。分析频率为30个样品·h-1,特别适合大批样品的测定。     

工业废水中微量铜（Ⅱ）和氰化物的流动注射光度分析

采用ＦＩＡ技术，以光度比色法为基础，建立了工业废水中微量Ｃｕ＾２＋和ＣＮ＾－的顺序自动分析方法和装置。其对二种离子的测定频率为６０样／ｈ，相对标准偏差＜１．０％，工作曲线的ｒ值≥０．９９９，各项分析技术指标均优于手工法操作。     

微孔膜气体扩散分离流动注射光度法测定废水中氰化物

研究了利用吡啶-巴比妥酸显色体系反应的中间产物,采用微孔膜气体扩散分离流动注射分析技术测定工业废水中氰化物,该法具有简便、快速并能消除某些干扰的特点。进样频率为65个样/h,检出限为0.02μg/ml,取氰化物2.5μg/ml时测量的相对标准偏差为0.3％(n=20),测定实际样品结果令人满意。     

流动注射-分光光度法测定水中氰化物

使用流动注射(FIA)-分光光度法测定水中的氰化物的含量,并与传统分光光度法的分析结果进行比对。实验证明流动注射(FIA)-分光光度法操作简便、线性好,灵敏度、精密度、准确度都能符合分析工作要求。检出限为0.2μg/L,适用于水中微量氰化物的检测。分析频率为每小时30个样品,特别适合大批样品的测定。     

鲁米诺-氰化物化学发光反应的研究——环境水样中氰化物的测定

本文提出了利用鲁米诺-氰化物化学发光体系测定氰化物的新方法。方法的检出限是1.2ng/ml,校正曲线在2～100ng/ml CN~-范围内具有良好的线性。相对标准偏差小于4％。此方法已用于自来水和工业废水中氰化物的测定。文中对鲁米诺与氰化物化学发光反应的可能机理作了初步探讨。     

水中易释放氰化物能力验证样品的研制及应用

根据国家地表水环境质量监测网监测任务要求和环境监测的实际需要,制备了水中易释放氰化物能力验证样品。通过均匀性、稳定性检验以及量值一致性评价,研制的样品均匀性良好,在3℃~6℃冷藏避光保存条件下1年内稳定,样品配制值与多家实验室协作测定结果一致。探讨了样品在能力验证活动中的应用,共有来自全国11个省的32家实验室参加了水中易释放氰化物的能力验证计划,实验室满意率在80%以上,实验室结果出现有问题或不满意主要是由于样品前处理以及检测过程质量控制不当导致的。经检测及实验室反馈的数据验证,该能力验证样品能够应用于能力验证活动。     

基于氰化物对辣根过氧化物酶的抑制作用测定氰化物的研究

基于氰化物对辣根过氧化物酶(HRP)的抑制作用,将辣根过氧化物酶电极用于水中的微量氰化物的测定。酶电极制作中,先在金电极表面自组装一层半胱胺单层膜,再用戊二醛交联HRP。采用这种酶固定化方法,电极在6.0×10-5～4×10-3mol/LH2O2的浓度范围呈线性关系。探讨了工作电位、介体浓度、pH值、底物浓度等实验条件对酶电极性能及抑制过程中响应电流的影响,考察了电极的重现性、干扰及使用寿命。电极检测氰化物的线性范围为0.3～20μg/mL,检出限为100ng/mL,将电极用于水中CN-回收率的测定,结果良好。     

化学毒剂探测技术发展现状

化学毒剂(CWAs)作为一种大规模杀伤性武器,具有杀伤力强、影响范围广、防护困难、易于制作施放等特征,从诞生之初即常被用于战争冲突,在现代非对称战争、恐怖袭击中也造成了巨大威胁.因此如何及时地探测化学毒剂成为世界各国国土安全的重点研究方向.该文聚焦于化学毒剂现有主流及具有潜力的各类探测技术,对各种检测技术的基本原理及其...     

Solvent-Free Synthesis of Arylsulfonyl Cyanides Using Potassium Hexacyanoferrate(II) as An Ecofriendly Cyanide Source

Abstract

A solvent-free synthetic method for arylsulfonyl cyanides directly from corresponding sulfonyl chlorides using potassium hexacyanoferrate(II) as an ecofriendly cyanide source is described. The protocol has the advantages of no uses of highly toxic cyanating agent and volatile organic solvents, high yield, and simple work-up procedures.     

Recent advances in miniaturization of portable liquid chromatography with emphasis on detection

Liquid chromatography is a prominent analytical technique in separation science and chemical analysis, applied across numerous fields of research and within industrial applications. Over the past few decades, there has been a growing interest in the miniaturization of this technique, which has been particularly enabled through new miniature and portable detection technologies for in-field, at-site, and point-of-need (collectively ‘out-of-lab’) analyses. Accordingly, significant advances have been made in recent years in the development of miniaturized liquid chromatography with photometric, electrochemical, and mass spectrometric detection, enabling the development of field-deployable and portable instruments for various applications. Herein, recent developments in the miniaturization of detection systems for inclusion within, and/or coupling with, portable liquid chromatographic systems, are reviewed in detail together with critical comments and expected future trends in this area.     

Microdetermination of Cyanide

Abstract

A volumetric procedure is described for the micro-determination of cyanide. Small amounts of cyanide can be estimated even in presence of chloride if it is present in the electrolytic bath. N-Bromosuccinimide (NBS) is used to quantitatively oxidized cyanide to cyanate. The end point is reached when the rose red color of the bordeaux red is changed to distinct yellow. From 1–6 mg. of cyanide were analyzed with an average relative standard deviation of about 0.66%.     

Indirect spectrophotometric determination of cyanide

A spectrophotometric method for cyanide based on its inhibition of the colour formation reaction between nickel(II) and 3-(4,5-dimethyl-2-thiazolylazo)-2,6-dihydroxybenzoic acid has been developed, and allows the determination of down to 0.1 g of cyanide. Most of the interferences can be avoided by displacement of the hydrogen cyanide using an arsine generator.     

Review of analytical methods for the determination of chlorine dioxide

The present study reviews more than twenty years (1985-present) of published research on the development and application of analytical procedures for the determination of chlorine dioxide, a widely used disinfectant and bleaching agent. The review covers a variety of techniques including batch and automated spectrophotometry and fluorimetry, electroanalysis and chromatography. The analytical figures of merit to the methods are presented, while critical discussion regarding their advantages and disadvantages is addressed.      

红外光谱技术在茶叶分析中的应用综述

在总结大量文献的基础上,对中、近红外光谱技术在茶叶分析中的应用进行了较为全面的综述;指出红外光谱技术因具有速度快、成本低及重现性好等优点,近年来在生物和食品等领域得到了越来越广泛的应用.     

Unlocking Mizoroki–Heck‐Type Reactions of Aryl Cyanides Using Transfer Hydrocyanation as a Turnover‐Enabling Step

A new transfer hydrofunctionalization strategy to turnover H‐M^II‐X complexes has enabled both intra‐ and intermolecular Mizoroki–Heck (MH)‐type reactions of aryl cyanides that are challenging to realize under traditional, basic conditions. Initially, a cascade carbonickelation/MH reaction of 2‐cyanostyrenes was achieved using a key alkyne transfer hydrocyanation step. Mechanistic experiments supported the proposed catalytic cycle, including the turnover‐enabling transfer hydrocyanation step. The reactivity was then extended to the intermolecular MH reaction of benzonitriles and styrenes.     

端粒酶活性检测研究进展

端粒酶活性检测方法经过近30年的不断改革与发展,取得了巨大突破。该文重点综述了近3年的端粒酶活性检测方法,其中包括化学反应发光法、电化学法、荧光分析法、比色法等,旨在更加全面地了解目前端粒酶活性检测的研究进展,为设计新的端粒酶活性检测方法和克服端粒酶活性检测方法在临床试验中的挑战提供思路。     

Determination of Fluoride,Cyanide, and Thiocyanate Using Horseradish Peroxidase Immobilized on Modified Silica Gel

Abstract

Silica gels modified with different functional groups (amino, epoxy, cycloepoxy, isocyanate, and thiocyanate) were used for the covalent immobilization of horseradish peroxidase (HRP). The catalytic activity and stability of the obtained enzyme preparations were studied using the reaction of o‐dianisidine oxidation with hydrogen peroxide as an indicator. The covalent immobilization of horseradish peroxidase using silica gel modified with thiocyanate groups provided not only the improvement of the enzyme stability, but also the development of the sensitive, rapid, and simple procedures for the determination of fluoride, cyanide, and thiocyanate. Enzymatic determination of inorganic anions is based on their inhibitory effect on the enzyme as the ligands capable to form stable complexes with Fe(III)‐HRP cofactor. The proposed procedures were applied for the determination of F^? in mineral and drinking waters; CN^? and SCN^?—in biological fluids (blood and saliva).