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1.
高锰酸钾-甲醛-无机还原剂化学发光体系   总被引:10,自引:0,他引:10  
何云华  吕九如 《分析化学》2002,30(5):598-600
在甲醛存在下,高锰酸钾与无机还原剂Fe(Ⅱ),S^2-,I^-,Cu(Ⅰ)等能够发生化学发光反应,产生很强的化学发光,据此利用流动注射技术研究了这些化学发光反应。考察了这些反应应用于铁,硫、碘、铜等元素化学发光测定的可行性,并探讨了反应机理。  相似文献   

2.
液相色谱化学发光检测法的新进展   总被引:4,自引:0,他引:4  
武竟存  章竹君 《分析化学》1994,22(4):396-405
本文评述了近年来液相色谱化学发光检测法的新进展,内容涉及各类化学发光发反应,生物发光反应和电致化学发光反应同色谱体系的偶合方式,仪器设计,多种无机,有机,生物大分子和生物活性物质的分析方法及其在环境,生物医学科学和生命科学中的应用和发展方向。引用文献168篇。  相似文献   

3.
固体表面化学发光分析 Ⅱ.单矿物和钢中镍的微量测定   总被引:3,自引:0,他引:3  
本文建立了Ni(OH)^2-nn催化剂H2O2氧化Luminol的化学发光反应,与Ni^2+的催化化学发光反应比较,它更适合于固体表面化学发光分析。利用Ni^2+在用丙酮-盐酸-水作展开剂的纸上色谱行为中Rt值为零的特点,与大多数干扰离子进行分离,实现了单矿物和钢铁中镍的快速纸上色谱-固体表面化学发光分析。  相似文献   

4.
流动注射化学发光检测法的进展   总被引:11,自引:0,他引:11  
周延秀  朱果逸 《分析化学》1997,25(2):222-230
评述近年来流动注射化学发光检测法及生物发光检测法的最新进展。内容涉及各类化学发光反应、生物发光和电致化学发光反应同流主射体系的耦合方式,仪器设计,多种无机、有机、生物大分子、生物活性的药物的分析方法及其在环境、生物医学客生命科学、化学及药物化学中的应用和发展方向。  相似文献   

5.
针对大多数化学发光反应选择性差的缺陷,建立了一种基于外参比校正的化学发光新技术,从而实现了化学发光法对待测物的选择性识别.区别于以前常用的单个化学发光反应,偶合两个相似的化学发光反应,进行样品中叠氮化钠的选择性识别.两个相似的化学发光反应所用的氧化剂和催化剂相同,但化学发光增强剂不同.实验结果证明:偶合下列两个反应:H2O2-CH3CN-四环素(工作反应)和H2O2-CH3CN-N-乙酰-5-甲氧基色胺(参比反应),我们能够从多种相似的自由基淬灭剂中选择性地识别出叠氮化钠.这是因为叠氮化钠仅淬灭"工作反应"的化学发光信号,而其它的自由基淬灭剂则同时淬灭"工作反应"和"参比反应"的化学发光信号.作为应用示例,已利用该技术选择性识别并定量分析了商品化胰岛素试剂盒中各种试剂、人血清白蛋白和羊抗人IgG抗体样品中的叠氮化钠.  相似文献   

6.
杜建修  刘文侠  吕九如 《化学学报》2004,62(14):1323-1326,J004
将被认为没有化学发光活性的第二主族(碱土金属)离子Mg^2 ,Ca^2 ,Sr^2 ,Ba^2 溶液注入到已充分反应的高锰酸钾与鲁米诺混合液中时,又发生了新的化学发光反应,并检测到强的化学发光信号.在对有关反应的动力学性质、化学发光光谱、紫外可见光谱及其它一系列实验研究的基础上,提出了可能的化学发光反应机理.同时,优化了反应条件,评价了这一反应用于Mg^2 ,Ca^2 ,Sr^2 ,Ba^2 分析的可行性.  相似文献   

7.
儿茶酚胺类药物的流动注射化学发光分析   总被引:5,自引:2,他引:5  
李建国  吕九如 《分析化学》1997,25(3):314-317
观察到雷盐(NH4「Cr(NH3)2」(SCN)4」。H2O)对鲁米诺-H2O2化学发光反应的催化作用。根据儿茶酚胺类物质可与雷氏盐发生沉积反应而导致鲁米诺-H2O-2雷氏盐体系化学发光强度降低的性质,建立了儿茶酚胺类物质多巴胺,肾上腺素和异丙肾上腺素的流动注射化学发光分析法。  相似文献   

8.
吐温—80固相化学发光测定痕量金的研究及其应用   总被引:6,自引:1,他引:6  
韩鹤友  何治柯 《分析化学》1998,26(8):974-976
研究了吐味-80与An(Ⅲ)的因相化学发光反应。比较了其在不同固相上的反应情况,用自制的固相化学发光仪,以巯基泡沫塑料(SPF)吸附溶液中Au(Ⅲ),采用圆表制片直接在SPF表面进行化学发光测定,建立了痕量金的固相化学发光分析法。方法的线性范围为0.01-10μgAu(Ⅲ),对1.0μg(Ⅲ)测定11次的相对标准偏差为4.2%,用于实际矿样痕量金的测定,结果满意。  相似文献   

9.
化学发光的基础理论和分析应用已经有多年的研究历史,但化学发光的研究多局限于分子和离子水平。纳米粒子由于其量子尺寸效应、表面能高以及比表面积大,因而常作为氧化还原反应的催化剂来放大反应信号。近年来,纳米粒子直接或者间接参与的化学发光拓展了化学发光的理论和应用研究范畴,己发现纳米粒子能够作为催化剂、还原剂、微尺度反应平台和能量接受体等参与化学发光反应。本文详细介绍了纳米粒子参与的鲁米诺化学发光体系,并重点评述了部分纳米粒子参与的鲁米诺化学发光与高效液相色谱、毛细管电泳等分离技术联用实例。纳米粒子作为一种新型化学发光响应单元,可提高鲁米诺化学发光反应的效率,对开发新的鲁米诺化学发光反应体系具有重要意义,已有关于金、铂、银、合金、半导体、磁性等纳米粒子参与的鲁米诺化学发光报道。除应用于环境、药品及食品等分析领域外,其在免疫分析方面也表现出巨大的应用潜力。最后,提出了纳米粒子参与鲁米诺化学发光体系研究目前存在的问题,并对其未来的发展方向进行了展望。  相似文献   

10.
流动注射化学发光法测定异烟肼   总被引:11,自引:0,他引:11  
赵芳  吴远远 《分析化学》1997,25(8):927-929
报道一种微量测定抗结核药物剧烟的新方法,方法是基于异烟肼对鲁米诺-锰(Ⅱ)-高碘酸钾化学发光反应的增敏作用,建立了微量异烟肼流的流动注射化学发光分析法。  相似文献   

11.
用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.  相似文献   

12.
Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.  相似文献   

13.
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.  相似文献   

14.
The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.  相似文献   

15.
KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.  相似文献   

16.
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.  相似文献   

17.
The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.  相似文献   

18.
A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.  相似文献   

19.
A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.  相似文献   

20.
Zhanhui Yang  Shiyi Yang  Jiaxi Xu 《Tetrahedron》2017,73(23):3240-3248
Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.  相似文献   

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