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本文报导了以玻碳电极为基体的1:12硅钼杂多阴离子薄膜化学修铈电极的制备及其电化学特性。并应用于导数伏安法测定。在4.0×10 ̄(-3)m0l/L(NH_4)_6MO_7O_(24)-6.8×10 ̄(-2)mol/LNa_3Cit-0.48mol/LNHO_3体系中,硅浓度在8.3×10 ̄(-7)~1.7×10 ̄(-3)mol/L范围内与峰电流呈良好线性关系,检测限为8.0×10 ̄(-7)mol/L。对可溶性硅(以SiO_2计)为245.05mg/L的黑液,稀释10倍后,取2.00mL平行测定9次,RSD为0.58%,加标回收率在97.3%~104.4%间。 相似文献
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5-(对-羟基苯基):-5-苯基乙内酰脲的反相高效液相手性分离测定法 总被引:2,自引:0,他引:2
以β-CD为手性流动相添加剂、苯巴比妥为内标,于FLC-C8反相柱上建立了鼠肝微粒体中5-(对-羟基苯基)-5-苯基乙内酰脲(p-HPPH)外消旋体的拆分方法。测得p-HPPH对映体的线性范围为0.5~110mg/L(r=0.9996);最低检出量为5ng(S/N=3);S-p-HPPH的回收率为93.6%±2.8%,R-p-HPPH的回收率为94.7%±1.8%;日内和日间精密度RSD值均小于2%。所建立的方法具有结果准确、操作方便等特点。 相似文献
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基于固定化酶的流动荧光法测定血清中的葡萄糖 总被引:5,自引:0,他引:5
本文将固定化酶柱,光纤以及停流技术结合起来,研究了以廉价而易得的硫胺素为荧光底物的葡萄糖的荧光分析,提出了一种快速、简便、精确地测定葡萄糖的新方法。其线性范围为1.0 ̄60.0mg/L,线性相关系数为0.999,检测限为0.15mg/L。以5.0mg/L的葡萄糖作精度试验,RSD%=2.1%(n=11)。该方法已成功地用于血清中葡萄糖的测定,结果与光度法相符。 相似文献
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火焰原子吸收光谱法间接测定非金属材料中氯 总被引:9,自引:0,他引:9
报道了火焰原子吸收光谱法(FAAS)间接测定非金属材料中氯的方法,采用AgCl沉淀,测定剩余Ag~+间接求出氯含量。方法的特征浓度为0.014mg/L(1%吸收),检出限为0.032mg/L(3),测定下限为0.11mg/L,相对标准偏差(RSD)为1.5%~10%,样品加标准回收率在91.4%-105%之间。 相似文献
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测定N—亚硝基化合物的分光光度法 总被引:2,自引:0,他引:2
利用N-亚硝基化合物的化学去亚硝基反应,建立了一种间接测定N-亚硝基化合物的分光光度法。实验结果表明,N-二苯基亚硝胺在0.2 ̄9.0mg/L浓度内呈线性关系。该法应用于香烟烟丝及侧流烟雾萃取液的分析,4次测定RSD及回收率分别为1.86% ̄6.32%,86.2% ̄96.6%;3.01% ̄5.03%,101.1% ̄109.1%。 相似文献
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手性毛细管色谱法测定人尿中美芬妥英对映体的含量及其在代谢分型中的应用 总被引:2,自引:0,他引:2
采用手性毛细管色谱柱和FID检测器建立了人尿中美芬妥英(MP)对映体的定量分析方法。尿样用二氯乙烷提取,用酸、碱洗涤得以纯化,测得各对映体的最低检测限为60μg/L。在115~690μg/L浓度范围内,标准曲线呈良好的线性关系,r>0.99,日内、日间精密度RSD<6.5%,S-MP的平均回收率为74.41%,R-MP的平均回收率为73.78%。并以MP为探针药物,对32名志愿者的尿样进行了MP氧化代谢分型研究。 相似文献
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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
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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
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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
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
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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
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
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
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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
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
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
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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
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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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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