聚谷氨酸修饰电极测定盐酸异丙肾上腺素

盐酸异丙肾上腺素( Isoprenaline Hydrochloride)是β肾上腺素受体激动药,有舒张支气管、改善心肌传导和扩张周围血管作用.目前,测定异丙肾上腺素的方法有高效液相色谱法[1,2]、毛细管区带电泳法[3]、化学发光法[4]和激光散斑法[5]等.     

铁氰化钾—三氯化铁显色体系分光光度法测定特布他林

特布他林(间羟舒喘灵,Terbutaline,TB)系一种选择性β2受体激动剂,有松弛支气管平滑肌,抑制内源性痉挛物质的释放及内源性介质引起的水肿等功能.临床上已广泛用于治疗支气管哮喘、慢性支气管炎、肺气肿和其它伴有支气管痉挛的肺部疾病.已报道测定特布他林的方法有色谱法[1,2],磷光分光光度法[3],毛细管电泳法[4]和流体注射化学发光法[5]等.     

共振瑞利散射法测定头孢米诺

<正>头孢米诺钠为临床上应用十分广泛的β-内酰胺类的头孢菌素,具有强抗菌、耐青霉素酶、临床疗效高等特点。头孢米诺钠主要用于呼吸道、泌尿道、胆道、腹腔和子宫等部位感染的治疗,也用于败血症的治疗。目前,头孢米诺的检测方法主要有高效液相色谱法[1]、分光光度法[2]、毛细管电泳法[3]、化学发光法[4]和荧光光度法[5]等。但未见用共振瑞利散射法研究的报道。本工作发现,在氢氧化钠溶液中,灿烂绿与头孢米诺的结合物能使共振瑞利散射显著增     

化学发光新体系NaIO4-H2O2-痕量环己烷-多羟基酚的研究及其应用

近年来,一些无机氧化剂在氧化有机物时伴随的化学发光现象引起了分析工作者的广泛兴趣[1,2].NaIO4氧化H2O2会产生弱化学发光,不同的多羟基酚类物质能不同程度地增强这一化学发光行为,据此建立了测定多羟基酚的化学发光法.目前,利用该法测定的酚主要有苯酚[3]、酚的衍生物[4]和连苯三酚[5,6].本文建立的测定连苯三酚的方法检测限较王伦等[3]的利用苯酚对Luminol-H2O2发光体系猝灭作用测定工业废水及Ermiridis[5]以IO4-在碱性介质中直接氧化连苯三酚的检测限低两个数量级,且扩大了测定酚的种类.研究发现,一些非极性有机溶剂对这一化学发光亦有增强和增稳作用,而痕量非极性溶剂由于在水中的溶解性较差,对化学发光的作用尚未受到注意.     

流动注射化学发光法测定诺氟沙星

诺氟沙星为第三代氟喹诺酮类抗菌药物,抗菌谱广、抗菌作用强,尤其对需氧革兰阴性杆菌的抗菌活性高.文献报道的测定诺氟沙星的方法主要有高效液相色谱法[1,2]、毛细管电泳法[3]、分光光度法[4-6]、荧光法[7]和化学发光法[8-10].本研究观察到在碱性介质中诺氟沙星对鲁米诺-高碘酸钾化学发光反应有很强的抑制作用,与文献[8-10]报道的化学发光法相比,发现此体系十分稳定,操作简单,试验费用低;方法的检出限为 2.0×10-6g·L-1,线性范围为8.4×10-6～1.2×10-2g·L-1,对 6.O×10-4g·L-1诺氟沙星平行测定 11 次,相对标准偏差为2.6%,已用于滴眼液及胶囊中诺氟沙星的分析.     

丹皮酚的选择性溴化反应

丹皮酚 (Paeonol)化学名为 4 甲氧基 2 羟基苯乙酮 ,是中药材牡丹皮中所含的主要活性成分 ,具有抑菌抗炎、解热镇痛 ,降压利尿 ,抗凝血 ,抑制肿瘤 ,抗癌 ,增强免疫功能等作用[1～ 3] ,在医药、香料、化工领域具有广泛的用途。对丹皮酚进行选择性溴代是进一步开发丹皮酚药用价值的有效途径之一。α 卤代酮是有机合成的中间体 ,一般是在酸催化下用卤素直接卤化制得[4] 。但丹皮酚的苯环较活泼 ,若用溴直接作溴化剂 ,苯环和侧链羰基α 氢可同时发生反应。陈俊杰等[5] 用溴化铜作为羟基苯乙酮的α 溴化剂 ,有较高的选择性 ,溴代只发生在侧链羰…     

用偶合反应化学发光法研究丹皮酚在兔体内的药物代谢动力学

为了研究丹皮酚的药物代谢动力学，采用高灵敏的偶合反应化学发光法，对兔血中的血药浓度进行监测，在ｐＨ为９．２的介质中，以Ｈ２Ｏ２氧化丹皮酚的反应与Ｌｕｍｉｎｏｌ－Ｈ２Ｏ２－ＣＯ＾２＋化学发光反应相偶合，测得牡丹皮和徐长卿中丹皮酚在兔体内的吸收速率分别为２．０７和０．４９９ｈ＾－１，消除半衰期分别为１１．７６和３．０４ｈ，相对而言牡丹皮所含丹皮酚具有吸收快、消除慢、生物利用度大的优点。     

阻抑光度法测定痕量铁(Ⅲ)

铁是人体不可缺少的微量元素,是血红蛋白的核心部分,正常成人体内铁的总量为2~4g。目前,测定痕量铁的方法有伏安法[1]、化学发光法[2]、色谱法[3]、极谱法[4]、原子吸收光谱法[5]、激光光热折射光谱法[6]、微晶石蜡柱固相萃取法[7]、二阶导数光谱-峰面积积分光度法[8]和分光光度法[9]等。阻抑动力学分光光度法是利用具有氧化性的物质如高碘酸钾、过氧化氢、三价铁离子、溴酸钾等,对在不同波     

阻抑动力学荧光法测定氨苄青霉素

氨苄青霉素属于β-内酰胺类抗生素,是国内临床上广泛使用的广谱青霉素,其含量测定多采用紫外可见分光光度法[1-2]、高效液相色谱法[3]、电位滴定法[4]、化学发光法[5]、极谱法[6]等。但上述方法有的试剂繁多操作复杂,有的费时,灵敏度不高,线性范围较窄。美国药典(第23版)采用剩     

溴酸钾-RB体系催化动力学光度法测定痕量钒

钒是人体不可缺少的微量元素之一,人体中钒含量过高或过低都会影响人体的新陈代谢,从而引起不适应症状甚至病变。钒主要存在于岩石矿物中,钢铁、淤泥、废水、食品甚至于人的头发中也含有微量钒。目前,钒的测定主要有光度法[1]、荧光法[2]、化学发光法[3]、极谱法[4]、色谱法[5]     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

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%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

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.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

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.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

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.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

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.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

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.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

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.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

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.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

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.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

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.