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双波长分光光度法同时测定贵金属钯和锇 总被引:4,自引:0,他引:4
本文提出了在对羟基苯基荧光酮和溴化十六烷基三甲烷基甲胺存在下,双波长分光光度法同时测定微量和锇的新方法,在pH=7.6~8.0的磷酸盐介质中,钯和锇的对羟基苯基荧光酮-CTMAB配合物吸收光谱相互重叠,选择测定钯配合物的波长对为580.5nm与530.5nm,测定锇配合物的波长对为553.5nm与604.5nm,钯含量在0~7.0μg/10mL范围内,锇含量在0~9.0μg/mL范围内,与ΔA值呈 相似文献
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研究了氨酰心安的荧光光度法,其最大激发波长和荧光波长分别为222.3nm和297.4nm。该法灵敏度高,操作简便,氨酰心安浓度在0~3.00μg/mL范围内与相对荧光强度呈线性关系,相关系数为0.9997,检测限为0.0169μg/mL。该法用于测定片剂中氨酰心安含量,结果满意。 相似文献
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流动注射—胶束荧光法快速测定葡萄糖中的微量铝 总被引:1,自引:0,他引:1
本提出Al-Calcein-CTMAB-Tween-80体系,用流动注射-胶束荧光法快速测定葡萄糖中微量铝的方法。荧光最大激发波长和发射波长分别为478.0和509.0nm.Al^3+的浓度在0-6μg/mL范围内标准曲线呈线性关系,方法检出下限为8.42×10^-3μ/mL。方法已用于测定葡萄糖中微量铝,相对标准偏差为1%左右,回收率为95-101%,进样频率为140次/h,进样量为0.443 相似文献
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荧光光度法直接测定环境水中苯酚和十二烷基苯磺酸钠的含量 总被引:2,自引:1,他引:2
本文研究了用荧光分光光度法直接测定环境水中苯酚和十二烷基苯磺酸钠(SDBS)二种水中污染物。在pH〉11直接测定SDBS含量,波长为λex/λem=230/295nm,检出限4.4ng/mL,线性范围0 ̄2.2μg/ml。在pH=6,波长为λex/λem=230/295nm,测得二者合量,从合量中减去SDBS含量即得苯酚含量,检出限4.0ng/ml,线性范围0 ̄0.85μg/mL,回收率达99% ̄ 相似文献
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流动注射光化学荧光法测定药物制剂中的盐酸氯丙嗪 总被引:10,自引:3,他引:10
氯丙嗪的流动注射光化学反应在一编结反应器中进行,该反应器盘绕在一荧光灯上并接受由该灯发生出的最大幅波长为365nm的紫外线照射。用253.0nm的激发波长和374.5nm的荧光波长在线测定光化学反应产物的荧光强度。在最佳条件下,检测限为5.4μg/L,采样速度为90次/h,1mg/L的分析物11次测定的相对标准偏差为0.5%,动态线性范围为0.01-6.00mg/L。所建立的方法已成功地地用于片剂 相似文献
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钯(Ⅱ)—二溴羟基苯基荧光酮—溴化十六烷基三甲铵体系分光光度法的… 总被引:9,自引:0,他引:9
在PH6.1-6.7的磷酸盐介质中,钯(Ⅱ)与二溴羟基苯荧光酮溴化十六烷基三甲铵于室温下反应,生成水溶性和稳定性皆佳的紫色三元配合物,最大吸收波长为600nm,对比度为70nm,表观摩尔吸光系数为9.48 ×10^4L.mol^-1cm^-1,桑德尔灵敏度为1.12×10^-3μg.cm^-2,钯含量在0.7.0μg/10mL范围内服从比尔定律。据此了一个灵敏、简便分光光度法测定钯的瓣方法,用于合 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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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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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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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
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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
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The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 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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Microwave-assisted copper-catalyzed ring expansions of three-membered heterocycles with α-diazo-β-dicarbonyl compounds were investigated. Thiiranes generated 3-acyl-5,6-dihydro-1,4-oxathiines in the presence of copper sulfate and trans-3-acyl-5,6-dihydro-1,4-oxathiines as stereospecific products for 1,2-disubstituted cis-thiiranes through an intramolecular SN2 process. Oxiranes gave rise to 2-acyl-5,6-dihydro-1,4-dioxines under the catalysis of copper hexafluoroacetylacetonate and cis-3-acyl-5,6-dihydro-1,4-dioxines as stereospecific products for 1,2-disubstituted cis-oxiranes via an intimate ion-pair mechanism. The current method provides a direct and simple strategy in efficient preparation of 3-acyl-5,6-dihydro-1,4-oxathiines and 2-acyl-5,6-dihydro-1,4-dioxines, important agents in medicinal and agricultural chemistry, from readily available thiiranes and oxiranes, respectively. 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