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941.
利用电荷迁移反应测定头孢羟氨苄 总被引:4,自引:0,他引:4
提出一种基于电荷迁移反应简便可靠地测定头孢羟氨苄的分光光度法。在甲醇-乙醇介质中,头孢羟氨苄与氯冉酸于50℃反应15min能够形成稳定的1:1络合物,其λmax=528nm,线性范围为20 ̄400mg/L。用拟定的方法测定原粉和胶囊,结果与药典法一致。对浓度100mg/L的药物10次测定相对标准偏差为1.4%,样品的标准加入回收率为99.0% ̄100.8%。 相似文献
942.
Summary The use of non-segmented flow, post-column reaction detection is evaluated for use with miniaturized HPLC. Non-segmented open-tubular reactors with internal diameters 0.1 mm to 0.25 mm and packed-bed reactors with internal diameters of 1 mm, filled with 5 and 10 m particles are evaluated theoretically and experimentally with respect to band broadening and pressure drop characteristics. An integrated system consisting of miniaturized HPLC (1 mm i. d.) columns and compatible hardware is described. An example of the separation of catecholamines is given. 相似文献
943.
Šárka Králíková 《Tetrahedron》2006,62(20):4917-4932
We found that various dialkyl phosphites, dialkyl trimethylsilyl phosphites, and tris-trimethylsilyl phosphite reacted smoothly with nucleoside 5′-aldehydes to afford epimeric nucleoside 5′-C-phosphonates in high yields. A number of these compounds in both the 2′-deoxyribo and ribo series were prepared. In the case of 2′-deoxythymidine-5′-aldehyde, a thorough study was made on the influence of the 3′-hydroxyl protecting group, type of phosphite, base, and solvent, on the yield and epimeric ratio of the resulting 5′-hydroxyphosphonates. Partial stereoselectivity in favour of either R or S epimers was observed. An attempt to transform the α-hydroxyl of the phosphonate moiety into a halo or azido moiety was not successful. Only intramolecular substitution reaction of the mesyloxy group for an alkoxy residue of the 2-hydroxyethyl ester took place in a low yield. 相似文献
944.
Eduardo A. Véliz 《Tetrahedron letters》2006,47(18):3153-3156
Herein, we report the use of triisopropyl phosphite (TIP) as an effective substitute for triphenylphosphine in the Mitsunobu reaction of nucleoside analogs. In addition, the use of triphenyl phosphite as an alternative reagent for the expensive hexamethylphosphorous triamide (HMPT) in the Véliz-Beal bromination protocol is reported. 相似文献
945.
Ai Suzuki Parasuraman Selvam Tomonori Kusagaya Seiichi Takami Momoji Kubo Akira Imamura Akira Miyamoto 《International journal of quantum chemistry》2005,102(3):318-327
The decomposition reaction dynamics of 2,3,4,4′,5‐penta‐chlorinated biphenyl (2,3,4,4′,5‐PeCB), 3,3′,4,4′,5‐penta‐chlorinated biphenyl (3,3′,4,4′,5‐PeCB), and 2,3,7,8‐tetra‐chlorinated dibenzo‐p‐dioxin (2,3,7,8‐TCDD) was clarified for the first time at atomic and electronic levels, using our novel tight‐binding quantum chemical molecular dynamics method with first‐principles parameterization. The calculation speed of our new method is over 5000 times faster than that of the conventional first‐principles molecular dynamics method. We confirmed that the structure, energy, and electronic states of the above molecules calculated by our new method are quantitatively consistent with those by first‐principles calculations. After the confirmation of our methodology, we investigated the decomposition reaction dynamics of the above molecules and the calculated dynamic behaviors indicate that the oxidation of the 2,3,4,4′,5‐PeCB, 3,3′,4,4′,5‐PeCB, and 2,3,7,8‐TCDD proceeds through an epoxide intermediate, which is in good agreement with the previous experimental reports and consistent with our static density functional theory calculations. These results proved that our new tight‐binding quantum chemical molecular dynamics method with first‐principles parameterization is an effective tool to clarify the chemical reaction dynamics at reaction temperatures. © 2004 Wiley Periodicals, Inc. Int J Quantum Chem, 2005 相似文献
946.
947.
偶合反应化学发光法测定痕量银的研究 总被引:6,自引:0,他引:6
本将Ag(Ⅰ)催化S2O^2-8氧化Mn(Ⅱ)生成MnO^-4的催化反应与LuminolMnO^-4-OH^-的化学发光反应相偶合,建立起一种新的灵敏测定痕量银的化学发光分析法,在所研究的优化条件下,该法测定银的选择性较好,检测限达到3.2×10^-12g/mLAg线性浓度范围为1.0×10^-11-1.0×10^-5g/mLAg,用于水样分析,结果较为满意。 相似文献
948.
以电化学循环伏安、现场ESR电化学以及现场薄层电化学方法研究了电生Co(I)TPP与溴代五己烷的反机制。在DMF中,Co(Ⅱ)/Co(Ⅰ)的氧化还原有明显的催化溴代环己烷还原的特片,反现场有自由基生成,反应产物之一是Co-C键化合物,可以在1.30V(SCE)-电子还原,当存在CH2-CHCN时,。生成另一种Co-C键化合物,该化合物在-1.10V(SCE)处一电子还原,证明溴代环己烷与Co(I) 相似文献
949.
采用均相反应的方法合成了6个含羟基芳基或氨基芳基的磷酰胺酯衍生物:[(ClCH_2CH_2)_2NP(O)(OPh)(XArY)](X:O,NH;Y:m或p-OH或NH_2).用元素分析、红外光谱、氢核磁共振谱及质谱证实了它们的组成及结构. 相似文献
950.
Bjrn E. Berg Ellen M. Hansen Synnve Gjrven Tyge Greibrokk 《Journal of separation science》1993,16(6):358-363
Supercritical carbon dioxide can be utilized both as an introduction solvent in capillary SFC and as a reaction medium; both possibilities are illustrated in this study. An off-line SFE unit was modified for on-line SFE-SFC. To facilitate rapid depressurization of the extraction cell and to prevent memory effects, a 6-port valve was installed at the outlet line of the extraction unit. An increased background signal was obtained when PEEK polymer was used in the construction of the extraction vessel; when stainless steel was used, the blanks improved. The synthesis of methyl esters and butyl esters of fatty acids from triglycerides in edible fat was examined using an immobilized lipase as a catalyst in on-line SFE-SFC. As a result of 30 minutes reaction – extraction time, high yields of fatty acid esters were obtained at a pressure of 150 bar and a temperature of 50°C. 相似文献