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931.
Jemal M Huang M Mao Y Whigan D Schuster A 《Rapid communications in mass spectrometry : RCM》2000,14(12):1023-1028
A sensitive, specific, accurate and reproducible liquid chromatography/electrospray tandem mass spectrometry method was developed and validated for the quantitation of fosinoprilat in 0.2 mL of human serum. The method employed acidification (with pH 4.0 sodium acetate buffer) of the serum samples to minimize the hydrolysis of the prodrug fosinopril to fosinoprilat prior to purification by automated 96-well solid-phase extraction. The required chromatographic separation of fosinoprilat and fosinopril was achieved isocratically on a Luna C8 analytical column (2 x 50 mm, 3 microm). The total run time was 2 min. The mobile phase contained methanol and water with 10 mM ammonium acetate. Detection was by positive ion electrospray tandem mass spectrometry. The standard curve, which ranged from 2.00 to 500 ng/mL, was fitted to a 1/x(2) weighted linear regression model. Fosinoprilat quality control (QC) samples used to determine the accuracy and precision of the method were prepared in human serum at concentrations of 5.00, 200, 400 and 1000 ng/mL. The assay accuracy was within 8% (dev). The intra- and inter-assay precisions were within 6 and 3% (RSD), respectively. Fosinopril QC samples used to gauge the rate of hydrolysis of fosinopril to fosinoprilat during the assay procedure were prepared in human serum at 500 ng/mL. The hydrolysis of fosinopril to fosinoprilat was =1%. This degree of conversion would cause little error in the analysis of post-dose serum samples since such samples are known to contain low levels of the prodrug compared with the drug. 相似文献
932.
Wang D Schwinden MD Radesca L Patel B Kronenthal D Huang MH Nugent WA 《The Journal of organic chemistry》2004,69(5):1629-1633
The reaction of a variety of methyl esters with dimethylsulfoxonium methylide at 0-25 degrees C affords the chain-extended beta-keto dimethylsulfoxonium ylides. Subsequent treatment with hydrogen chloride in THF proceeds with loss of DMSO to afford the corresponding alpha-chloroketones. This sequence has been utilized to convert the methyl esters of CBZ-protected alanine and valine to the anti N-protected alpha-amino epoxides, which are important pharmaceutical intermediates. When the same protocol is applied to BOC-protected phenylalanine methyl ester, epimerization occurs so that the use of a more reactive aryl ester is required. This chemistry provides a practical route to alpha-chloroketones that avoids the use of toxic and explosive diazomethane. 相似文献
933.
Tseng CM Dyakov YA Huang CL Mebel AM Lin SH Lee YT Ni CK 《Journal of the American Chemical Society》2004,126(28):8760-8768
Photoisomerization and photodissociation of aniline and 4-methylpyridine at 193 nm were studied separately using multimass ion imaging techniques. Photofragment translational energy distributions and dissociation rates were measured. Our results demonstrate that more than 23% of the ground electronic state aniline and 10% of 4-methylpyridine produced from the excitation by 193 nm photons after internal conversion isomerize to seven-membered ring isomers, followed by the H atom migration in the seven-membered ring, and then rearomatize to both methylpyridine and aniline prior to dissociation. The significance of this isomerization is that the carbon, nitrogen, and hydrogen atoms belonging to the alkyl or amino groups are involved in the exchange with those atoms in the aromatic ring during the isomerization. 相似文献
934.
935.
邻苯二胺合钴氧合反应的研究Ⅰ 水溶液中配合物及其氧合配合物稳定常数的测定 总被引:2,自引:0,他引:2
自1938年Tsumaki报道犤1犦氧载体以来,这方面的研究已有很大进展犤2犦,只是理论研究居多。氧载体的氧合常数是氧载体研究中的一个重要参数,它的测定是氧载体研究中的一项重要内容,用pH电位法测定氧载体的氧合常数已有研究报道犤2~4犦,作者在研究中发现,邻苯二胺合钴(o-Phdn-Co)配合物在固相和水溶液中与O2反应时表现出很大差异,其反应产物的组成比分别为液相配合物Co∶O2=2∶1,而固相配合物Co∶O2=1∶2,为究其成因和进行理论探讨,有必要先测定其氧合常数。由于o-Phdn-Co配合物的配位常数也未见文献… 相似文献
936.
Dependence of Performance of Organic Light-emitting Devices on Sheet Resistance of Indium-tin-oxide Anodes 总被引:2,自引:0,他引:2
ZHOU Liang ZHANG Hong-jie YU Jiang-bo MENG Qing-guo PENG Chun-yun LIU Feng-yi DENG Rui-ping PENG Ze-ping LI Zhe-feng 《高等学校化学研究》2006,22(4):427-431
IntroductionIndium-tin-oxide(ITO) has been widely used asthe anode material in organic light-emitting devices(OLEDs) because of its high transmittance in the visi-ble region and low electrical resistivity. In the pastyears, many investigations focused on … 相似文献
937.
蔗糖酯分子在碱性条件下,加热水解为蔗糖和硬酯酸,在pH>10的NH_3·N_2O-(NH_3)_3C_6H_5O_7体系中,于示波极谱仪上,峰电位─0.91V处出现一灵敏度高和稳定性好的极谱图,其浓度从0.02~0.28mg/mL与峰电流呈线性关系,最低检出限为0.004mg/mL,相对标准偏差为1.3%。 相似文献
938.
Three types of dual-frequency oscillations in KBrO3-galactose-acetone-MnSO4-H2SO4 have been observed in a batch reactor depending on the initial concentration of H2SO4 or Br-. Similar phenomena were also observed when galactose was replaced by other aldosugars such as glucose, arabi-nose, lactose and maltose. However no dual-frequency oscillation has been found when ketosugar like fructose was used instead of galactose as the substrate. The roles of acidity, bromide ion and acetone in dual-frequency oscillations have been analyzed. The mechanism of dual-frequency oscillations has been discussed. 相似文献
939.
Study on flame-retardant mechanism of polycarbonate containing sulfonate-silsesquioxane-fluoro retardants by TGA and FTIR 总被引:1,自引:0,他引:1
Shumei Liu Yongsheng Zhou Zhijie Jiang Xianbo Huang 《Polymer Degradation and Stability》2006,91(8):1808-1814
The flame retardancy of bisphenol A polycarbonate (PC) containing potassium diphenylsulfone sulfonate (KSS), poly(aminopropyl/phenylsilsesquioxane) (PAPSQ) and poly(vinylidenefluoride) (PVDF) was measured by limited oxygen index (LOI) and examined according to UL94. A high LOI and UL94 V-0 rating for 1.6 mm thickness samples were obtained by a combined use of equivalent KSS, PAPSQ and PVDF at 0.1-0.3 wt% loading, respectively. The improvement in flame retardancy of PC compositions arose from the synergistic interaction of three additives. Thermogravimetric analysis (TGA) indicated that the combination decreased the activation energy (E) of PC degradation and elevated the thermal degradation rate of PC to ensure the formation of an insulating carbon layer. FTIR analysis showed that the LOI char of PC containing the three additives took on a highly cross-linking aromatic ester and ether structure. 相似文献
940.