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51.
Yang M Wang GJ Wang SJ Li XT Xu YP Wang SP Xiang JD Pan SR Cao GX Ye WC 《Rapid communications in mass spectrometry : RCM》2005,19(12):1619-1623
23-Hydroxybetulinic acid is a newly isolated derivative of betulinic acid. The agent exhibits potential anti-tumor activity and functions in this regard via apoptosis. In support of pharmacokinetic and toxicological evaluations, a new assay based on liquid chromatography/mass spectrometry (LC/MS) was developed for the quantitative analysis of 23-hydroxybetulinic acid. Sample preparation consisted of extraction of the plasma by the addition of methylene chloride followed by centrifugation. Aliquots of the supernatant were analyzed using an isocratic reversed-phase high-performance liquid chromatography (HPLC) system coupled to a negative ion electrospray mass spectrometer. Molecules of 23-hydroxybetulinic acid and the internal standard limonin were detected using selected ion monitoring at m/z 471 and 469, respectively. The limit of detection of 23-hydroxybetulinic acid was 0.05 pg (0.11 fmol) injected on-column (10 pg/mL, 5 microL injection volume), and the limit of quantitation was 10 pg (21.19 fmol, 2 ng/mL, 5 muL injection volume). 23-Hydroxybetulinic acid was stable in plasma samples at -20 degrees C for at least 3 weeks. The intra-day and inter-day coefficients of variation of the assay were 3.0 and 4.8%, respectively. The utility of the assay was demonstrated by measuring 23-hydroxybetulinicacid in mouse plasma following intragastric administration (IG) in vivo. Pharmacokinetic parameters were calculated using the 3P97 pharmacokinetic software package. A two-compartment, first-order model was selected for pharmacokinetic modeling. The result showed that after IG of 200 mg/kg 23-hydroxybetulinic acid, the plasma concentrations reached peaks at 2 h with C(max) of 3.1 microg/mL. The 200 mg/kg 23-hydroxybetulinic acid suspension IG doses were found to have long elimination half-lives of 25.6 h and low bioavailability of 2.3%. No interference was noted due to endogenous substances. These analytical methods should be of value in future studies related to the development and characterization of 23-hydroxybetulinic acid. 相似文献
52.
Three photocatalytic oxidation (PCO) systems: C7H16-O2, SO2-O2 and C7H16-SO2-O2 were carried out with the aid of UV-illuminated TiO2 nanoparticles at room temperature in a batch reactor. In C7H16-O2-TiO2 system, no catalyst deactivation was observed, while for SO2-O2-TiO2 and C7H16-SO2-O2-TiO2 systems, the photocatalytic activity of used TiO2 powder showed decreasing and eventually no activity after used consecutively. The reaction products such as sulfur trioxide or sulfuric acid adsorbed onto the surface of TiO2 catalyst were poisoning species. Photocatalytic activity of the deactivated TiO2 powder could be regenerated by sonicating treatment with water and methanol for the two systems, respectively. 相似文献
53.
Rapid determination of volatile constituents of Michelia alba flowers by gas chromatography-mass spectrometry with solid-phase microextraction 总被引:12,自引:0,他引:12
The volatile constituents of Michelia alba flowers, including fresh flowers, frozen flowers and withered flowers, were investigated by GC-MS. The volatiles in a simulated natural environment were sampled by solid-phase microextraction (SPME), with a 100 microm polydimethylsiloxane fiber at 25+/-5 degrees C for 4 h. The fibers were desorbed in a GC injection liner at 250 degrees C for 3 min. With headspace SPME-GC-MS analysis, 61 peaks were separated. The main compounds in headspace of fresh Michelia alba flowers included alpha-myrcene, (S)-limonene, (R)-fenchone, linalool, camphor, caryophyllene, germacrene D, etc., a greater number of compounds than for frozen flowers and withered flowers. At the same time, the biomarkers of fresh flowers were compared with the frozen flowers and withered flowers. In this study, headspace SPME-GC-MS afforded a simple and more sensitive sampling method for fresh Michelia alba flowers and other fresh flowers. 相似文献
54.
Based on the theory of stochastic resonance, a new method carried on the quantitive analysis to weak chromatographic signal of glyburide in plasma, which was embedded in the noise background and the signal-to-noise ratio (SNR) of HPLC-UV is enhanced remarkably. This method enhances the quantification limit to 1 ng ml−1, which is the same as HPLC-MS, and makes it possible to detect the weak signal accurately by HPLC-UV, which was not suitable before. The results showed good recovery and linear range from 1 to 50 ng ml−1 of glyburide in plasma and the method can be used for quantitative analysis of glyburide. 相似文献
55.
A
modulated dsc study on the in situ polymerization of cyclic butylene terephthalate
oligomers 总被引:1,自引:0,他引:1
Z. A. Mohd Ishak P. P. Shang J. Karger-Kocsis 《Journal of Thermal Analysis and Calorimetry》2006,84(3):637-641
The polymerization of a cyclic butylene terephthalate
(CBT) oligomer was studied as a function of temperature (T=200
and 260°C, respectively) by modulated DSC (MDSC). The first heating was
followed by cooling after various holding times (5, 15 and 30 min) prior to
the second heating which ended always at T=260°C.
This allowed us to study the crystallization and melting behavior of the resulting
polybutylene terephthalate (PBT), as well. In contrary to the usual belief,
the CBT polymerization is exothermic and the related process is superimposed
to that of the CBT melting. The melting behavior of the PBT was affected by
the polymerization mode (performed below or above the melting temperature
of the PBT product) of the CBT. Annealing above the melting temperature of
PBT yielded a product featuring double melting. This was attributed to the
presence of crystallites with different degrees of perfection. The crystals
perfection which occurred via recrystallization/remelting was manifested by
a pronounced exothermic peak in the non-reversing trace. 相似文献
56.
57.
Cao C Dahal S Shang M Beatty AM Hibbs W Schulz CE Scheidt WR 《Inorganic chemistry》2003,42(17):5202-5210
The effect of a sixth ligand in a series of low-spin thiocarbonyl-ligated iron(II)octaethylporphyrinates has been investigated. Six-coordinate complexes have been synthesized and characterized by M?ssbauer and infrared spectroscopy and single-crystal X-ray structure determinations. The results are compared with the five-coordinate parent complex. The crystal structures of [Fe(OEP)(CS)(1-MeIm)] and [Fe(OEP)(CS)(Py)] are reported and discussed. The 1-methylimidazole and pyridine derivatives exhibit Fe-C(CS) bond distances of 1.703(4) and 1.706(2) A that are significantly longer than the 1.662(3) A reported for five-coordinate [Fe(OEP)(CS)] (Scheidt, W. R.; Geiger, D. K. Inorg. Chem. 1982, 21, 1208). The trans Fe-N(ligand) distances of 2.112(3) and 2.1550(15) A observed for the 1-methylimidazole and pyridine complex are approximately 0.13 A longer than those observed for analogous bis-ligated complexes and are consistent with a significant structural trans effect for the CS ligand. M?ssbauer investigations carried out for five- and six-coordinate thiocarbonyl derivatives with several different sixth axial ligands reveal interesting features. All derivatives exhibit very small isomer shift values, consistent with a very strong interaction between iron and CS. The five-coordinate derivative has delta(Fe) = 0.08 mm/s, and the six-coordinate complexes exhibit delta(Fe) = 0.14 to 0.19 mm/s at 4.2 K. The five-coordinate complex shows a large quadrupole splitting (DeltaE(q) = 1.93 mm/s at 4.2 K) which is reduced on coordination of the sixth ligand (DeltaE(q) = 0.42-0.80 mm/s at 4.2 K). Addition of a sixth ligand also leads to a small decrease in the value of nu(CS). Correlations in structural, IR, and M?ssbauer results suggest that the sixth ligand effect is primarily induced by changes in sigma-bonding. The structure of [Fe(OEP)(CS)(CH(3)OH)] is briefly reported. Crystal data: [Fe(OEP)(CS)(1-MeIm)] crystallizes in the monoclinic system, space group P2(1)/n, Z = 4, a = 9.5906(5) A, b = 16.704(4) A, c = 23.1417(6) A, beta = 100.453(7) degrees. [Fe(OEP)(CS)(Py)] crystallizes in the triclinic system, space group P1, Z = 5, a = 13.9073(6) A, b = 16.2624(7) A, c = 22.0709(9) A, alpha = 70.586(1) degrees, beta = 77.242(1) degrees, gamma = 77.959(1) degrees. [Fe(OEP)(CS)(CH(3)OH)] crystallizes in the triclinic system, space group P1, Z = 1, a = 9.0599(5) A, b = 9.4389(5) A, c = 11.0676(6) A, alpha = 90.261(1) degrees, beta = 100.362(1) degrees, gamma = 114.664(1) degrees. 相似文献
58.
Jie Shao Hai Lin Xue-Fang Shang Hua-Mei Chen Hua-Kuan Lin 《Journal of inclusion phenomena and macrocyclic chemistry》2007,59(3-4):371-375
A new urea-based receptor was designed to selectively recognize H2PO4− among other anions (such as F-, Cl-, Br-, I-, OH-, AcO-) in organic solvent (DMSO) through intermolecular hydrogen bonding. Addition of anions to the receptor caused changes in
UV–vis spectrum which provided the first indication of its anion binding ability.
Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users. 相似文献
59.
TiO2-双亲共聚物复合纳米粒子的合成与紫外光敏特性 总被引:3,自引:0,他引:3
用偶联剂乙烯基三乙氧基硅烷改性纳米粒子TiO2, 应用超声技术将TiO2 纳米粒子分散在甲醇介质中, 然后用苯乙烯(ST)原位聚合包封, 再用丙烯酰胺或乙烯基吡咯烷酮(VP)共聚, 两步原位分散聚合得到了有机聚合物为壳、TiO2为核的有机/无机复合粒子. 用红外光谱、紫外-可见光谱、透射电子显微镜等检测手段进行表征. 结果显示: 由于双亲共聚物对TiO2纳米粒子的敏化作用, 紫外-可见光谱图上两种纳米复合粒子的最大吸收峰均有明显红移, 并且吸收光谱的范围扩大了, 其中尤以TiO2/(PST-co-PVP)为甚. 意味着光敏化活性的提高, 特别是在可见光谱的范围内. 这种情形对宽带隙半导体材料如TiO2纳米粒子的光催化特性是有利的, 表明这类材料的应用空间得到了拓展. 相似文献
60.
在pH 3.2的酸性介质中,邻苯二酚与染料天青Ⅰ相互作用导致荧光强度明显增强,以发射波长343.0nm测定时,邻苯二酚的浓度在0.075~30μmol.L-1范围内与其荧光的增强程度呈线性关系,方法的检出限(3s/k)为7.51nmol.L-1。方法用于实际水样分析,加标回收率在97.0%~104%之间,测定值的相对标准偏差(n=5)在2.8%~3.9%之间。 相似文献