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151.
以万古霉素为流动相添加剂的高效液相色谱法手性分析系统的建立 总被引:2,自引:0,他引:2
以丹酰化苯甘氨酸、丹酰化苯丙氨酸、丹酰化丝氨酸、丹酯化丙氨酸为模型化合物,通过对色谱柱类型、缓冲液类型、pH和盐浓度、万古霉素用量、甲醇用量、柱温等色谱参数进行考察,建立了以万古霉素为手性流动相添加剂在普通色谱柱上进行手性分析的色谱系统,并在该系统中成功地拆分了酮洛芬对映体。 相似文献
152.
The qualitative analysis of bufadienolides in the Chinese drug ChanSu was performed using high-performance liquid chromatography with atmospheric pressure chemical ionization tandem mass spectrometry (APCI-MS/MS). Bufadienolides are the major bioactive constituents of ChanSu, which is used to treat heart failure and cancer in traditional Chinese medicine. The APCI-MS fragmentation behavior of bufadienolides was studied. For bufadienolides with only hydroxyl substituents, the fragmentation was characterized by successive eliminations of H(2)O and CO molecules, and the profile of MS/MS product ions was correlated with the number of hydroxyl groups. If a C-16 acetoxyl group was present, the fragmentation of [M+H](+) ions was triggered by initial loss of 60 Da (HOAc). The elimination of CO was significant for bufadienolides with a 19-formyl group, and the 19-hydroxyl group could be characterized by the loss of 30 Da (HCHO). These fragmentation rules were applied to the identification of bufadienolides in a methanolic extract of ChanSu, which was separated on a C(18) column with gradient elution. A total of 35 bufadienolides were identified, including four new constituents. The method established here facilitated the convenient and rapid quality control of ChanSu crude drug and its pharmaceutical preparations. 相似文献
153.
A high-performance capillary electrophoresis with electrochemical detection (CE-ED) method has been employed for the determination of six bioactive ingredients in traditional Chinese herbs, Herba cepbalanoplosis segeti and Herba cirsii japonici. The effects of several factors such as the acidity and concentration of running buffer, the separation voltage, the applied potential and the injection time on CE-ED were investigated. Under the optimum conditions, the six analytes could be well separated within 21 min in a 75 cm length capillary at the separation voltage of 15 kV in a 50 mmol L–1 borax running buffer (pH 8.4). A 300 m diameter carbon disk electrode was used as the working electrode positioned carefully opposite the outlet of the capillary in a wall-jet configuration at potential of +950 mV (vs. SCE). Good linear relationship was established between peak current and concentration of analytes over two orders of magnitude with detection limits (S/N=3) ranged from 1.5×10–7 to 6.0×10–7 g mL–1 for all six analytes. This proposed method has been successfully applied for the analysis of traditional Chinese herbs after a relatively simple extraction procedure, further on, for the differentiation of these above two seemingly identical herbs based on their electropherograms or characteristic electrochemical profiles. 相似文献
154.
The guaianolide ester is a potent inhibitor of cancer cells. Lactucopicrin, a guaianolide, shows analgesic, antitussic, and sedative activities. In order to investigate its structure, 1H and 13C NMR and 2D NMR have been carried out at a proton field strength of 400 MHz and a carbon field strength of 100 Mhz in DMSO-d
6 at 20°C. Resonances for all protons and carbons have been assigned. The results of HMQC and HMBC experiments suggest that the structure of lactucopicrin is as shown in Fig. 1. Its stereostructure is verified by the X-ray experiment. 1H and 13C NMR of lactucopicrin are reported. Its 2D NMR and X-ray are reported for the first time. 相似文献
155.
A second-order nonlinear optical polyurethane was formed with an X-type multi-dimensional charge-transfer (CT) chromophore (DNPIPDHPI) and 3,3′-dimethoxy-4,4′-diphenyl diisocyanate. Simultaneous poling and polymerization and in situ second harmonic generation (SHG) measurement technique was carried on to evaluate the thermal stability of the poling induced orientation. The SHG signal of the poled polymer film was not decay below 150 °C and remains 90% of relative d33 value at 200 °C, which is better than the results reported in literature. Comparison of thermal stability indicates that the X-type chromophores possess better property in controlling the decay of the SHG activity than classic chromophores. 相似文献
156.
157.
Shen J Ye Y Hu J Shen H Le Z 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2001,57(3):551-559
Copper(II), zinc(II), cobalt(II) and cobalt(III) complexes of N-D-glucosamine beta-naphthaldehyde (C17H19O6N, NG) and glycine were synthesized. The four novel metal complexes, Cu(II)C19H28O11N2(CuGNG), Zn(II)C19H24O9N2 (ZnGNG), Co(II)C19H28O11N2(Co(II)GNG) and Co(III)C21H29O12N2(Co(III)GNG) were characterized by means of infrared (IR), electronic absorption spectroscopy and NMR etc. The surface-enhanced Raman spectra of the four complexes and their interaction with DNA were studied. By comparison of the surface-enhanced Raman spectra (SERS), the information of the four complexes' SER active sites and adsorption orientation were obtained. Combined with fluorescence spectra of Ethidium bromide (EthBr) DNA system, we concluded that none of the four complexes intercalate into DNA and that the presence of the glycine ligand lowered the anticancer activity of NG series complexes. 相似文献
158.
邻苯二亚胺纤维素水溶液的荧光行为 总被引:3,自引:0,他引:3
目前,用于制造光致发光材料的基材均为合成高分子材料,如聚氯乙烯(PVC)等热塑性材料以及不饱和聚酯等热固性材料[1].天然高分子材料发光性能的研究并不多见.而与合成高分子相比,纤维素的结构特征决定了它易参与化学反应,可用以制备各种用途的功能材料,如高... 相似文献
159.
V. Ye. Zaichick 《Journal of Radioanalytical and Nuclear Chemistry》1993,169(2):307-316
A facility developed for the in-vivo neutron activation analysis (IVNAA) of calcium in some parts of tubular limb bones, in the hand, foot and spine is described. The48Ca(n, )49Ca reaction is used, the gamma-rays of49Ca (E=3.08 MeV, T1/2=8.8 min) are measured. The irradiation is carried out with five of ten238Pu–Be neutron sources with a source stength of 5·107 n s–1 each arranged in a bath filled with water. NaI(T1) detectors (from 2 to 4 in number) of 150×100 mm size supplied with lead and shadow shielding are used in the counting unit. The construction of the facility started in 1972 and has been in operation since 1974. It has been used for the examination of patients suffering from limb bone tumors, of children with rickets-like and similar diseases and for studies in space medicine. 相似文献