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121.
Preparative separation of methyl gallate in leaves extract of Acer truncatum Bunge was conducted using high-speed counter-current chromatography (HSCCC) with a solvent system composed of ethyl acetate-ethanol-water at volume ratios of 5:1:5 (v/v/v). In a single operation, 57.5 mg of methyl gallate was obtained from 120 mg of the extract. HPLC analyses of the counter-current chromatography (CCC) fraction revealed that the methyl gallate was having over 97% purity. Its structure was identified by 1H NMR and 13C NMR. 相似文献
122.
Wei-Zhi Tian 《Journal of Radioanalytical and Nuclear Chemistry》1987,111(2):449-468
A neutron spectrum-independent compound nuclear constant, Iko, is proposed for fission interference corrections in reactor NAA by parametric method. Ik0 values for eight major fission interference cases, belonging to three different types, have been determined in six irradiation positions (with
th/
e 13,7–134) of three research reactors in our Institute. The general agreement among experimental Ik0 's from different irradiation positions and between experimental and calculated Ik0 values for the same interference case verifies the validity of the method. Calculated Ik0 values for all the possible fission interferences are tabulated. Interferences from238U(n,) and232Th(n,) reactions and reactor fast neutron induced238U(n, f) and232Th(n, f) reactions are discussed. 相似文献
123.
A new anthraquinone glycoside, rubiayannone‐A ( 1 ), and a new coumarin, rubilatin‐A ( 2 ), together with twenty‐two known compounds were isolated and characterized from the roots of Rubia ustulata. A new anthraquinone, 2‐carbomethoxyanthraquinone ( 3 ), and rubiayannone‐A, 2‐formylanthraquinone were obtained from the roots of R. yunnanensis. The structures of those compounds were elucidated by spectroscopic methods. The antiplatelet aggregation activity of the isolated compounds 1, 4~6 were also discussed. 相似文献
124.
Huilan C Deyan H Tian L Hong Y Wenxia T Jian Chen J Peiju Zheng P Chenggang Chen C 《Inorganic chemistry》1996,35(6):1502-1508
Alkylcobalt(III) Schiff base B(12) model complexes with secondary alkyls or a bulky diamine in the equatorial position were synthesized and characterized. Structures have been first determined by X-ray diffraction analysis for i-C(4)H(9)Co(salen)(gamma-pic) (I), n-C(3)H(7)Co(salen)(gamma-pic) (II) and C(2)H(5)Co(SB) (III), where salen = N,N'-ethylenebis(salicylideneamine) dianion; SB = 1,1,2,2-tetramethyl-N,N'-ethylenebis(salicylideneamine) dianion, gamma-pic = gamma-picoline. Crystal data for I (CoC(26)N(3)O(2)H(30)): space group P2(1)/c with a = 6.661(5) ?, b = 18.612(2) ?, c = 19.533(3) ?, beta = 98.93(1) degrees, V = 2392.10 ?(3), D(calcd) = 1.320 g.cm(-3), Z = 4, and R = 0.048 for 4469 measured reflections. Crystal data for II (CoC(25)N(3)O(2)H(28)): space group P2(1)/c, a = 9.609(6) ?, b = 19.169(8) ?, c = 12.995(9) ?, beta = 106.9(7) degrees, V = 2290.4 ?(3), D(calcd) = 1.332 g.cm(-1), Z = 4, and R = 0.048 for 4358 measured reflections. Crystal data for III (CoC(22)N(2)O(2)H(27)): space group P2(1)/c, a = 8.318(3) ?, b = 21.579(2) ?, c = 11.572(2) ?, beta = 93.35(1) degrees, V = 2073.7 ?(3), D(calcd) = 1.314 g.cm(-1), Z = 4, and R = 0.060 for 3954 measured reflections. The crystal structure data reveal that complexes I and II display six-coordinate octahedral geometry; their Co-C, Co-N bond lengths, as well as the Co-C-C angles, are very close to those in 5'-deoxyadenosylcobalamin. Complex III is one of the very few compounds having five-coordinate square pyramidal geometry and observed instability of the Co-C bond. 相似文献
125.
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
126.
127.
128.
This paper reports an improved catalytic molecular beacon. Addition of the target oligonucleotide activates a DNA enzyme (DNAzyme), which, in turn, activates multiple copies of molecular beacons (MB) and gives rise to a strong fluorescence signal. In a previous design, the activated DNAzyme could oligomerize, especially dimerize, and result in inactivation of the DNAzyme. The current design avoids this problem, upon activated by the target DNA, the DNAzyme will stay constantly active. With the improved method, a detection of 10 pM DNA has been demonstrated, which is 1000 times more sensitive than the method previously reported. 相似文献
129.
运用三足四齿配体三(2-甲基吡啶)胺(TPA)或三(2-甲基苯丙咪唑)胺(TBA),得到两个双核铁(III)配合物,[Fe2L2(μ2-O)(μ2-p-NH2-C6H4COO)]3+
(L = TPA, 1 和 L = TBA,
2)。两个配合物均为单斜晶系,空间群为P2(1)/c.晶胞参数 1: a =
1.4529(4), b = 1.6622(5), c = 2.0625(6) nm, β= 100.327(5)º,
V = 4.900(3) nm3, z = 4, F(000) = 2344, 分子量Mr = 1142.91, Dc
= 1.549 g/cm3, R1 = 0.0544,
R2 = 0.0962. 2: a = 1.3378(4), b = 2.1174(7), c =
2.4351(7) nm, β= 97.315(6)º, V = 6.842(4) nm3,
z = 4, F (000) = 3116, 分子量Mr = 1505.08, Dc
= 1.444 g/cm3, R1 = 0.0793, R2 = 0.1623. 在两个双核铁(III)配合物中,中心的三价铁和配体TPA或TBA上的四个氮原子和两个氧原子通过不同的桥形成一个畸变的八面体构型。 相似文献
130.