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991.
Speciation analysis of selenomethylcysteine (SeMeCys), selenomethionine (SeMet) and selenocystine (SeCys) has been performed using a direct amino acid analysis method with high-performance anion-exchange chromatography (HPAEC) coupled with integrated pulsed amperometric detection (IPAD). Three selenoamino acids could be baseline-separated from 19 amino acids using gradient elution conditions for amino acids and determined under new six-potential waveform. Detection limits for SeMeCys, SeMet and SeCys were 0.25, 1 and 20 microg/L (25 microL injection, 10 times of the baseline noise), respectively. The relative standard deviations (RSDs) of 200 microg/L SeMeCys, SeMet and SeCys were 3.1, 4.1 and 2.8%, respectively (n=9, 25 microL injection). The proposed method has been applied for determination of selenoamino acids in extracts of garlic and selenious yeast granule samples. No selenoamino acids were found in garlic. Both SeMet and SeCys were detected in selenious yeast tablet with the content of 45 and 129 microg Se/g, respectively. Selenoamino acids standards were spiked in garlic and yeast granule samples and the recovery ranged from 90 to 106%. 相似文献
992.
An on-line coupled continuous flow liquid membrane extraction (CFLME) and C18 precolumn system was developed for sample preconcentration in liquid chromatography determination. After preconcentration by CFLME, which is based on the combination of continuous flow liquid–liquid extraction and supported liquid membrane, bisphenol A (BPA) was enriched in 960 μl of 1 mol l−1 NaOH used as acceptor. This acceptor was on-line neutralized and transported onto the C18 precolumn where analytes were absorbed and focused. Then the focused analytes were injected onto a C18 analytical column for separation and detected at 220 nm with a diode array detector. CFLME related parameters such as flow rates, pH of donor and acceptor, and enrichment time were optimized. The proposed method presents a detection limit of 0.03 μg l−1 (S/N=3) when 60 ml samples was enriched with an enrichment time of 30 min. Compared with C18 based column-switching procedure, this proposed procedure presents similar sample throughput and lower detection limits. The proposed method was successfully applied to determine BPA in tap water, river water, and municipal sewage effluent samples. 相似文献
993.
Eight ionic organotin compounds [R2SnCl2(2-quin)]−(HNEt3)+ have been synthesized by reactions of 2-quinH with R2SnCl2 (R = PhCH21, 2-Cl-C6H4CH22, 4-Cl-C6H4CH23, 2-F-C6H4CH24, 4-F-C6H4CH25, 4-CN-C6H4CH26, Ph 7, 2,4-Cl2-C6H3CH28) in the presence of organic base NEt3, and their structures have been characterized by elemental analysis, IR and multinuclear NMR (1H, 13C, 119Sn) spectroscopies. The structure of [(2,4-Cl2-C6H3CH2)2SnCl2(2-quin)]−(NEt3)+ (8) has been determined by X-ray diffraction study. Studies show that compound 8 has a monomeric structure with the central tin atom six-coordinate in a distorted octahedral configuration and the nitrogen atoms of the 2-quin ligands are coordinating to the tin atom in all the eight compounds. 相似文献
994.
Ab initio electronic structure calculations are reported for low-lying electronic states, 1A1, 1A2, 3A2, 1B1, 3B1, 1B2, and 3B2 of the FNO2 molecule. Geometric parameters for the ground state 1A1 are predicted by MRSDCI calculations with a double-zeta plus polarization basis set. The vertical excitation energies for these electronic states are determined using MRSDCI/DZ+P calculations at the ground-state equilibrium conformation. The oscillator strengths and radiative lifetimes for some electronic states are calculated based on the MRSDCI wave functions. © 1993 John Wiley & Sons, Inc. 相似文献
995.
This paper describes the results of the evaluation of retention dependence on the physicochemical properties of solutes in linear gradient elution by reversed-phase liquid chromatography (RPLC) based on linear solvation energy relationships (LSERs). Retention time data on Inertsil ODS(3) column by linear gradient elution were collected for both acetonitrile-water and methanol-water binary mobile phases under various gradient steepness. Based on the LSERs, the retention times were linearly correlated with the physicochemical properties (size, dipolarity, and hydrogen bond donor-acceptor acidity and basicity) of solutes. As predicted by LSERs, very acceptable linear relationships are observed for both mobile phases. While the magnitudes of the coefficients are modified by the gradient steepness, their signs are consistent with those obtained by isocratic elution. As obtained for isocratic elution, the dominant factors to retention in linear gradient elution of RPLC are the solutes' size and hydrogen bond acceptor basicity. The conclusions of the study allow us to predict retention in chromatographic method development by gradient elution. 相似文献
996.
Facile construction of novel organolanthanide square-planar macrocycles through addition of carbodiimide to an amino group 总被引:1,自引:0,他引:1
Ma L Zhang J Cai R Chen Z Zhou X 《Dalton transactions (Cambridge, England : 2003)》2007,(25):2718-2722
The reactivity of lanthanocene derivatives containing the p-aminothiophenolate ligand towards carbodiimide was examined. Reaction of Cp2Ln(p-SC6H4NH2)(THF) with RN=C=NR in THF at room temperature gave four novel organolanthanide guanidinate complexes [Cp2Ln(p-SC6H4N(H)C(NHR)=NR)]4 (R = iPr, Ln = Yb (1a), Er (2a); R = Cy, Ln = Yb (2a), Er (2b)), formed by the addition of the C[double bond, length as m-dash]N double bonds of the carbodiimide molecule to the para-position amino group. Their unique square-planar macrocycle structures have been determined through X-ray single-crystal diffraction analysis. This result provides a potential method for the construction of organolanthanide macrocycles. 相似文献
997.
998.
Liu H Zhang X Gao H Wang N Jin S Cai B Yao X Cai G 《Chemical & pharmaceutical bulletin》2005,53(10):1310-1313
Phytochemical study of the ethanol extract of the seeds of Aesculus assamica led to the isolation of two new triterpenoid saponins. The structure of the new compounds were elucidated on the basis of spectral data to be 28-O-acetyl-21-O-(4-O-angeloyl)-6-deoxy-beta-glucopyranosyl-3-O-[beta-glucopyranosyl(1-2)-O-[beta-glucopyranosyl(1-4)]-beta-glucuronopyranosyl]protoaescigenin (1), and 21-O-(4-O-angeloyl)-6-deoxy-beta-glucopyranosyl-3-O-[beta-glucopyranosyl(1-2)-O-[beta-glucopyranosyl(1-4)]-beta-glucuronopyranosyl]protoaescigenin (2). Their in vitro bioactivity against plant pathogenic fungus Pyricularia oryzae and cytotoxicity against K562 and HCT-15 cell lines were evaluated. 相似文献
999.
Promotion of Ionic Liquid to Dimethyl Carbonate Synthesis from Methanol and Carbcn Dioxide 总被引:2,自引:0,他引:2
Promotion of ionic liquid, 1-ethyl-3-methylimidazolium bromide (emimBr), to the synthesis of dimethyl carbonate (DMC) from methanol and carbon dioxide in the presence of potassium carbonate and less amount of methyl iodide under mild conditions was investigated. The results showed that the high selectivity and raised yield of DMC was achieved due to the addition of emimBr in the reaction system. And effect of several reaction conditions such as temperature, pressure and amount of emimBr was discussed. 相似文献
1000.
CuI/N,N-dimethylglycine-catalyzed coupling reaction of L-tyrosine derivatives and L-phenylalanine-derived iodides in the presence of Cs2CO3 works at 90 degrees C to provide the corresponding diaryl ether. Partial racemization occurs when N-Boc- and N-Cbz-protected aromatic amino esters are used, while N-trityl- and N,N-dibenzyl-protected aromatic amino esters give rise to coupling products without loss of optical purity. Little racemization is also observed in cases of N-Boc- and N-Cbz-protected aromatic amino acids as substrates. But their reaction yields are moderate. On the basis of these studies, shorter protocols for assembling (S,S)-isodityrosine and K-13 are developed. 相似文献