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161.
Ning Li Chunhui Deng Ning Yao Xizhong Shen Xiangmin Zhang 《Analytica chimica acta》2005,540(2):317-323
In the study, we developed a simple, rapid, sensitive, and inexpensive method for determination of the disease biomarkers of acetone, hexanal and heptanal in human blood. For the first time, derivatization of carbonyls with O-2,3,4,5,6-(pentafluorobenzyl)hydroxylamine (PFBHA) was combined with headspace single-drop microextractin (HS-SDME) and gas chromatography-mass spectrometry (GC–MS) and applied to the analysis of acetone, hexanal, and heptanal in human blood. At first, acetone, hexanal and heptanal in blood were derivatized with PFBHA and formed oximes in several seconds. Sequentially, the oximes were headspace extracted and concentrated by a microdrop solvent. Finally, the extracted oximes were analyzed by GC–MS. HS-SDME conditions and method validations were studied. Due to needing of only 2 μl organic solvent, short extraction time of 8 min, and simple operation, derivatization-HS-SDME was shown to be a rapid, simple, and inexpensive technique for analysis of acetone, hexanal, and heptanal in human blood. Moreover, it had low detection limit values from 0.24 to 0.62 nM, and good reproducibility (R.S.D. less than 12%). 相似文献
162.
含氮宾的两个三核羰基铁簇合物是由[Et_3NH][HFe_3(CO)_(11)]与C_6H_5NCO在苯中反应获得。应用四园衍射仪测定了H_2Fe_3(N-C_6H_5)(CO)_9(Ⅰ)和Fe_3(N-C_6H_5)(μ_3-CO)(CO)_9(Ⅱ)的晶体结构。晶体数据为:C_(15)H_7NO_9Fe_3(Ⅰ),空间群P2_1/a,a=18.343(2),b=9.072(1),c=11.451(1)(?),β=102.03(1)°,V=1863.7(?)~3,Z=4,D_c=2.143g/cm~3;C_(16)H_5NO_(10)Fe_3(Ⅱ),空间群P2_1/c,a=8.634(1),b=13.026(1),c=17.642(2)(?),β=97.68(1)°,V=1966.3(?)~3,Z=4,D_c=1.820g/cm结构系用直接法解出,最后R_(Ⅰ)因子为0.033,R_(Ⅱ)因子为0.027。测定结果表明,(Ⅰ)和(Ⅱ)分子均具有C_s对称性,且三个Fe原子共面,呈近似等边三角形结构。(Ⅰ)中面桥N原子以不对称方式与三个Fe原子成键;(Ⅱ)中面桥羰基以不对称方式与三个Fe原子键连。Fe-N和Fe-C键长分别在1.896-1.938(?)和2.006-2.110(?)之间。 相似文献
163.
Ning Luo J. Brian Hutchison Kristi S. Anseth Christopher N. Bowman 《Journal of polymer science. Part A, Polymer chemistry》2002,40(11):1885-1891
(Methacryloyl ethylenedioxycarbonyl) benzyl N,N‐diethyldithiocarbamate (HEMA‐E‐In) was synthesized and used as a monomer iniferter to develop a novel, photopatternable grafting technology. This molecule functions as both a methacrylic monomer and a photoiniferter (photoinitiator–transfer agent–terminator). The structure of HEMA‐E‐In was characterized by 1H NMR, Fourier transform infrared, and ultraviolet–visible spectroscopies. In the presence of the monomer iniferter, methyl methacrylate was polymerized by exposure to 365‐nm ultraviolet radiation, confirming the initiation capability of HEMA‐E‐In. After the copolymerization of HEMA‐E‐In into a methacrylate‐based polymer, attenuated total reflectance Fourier transform infrared spectra revealed that the photoiniferter functionality was present at the surface of this polymeric substrate. Photografting of poly(ethylene glycol) monomethacrylate monomer from the surface caused a significant change in the hydrophobicity of the surface as demonstrated by contact angle measurements. The novel monomer photoiniferter HEMA‐E‐In initiates the polymerization of bulk monomer and provides a reactive functionality that facilitates further initiation and polymer modification by the polymerization of different monomers. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 1885–1891, 2002 相似文献
164.
WU Yan-Qi LOU Ning LI Yu 《有机化学》2003,23(Z1):442-442
From the ethanolic extract of the whole plant of Anaphalis aureo-punctata, a new acylated flavonoid glycoside 3-O-kaempferol-3-O-acetyl-6-O-(p-coumaroyl)-β-D-glucopyranoside (1), and five known phenolic compounds 3-O-kaempferol-6- O- ( p-coumaroyl )-β-D-glucopyranoside ( 2 ), kaempferol-3- O-β-D-glucopyranoside 3,6-(4′-hydroxystyryl)-4-methoxy-2-pyrone (4), 2H-pyran-2-one, 6-[ 2-( 4-(β-D-glucopyranosyloxy ) phenyl ) ethenyl ]-4-methoxy-( E ) (5) and 4-hydroxy-3-methoxycinnamic hexacosyl ester (6) were isolated. Their structures were established by spectral methods (UV, IR, MS, 1D, 2D-NMR). The flavonoid glycosides, 1, 2 and 3 showed markedly inhibited oxidative DNA strand breaks induced by Fenton reaction and NADH/PMS in a concentration-dependent manner. 相似文献
165.
Ronghu W Xijuan Y Huiyu S Qingde S 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2003,59(13):2915-2920
The structural variations of silica gels heated at different temperatures have been firstly studied using Nd(3+) as a probe by photoacoustic spectroscopy (PAS), together with IR spectroscopy and thermal analysis. With increasing temperature, the f-f transitions of Nd(3+) show a red shift and the PA intensities increase. The PA branching vector of the transitions from ground state to 4G(5/2)+(2)G(7/2), which are hypersensitive transitions, increase and the others decrease or change little. These indicate that the covalency of the bond that Nd(3+) forms increases and the symmetry around Nd(3+) decreases, which reflects the structural variations of silica gels. 相似文献
166.
167.
Determination of Organophosphorus Pesticides in Soil by MMSPD-GC-NPD and Confirmation by GC-MS 总被引:1,自引:0,他引:1
A novel method, modified matrix solid-phase dispersion (MMSPD), has been developed for quantitative analysis of organophosphorus
pesticide residues in soil. It was based on matrix solid-phase dispersion (MSPD) and continuous liquid-solid extraction (continuous
LSE), using Florisil as sorbent and dichloromethane as the recycling solvent. Two soils with different texture and physicochemical
properties were studied to validate the method. The effect of residence time of pesticides in soil was also studied. MMSPD
was compared with MSPD and continuous LSE respectively. Determination was carried out by gas chromatography with nitrogen-phosphorus
detection (GC-NPD). The method gave recoveries ranging from 72–105% with relative standard deviations (RSDs) lower than 15%
for the pesticides studied. The limits of detection (LODs) ranged from 0.1 to 0.6 ng g−1. Two pesticide residues have been detected in real soil samples from Fujian, China, using MMSPD. The pesticides were confirmed
by gas chromatography-mass spectrometry (GC-MS) in a selected-ion monitoring (SIM) mode.
Revised: 4 and 9 April 2006 相似文献
168.
二苄亚砜硝酸钕Nd(NO_3)_3·[(C_6H_5CH_2)_2S0]属三斜晶系,P1空间群,晶胞参数:a=9.835(2),b=12.445(2),c=19.971(5)A,α=104.13(2)°,β=90.34(2)°γ=74.96(1)°Z=2。晶体结构用重原子法解出,经最小二乘修正后R因子为0.031。钕离子由九个氧配位,形成稍歪扭的三帽三方棱柱配位多面体,其中一个三角面由三个二苄亚砜(DBSO)提供的氧形成,其他氧原子则由硝酸根提供。平均Nd-O(DBSO)=2.379A,Nd-O(NO_3)=2.536A。 相似文献
169.
In the present paper, we describe a microfluidics-based sensing system for nonelectroactive anions under negative separation electric field by mounting a single carbon fiber disk working electrode (WE) in the end part of a poly(dimethylsiloxane) microchannel. In contrast to work in a positive separation electric field described in our previous paper (Anal. Chem. 2004, 76, 6902-6907), here the electrochemical reduction reaction at the WE is not coupled with the separation high-voltage (HV) system, whereas the electrochemical oxidation reaction at the WE is coupled with the separation HV system. The electroactive indicator is the carbon fiber WE itself but not dissolved oxygen. This provides a convenient and sensitive means for the determination of nonelectroactive anions by amperometry. The influences of separation voltage, detection potential, and the distance between the WE and the separation channel outlet on the response of the detector have been investigated. The present detection mode is successfully used to electrochemically detect F-, Cl-, SO4(2-), CH3COO-, H2PO4-. Based on the preliminary results, a detection limit of 2 microM and a dynamic range up to three orders of magnitude for Cl- could be achieved. 相似文献
170.