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991.
建立了高效毛细管电泳拆分阿苯达唑亚砜对映体的方法,考察了背景电解质pH、环糊精种类和浓度,有机改性剂种类和浓度对分离的影响,对分离条件进行了优化。实验结果表明:在含36g/L磺化β-环糊精和10%甲醇的20mmol/L Tris-H3PO4(pH2.5)缓冲体系中,阿苯达唑亚砜对映体具有良好的分离效果。 相似文献
992.
交替三线性分解算法与反相高效液相-二极管阵列检测方法相结合同时测定苯二酚的位置异构体 总被引:3,自引:0,他引:3
利用交替三线性分解算法与反相高效液相 二极管阵列检测 (RP HPLC DAD)相结合 ,在洗脱时间为1 0 86min~ 1 399min(间隔 1 / 1 50min)、紫外吸收波长为 2 68nm~ 2 98nm(间隔 1nm)时对苯二酚位置异构体的重叠及光谱体系进行了分辨研究。分辨结果与实际结果一致。同时测定了水溶液中共存的邻苯二酚、间苯二酚和对苯二酚的含量 ,回收率分别为 (1 0 0 1± 1 0 ) % ,(99 4± 1 4) % ,(1 0 0 5± 1 7) %。研究结果表明 :该方法定量快速准确 ,实验操作步骤简单 ,解决了在干扰物存在条件下三者很难同时分辨的问题。 相似文献
993.
K. H. Kim J. H. Lee M. Y. Ko K. S. Shin J. S. Kang W. C. Mar J. R. Youm 《Chromatographia》2002,55(1-2):81-85
Summary A method for the assay of R-(+)- and S-(−)- metoprolol in human urine has been developed using gas chromatography-mass spectrometry.
The method involved purification by liquid-liquid extraction and derivatization with N-methyl-N-(trimethylsilyl)trifluoroacetamide
to form an O-silyl ether, followed by subsequent chiral derivatization with (−)-α-methoxy-α-(trifluoromethyl)phenylacetyl
chloride to form diastereomeric amide. The reaction was rapid and the diastereomeric derivatives were well resolved. Quantitation
was performed by selected-ion monitoring of fragment ions of the diastereomers in electron impact ionization mode. No racemization
was found during the reaction. The detection limit was 0.5 ng·mL−1. The intra-day variation ranged between 0.38 and 7.86% in relation to the measured concentration and inter-day variation
was 2.26–8.06%. The method has been applied to the determination of R-(+)-and S-(−)- metoprolol in human urine from healthy
volunteers dosed with racemic metoprolol tartrate. 相似文献
994.
Abdulqawi NumanNeil D Danielson 《Analytica chimica acta》2002,460(1):49-60
The application of on-line photochemistry with flow injection (FI) and liquid chromatography (LC) in conjunction with atmospheric pressure electrospray mass spectrometry (LC-APESI-MS) for the identification of similar indole derivatives is reported here. The photo-transformation of the indole compounds is strongly affected by the substituent groups on the aromatic and heterocyclic rings. Upon photolysis for 2.5 min, the mass spectrum of tryptamine (Try) which has no OH substituent on the aromatic ring does not differ greatly from that obtained without photolysis. However, after photolysis of serotonin (Ser) which has one OH group on C5 of the aromatic ring, the mass spectrum indicates the formation of dimers and higher molecular weight ions. The fragmentation pattern of 5-hydroxytryptophol (Phol) without photolysis resembles that of Ser with a base peak of m/z 160. Upon photolysis using MeOH-H2O (10/90), Phol is found to form a base peak at m/z 375 (100%) and a major peak at m/z 214 (66%) in addition to other ions with lower abundance. Melatonin (Mel) and tryptophan (Phan) upon photolysis are found to form high molecular weight ions with a relative low abundance. The mass spectrum of indole-3-acetic acid (Inaa) with on-line photolysis also shows different ions that are not formed without photolysis. 相似文献
995.
J. Díaz-Ferrero M.C. Rodríguez-Larena L. Comellas B. Jiménez 《Trends in analytical chemistry : TRAC》1997,16(10):1865-573
The usual methods for determining polychlorinated dibenzo-p-dioxins (PCDD), polychlorinated dibenzofurans (PCDF) and polychlorinated biphenyls (PCB) are generally expensive and time consuming. This fact has favored the development of faster and cheaper techniques, based on immunoassays and bioassays. This paper reviews these bioanalytical methods and their analytical importance at the present moment. 相似文献
996.
997.
Pradip K. Bhowmik Robert W. Lenz 《Journal of polymer science. Part A, Polymer chemistry》1993,31(8):2115-2122
A series of fully aromatic thermotropic polyesters based on mono-, di-, and tetra-substituted biphenols was prepared by the melt polycondensation method and examined for their thermotropic behavior by a variety of experimental techniques. The homopolyesters obtained from substituted biphenols containing either one phenyl or two phenyl groups as substituent(s) and TA formed nematic melts, but the homopolymers of the substituted biphenols containing either four sec-butyl groups or two tert-butyl groups with TA had melting transitions, Tm, above 400°C. Thus, it was not possible to determine whether they formed nematic melts. On copolymerization with 30 mol % HBA most of the resulting copolyesters had much lower Tm values, compared to those of respective homopolyesters, and the copolymers of the biphenol monomer containing the tert-butyl groups formed a nematic melt at an observable temperature. However, the copolymer of the biphenol with sec-butyl groups still had a Tm above 400°C. © 1993 John Wiley & Sons, Inc. 相似文献
998.
《Surface and interface analysis : SIA》2004,36(1):92-95
By using modern XPS systems it is possible to obtain spectra with well‐resolved spin orbit, multiplet and field splitting even with powder samples mounted using adhesive tape. Measurement of Cr2O3 powder with the latest generation of XPS spectrometers, which are able to analyse non‐conductive powders with ultimate energy resolution, revealed multiplet splitting features and satellite emission in the Cr 2p spectrum. Therefore, peak‐fit analysis of Cr 2p XPS spectra of Cr(III) compounds requires a more appropriate approach and common practice has to be reconsidered. One possible way to analyse this spectrum is proposed, based on the experimental and theoretical work of other authors. Copyright © 2004 John Wiley & Sons, Ltd. 相似文献
999.
我国粘度计量工作中存在的问题 总被引:1,自引:0,他引:1
指出我国粘度计量工作中存在的一些问题,在修订粘度计检定规程,规范标准粘度的名称和有效期以及加强对粘度计检定工作的管理等方面的出了建议,强调了在标准粘度液证书中应给出不同温度下的运动粘度和粘度值,以满足粘度计检定工作的需要。 相似文献
1000.
Zai-Chang Y Bo-Chu W Xiao-Sheng Y Qiang W 《Colloids and surfaces. B, Biointerfaces》2005,43(3-4):198-202
The volatile oil of the roots of Cynanchum stauntonii was examined by gas chromatography–mass spectrometry (GC–MS). Thirty-eight constituents were identified. (E,E)-2,4-Decadienal, 3-efhyl-4-methypentanol, 5-pentyl-3H-furan-2-one, (E,Z)-2,4-decadienal and 2(3H)-furanone,dihydro-5-pentyl were found to be the major components. The volatile oil exhibited the activities against influenza virus in vitro (IC50s = 64 μg/ml). In in vivo experiment, it prevented influenza virus-induced deaths in a dose-dependent manner. 相似文献