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801.
Lumbierres M Palomo JM Kragol G Roehrs S Müller O Waldmann H 《Chemistry (Weinheim an der Bergstrasse, Germany)》2005,11(24):7405-7415
A new flexible and efficient methodology for the solid-phase synthesis of lipidated peptides has been developed. The approach is based on the use of previously synthesized building blocks and overcomes the limitations of previously reported methods, since long doubly lipidated peptides can be synthesized by using this route. Furthermore, it was thus possible to prepare a large number of N- and H-Ras peptides bearing a wide range of reporter and/or linking groups--efficient tools for the investigation of biological processes. In terms of efficiency and flexibility this solid-phase method is superior to the solution-phase synthesis. It gives pure peptides in multimilligram amounts within a much shorter time and with superior overall yield. 相似文献
802.
Simplified Solid-Phase Extraction Procedure and Liquid Chromatographic Determination of Celecoxib in Rat Serum 总被引:1,自引:0,他引:1
A simplified solid phase extraction method, eliminating a preliminary protein precipitation has been developed for the determination of celecoxib in rat plasma. The technique included a solid phase extraction of the serum samples on a [poly (divinylbenzene-co-N-vinylpyrrolidone)] sorbent. After conditioning, the cartridge was loaded with 0.5 mL of acidified serum containing internal standard. Elution was made with 1 mL of a mixture of acetonitrile and methanol (1/1, v/v). After evaporation of the eluate to dryness and reconstitution with methanol, the samples were analyzed on an octadecyl bonded phase with several mobile phases containing acetonitrile and a phosphate buffer. Detection was carried out using a Photodiode Array Detector. Full validation of the proposed method was provided (linearity range: 0.01–2 mg. L–1, average extraction efficiency: 92.4%; average intra-day variability: 4.6% with an accuracy of 94.8%; average interday variability: 5% with an accuracy of 95.3%, limit of detection: 0.005 mg. L–1, limit of quantification: 0.002 mg. L–1). The proposed method was successfully utilised to quantify celecoxib in rat plasma for a pharmacokinetic study.Revised: 26 January and 23 April 2004 相似文献
803.
通过酸洗、硅烷偶联剂表面活化、键合苯甲酰异硫氰酸酯对蒙脱土进行改性,制得新型固相萃取(SPE)材料。 采用红外光谱、扫描电子显微镜、X射线光电子能谱表征了改性蒙脱土的结构和形貌。 考察了制备的SPE填料对水中As3+、Bi3+、Cu2+、Sb3+、Sn2+和Pb2+的吸附性能,确定了最佳固相萃取条件,对6种金属离子吸附容量分别为10.83、11.92、12.67、10.43、10.01及10.54 mg/g。 通过SPE与电感耦合等离子体质谱联用测定了样品中As3+、Bi3+、Cu2+、Sb3+、Sn2+和Pb2+ 6种重金属离子的含量,检出限分别为0.024、0.013、0.075、0.037、0.011和0.064 μg/L。 相似文献
804.
以不同种类的离子液体作为相转移催化剂,用双氧水作为氧化剂,Na2WO4·2H2O为催化剂,在适当的反应条件下,能有效进行相转移催化环己醇氧化制备环己酮.实验结果表明,采用酸性离子液体[C16mim]HSO4和[C14mim]HSO4相转移催化合成环己酮,可提高环己酮的产率,具有反应条件温和、操作简便、需用时间短、相转移催化剂可以循环使用等优点.在反应温度为90℃,反应时间为50min条件下,环己醇的转化率高达100%,选择性99%以上. 相似文献
805.
The reaction of fluorobenzene with urotropine in trifluoroacetic acid (TFAA) at high pressures and temperatures affords predominantly fluorobenzaldehydes andN-(fluorophenylmethyl)trifluoroacetamides. The yields of these products depend considerably on the reaction conditions. The rates of their formation have the maximum values at the momemt of the phase transition (PT) of TFAA. A new efficient cyclic (dynamic) regime is proposed for the synthesis at high pressures. The regime involves periodically occurring PT of the solvent. The change in the relative rate of product formation with the degree of fluorobenzene conversion is wave-like.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 319–323, February, 1995. 相似文献
806.
G. E. Nikiforova V. B. Lazarev I. S. Shaplygin 《Journal of Thermal Analysis and Calorimetry》1993,40(1):373-378
The termal stabilities of several families of high-T c superconductors (HTSC), as well as the dependence of phase transitions on temperature and stoichiometry, have been studied by X-ray diffraction, DTA, TG and DSC. Experimental results are discussed in the context of decomposition models. 相似文献
807.
On the plastic deformation of bulk syndiotactic polypropylene 总被引:1,自引:0,他引:1
The plastic deformation of syndiotactic polypropylene (sPP) bulk samples has been investigated. A structural comparison of
the initial states before and after plastic deformation by necking is carried out by X-ray diffraction observations. Independent
of the initial states (amorphous, semi-crystalline with different crystal phases), only the planar all-trans crystal form of sPP is present in the deformed samples after necking. Form these results, molecular mechanisms of the plastic
deformation in the neck zone of semi-crystalline polymers will be discussed.
Received: 11 February 1997 Accepted: 15 August 1997 相似文献
808.
Helga Mikler 《Monatshefte für Chemie / Chemical Monthly》1989,120(1):7-10
Summary Using a high pressure X-ray camera Cu2HgI4 was subjected at room temperature to pressures up to about 8 GPa. A hexagonal high pressure phase (a=8.28 (2) Å,c=3.40 (0) Å, space group P
lm,Z=1) could be detected. This phase shows a reversible transformation with pressure hysteresis. The transition occurs at 7 GPa when the pressure is increased but at 6 GPa when the pressure is decreased.
Hexagonale Hochdruckphase von Kupfer(I)tetraiodomercurat (Cu2HgI4)
Zusammenfassung Cu2HgI4 wurde in einer Hochdruckkamera bei Raumtemperatur mit einem Druck bis zu 8 GPa belastet. Dabei bildete sich eine hexagonale Hochdruckmodifikation (a=8.28 (2) Å,c=3.40 (0) Å, Raumgruppe P lm,Z=1). Für diese Phase wurde eine reversible Umwandlung mit Druckhysterese festgestellt. Mit steigendem Druck findet die Umwandlung bei 7 GPa mit sinkendem Druck jedoch bei 6 GPa statt.相似文献
809.
Yu. A. Dyadin F. V. Zhurko T. V. Mikina R. K. Udachin 《Journal of inclusion phenomena and macrocyclic chemistry》1990,9(1):37-49
P,T,X phase diagrams of the CH2Cl2-H2O, the CHCl3-H2O and the CCl4-H2) systems have been studied by DTA in the pressure range 10–3 to 5.0 kbar. Under pressure the cubic structure II (CS-II) hydrates forming in all the systems are replaced by hydrates with the composition M·7.3 H2O whose stoichiometry and positive dT/dP values of melting lead us to believe that they are CS-I hydrates.In the CH2Cl2 and CHCl3 systems the nonvariant point coordinates of the hydrate transformationQ
2
h
(l1h17h7l2, where l1 and l2 are liquid phases abundant in water and hydrate former, respectively, h17 and h7 are hydrates with hydrate numbers 17 and 7, respectively) areP = 0.6 kbar, T = –1.5°C andP =2.65 kbar,T = –10.5°C, respectively. In the CCl4 system the 4-phaseQ
3
h
point (l1h17h7s, where s is crystalline CCl4) has coordinatesP = 0.75 kbar and T = 0.4°C.The main obstacle of the present study, the very slow achievement of equilibrium, has been eliminated by adding small amounts (0.25% by mass) of surfactants followed by ultrasonic mixing. We have shown that this accelerates the achievement of equilibrium without changing its position. 相似文献
810.
Harald Greger Otmar Hofer Andreas Werner 《Monatshefte für Chemie / Chemical Monthly》1985,116(2):273-277
In addition to the well known affinin [=spilanthol, (2E,6Z,8E)-deca-2,6,8-trienoic acid isobutylamide (1)], the corresponding 2-methyl-butylamide (2), and two new acetylenic alkamides were isolated fromSpilanthes oleracea L. by reversed phase medium pressure chromatography: (Z)-non-2-en-6,8-diynoic acid isobutylamide (3) and (Z)-dec-2-en-6,8-diynoic acid isobutylamide (4). The structures and their stereochemistries were elucidated by1H-NMR,13C-NMR (2 and3), MS, UV, IR, and CD (2). The chemotaxonomic significance of the distribution of alkamides within theCompositae tribeHeliantheae is briefly discussed.
Neue Amide ausSpilanthes oleracea (Kurze Mitteilung)
Zusammenfassung AusSpilanthes oleracea wurden neben dem seit langem bekannten Affinin [=Spilanthol, (2E,6Z,8E)-Deca-2,6,8-triensäureisobutylamid (1)] durch Umkehrphasen-Mitteldruckchromatographie das entsprechende 2-Methylbutylamid (2) und zwei neue acetylenische Alkamide isoliert: (Z)-Non-2-en-6,8-diinsäure-isobutylamid (3) und (Z)-Dec-2-en-6,8-diinsäure-isobutylamid (4). Die Strukturen und deren Stereochemie wurden mittels1H-NMR,13C-NMR (2 und3), MS, UV, IR und CD (2) aufgeklärt. Die chemotaxonomische Bedeutung der Verbreitung von Alkamiden innerhalb der Compositen-TribusHeliantheae wird kurz diskutiert.相似文献