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91.
Jerald S. Bradshaw Reed M. Izatt James J. Christensen Krzystof E. Krakowiak Bryon J. Tarbet Ronald L. Bruening S. Lifson 《Journal of inclusion phenomena and macrocyclic chemistry》1989,7(2):127-136
Silica gel-bound crown ethers and aza macrocycles have been synthesized with the attaching arm connected to the carbon framework of the macrocycles. The interactions of these bound macrocycles with cations are almost identical to those involving the analogous free macrocycles. This has allowed for predictable cation separation, concentration, and removal processes to be performed on a small scale. Quantum mechanical calculations and NMR measurements indicate that similarly bound chiral macrocycles will be capable of use in separating chiral organic amines.Dedicated to the memory of Professor James J. Christensen who died on 5 September 1987. 相似文献
92.
93.
Summary A simple and rapid systematic optimization scheme was described for the micellar electrokinetic chromatographic separation of a group of flavonoids. The scheme employed an interpretative optimization approach to predict the optimum conditions for the separation of a group of flavonoids by micellar electrokinetic chromatography. By performing a set of nine pre-planned experiments conducted over the maximum working range for the system, global optimum separation conditions could be determined. To validate the optimization procedure, additional experiments were performed using the optimum experimental conditions derived from the optimization scheme. The results showed that satisfactory separation of all the peaks could be obtained. In addition, the application of the method in micropreparative micellar electrokinetic chromatography of the flavonoids was demonstrated. 相似文献
94.
In this study porous glass fiber membranes were modified by reaction with octadecyl-trichlorosilane to form C18 hydrophobic membranes. The contact angle and the CH2 vibration bands at 2855 and 2920 cm(-1) found by FTIR measurements verified the successful immobilization of C18 groups on the glass fiber membranes. The resulting C18 hydrophobic membranes were used to adsorb terpene lactones from crude Ginkgo biloba L. extracts. In batch adsorption processes, the modified C18 membranes exhibited a better adsorption performance than commercial C18 solid phase extraction adsorbents. Different desorption solvents were tested and ethyl acetate was found to preferentially desorb terpene lactones from the modified C18 membranes. In flow adsorption experiments at 1 mL/min, terpene lactone contents higher than 6 wt% (the standardized content) could be achieved in the elution step using ethyl acetate. 相似文献
95.
96.
The viscosity of PEG-modified urethane acrylate (PMUA) showed peculiar behavior in the course of soap-free emulsification. Moreover, the viscosity change with added amounts of water was influenced by the reaction molar ratio of polyethylene glycol (PEG). The rate of increase in viscosity slowed and the ratio of increase in viscosity increased as the reaction molar ratio of PEG increased. This peculiar viscosity behavior was due to the microphase separation between hydrophilic and hydrophobic segments of PMUA, and the orientation of polyoxyethylene groups at O/W interface which influenced droplet size of the soap-free PMUA emulsion. The location of polyoxyethylene groups of this resin at O/W interface was confirmed using the adsorption isotherm measurement of PMUA molecules containing polyoxyethylene groups at water/benzene interface. The microphase separation behavior of PMUA between hydrophilic and hydrophobic segments could apply to the preparation of the PMUA gels containing peculiar structure. PMUA gels were prepared using dioxane (UAG) and the swelling behavior of these gels were compared to that of gels prepared using water (UAHG) in the same medium. In the same medium, the swelling behavior of UAHG gels differed from that of UAG gels because of the difference in the microstructure of gel due to the microphase separation between hydrophilic and hydrophobic segments. This phase separation in the course of gelation in water could be confirmed using contact angle measurement. 相似文献
97.
以交联聚乙烯醇为载体的离子交换剂对蛋白质的分离性能 总被引:2,自引:0,他引:2
本文对阴离子交换剂DEA—PVT常压液相离子交换色谱分离蛋白质的性能、分离条件进行了探讨。结果表明其对蛋白质的分离性能良好,容易洗脱。与载体交联聚乙烯醇相比,DEA—PVT对蛋白质的非特异性吸附明显降低。 相似文献
98.
The boxes contained kiwifruits were irradiated with cobalt-60 γ-rays at different dosages (0.6 , 1.8 and 3.6 KGy) and stored in a room ventilated at night, the natural ambient air being used as cool source.The results showed that the treatment which fruits irradiated with 0.6 KGy was the best after 85 days. It gave the normal-fruit rate of 95.10%, fruit flesh hardness of 4.10 Kg · cm-2, fresh and plump fruits, good quality and less Vc loss. 相似文献
99.
A polyaluminum chloride (PAC) sample was prepared using a slow alkaline titration method. The Bio-Gel P-100 gel column chromatographic
technique was used to separate and characterize the various forms of aluminum present in the prepared PAC solution. The effluents
from a gel column were monitored using online chemical method: Al-Ferron timed complexation spectrophotometry and by 27Al nuclear magnetic resonance (NMR) spectroscopy. Effects of different experimental conditions such as eluent flow rate, ionic
strength and pH on separation of Al13 were investigated. Experimental results indicated that molecule size exclusion was not the only parameter affecting the column
chromatographic separation efficiency of Al13 but molecule charge as well. Reducing the eluent flow rate, increasing the ionic strength and suitable pH resulted in increase
in the separation efficiency. Experimental results clearly indicated that by varying the experimental conditions, it is possible
to produce pure Al13 species using a gel column chromatographic technique. 相似文献
100.
Lukin O Müller WM Müller U Kaufmann A Schmidt C Leszczynski J Vögtle F 《Chemistry (Weinheim an der Bergstrasse, Germany)》2003,9(15):3507-3517
The readily available in gram quantities tris(allyloxy)knot of the amide-type 5 (knotane) can be completely and partially deprotected with nBu(3)SnH in the presence of a palladium catalyst resulting in hydroxyknotanes 7-9. These, in turn, react with diethylchlorophosphate giving rise to knotanes equipped with between one and three phosphoryl groups. Sulfonylation of bis(allyloxy)monohydroxyknotane 8 with p-toluenesulfonyl chloride and, following removal of one or two allyl groups from the intermediate monosulfonate 13, give rise to sulfonyloxy-allyloxy-hydroxy- and sulfonyloxy-dihydroxy-knotanes 15 and 14, respectively. This provides a convenient method for the preparation of knotanes with any substitution pattern. All new knotanes have been isolated in preparative amounts and as highly pure substances with an exception of allyloxy-dihydroxyknotane 9. This compound could only be obtained as a mixture with the corresponding monohydroxy-derivative 8. The structures of all synthesized compounds were established by means of FAB and MALDI TOF mass spectrometry, (1)H and (31)P NMR spectroscopy. The triphosphorylated knotane 10 exhibits high solubility in alcohols, allowing its complete enantiomeric resolution with a commercially available chiral HPLC column. (1)H,(1)H DQF-COSY correlation spectroscopy along with H/D exchange experiments and ab initio calculations provided the first detailed (1)H NMR signal assignments of knotanes in [D(6)]DMSO solution. The combination of variable temperature (1)H and (31)P NMR spectroscopy and molecular modeling has been applied to study the conformational behavior of the new knotanes in different solvents. It has been shown that in DMSO solution at room temperature knotanes exist in a relatively rigid nonsymmetrical conformation similar to that found in the solid state while faster conformational exchange leading to the average D(3) symmetrical structure was detected in a number of other solvents. 相似文献