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  • 1
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Enantiomer separation ; Chiral ovomucoid column ; Diltiazem hydrochloride ; Clentiazem maleate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A direct HPLC separation method was developed for the determination of the enantiomers of racemic precursors to diltiazem (I) and its 8-chloro derivatives (II). The enantiomers were successfully separated on a chiral ovomucoid column using an aqueous-organic mobile phase (reversed-phase HPLC). The influence of the organic modifier and buffer pH on the retention and enantioselectivity was investigated. The chromatographic conditions chosen for the separation permitted complete resolution of the enantiomers of both the acid (Ib and IIb) and methyl ester precursors (Ia and IIa) within 20 min. The influence of sample load on retention times, theoretical plates numbers, peak heights and peak areas was also investigated. The peak areas showed a good linearity over the concentration range examined, although all the others were influenced significantly by the sample size. An optical antipode of the intermediate to be determined could be detected by the area-percentage method down to ca. 0.1%, together with the determination of its precursor, including its optical purity.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 178 (1977), S. 3191-3195 
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Optimized syntheses of 1,3,6,9-tetraoxacycloundecane (2), 1,3,6,9,12-pentaoxacylotetradecane (3), and 1,3,6,9,12,14,17,20-octaoxacyclodocosane (4) as well as some physical and chemical properties and the proof of structure are reported.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 25 (1987), S. 2281-2288 
    ISSN: 0887-624X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ethynylated polystyrene resins were prepared as functionalized polymer supports by the iodination reaction of macroporous polystyrene resins and reacted with transition metal diethynyl complex (Mt = Ni) and metal halides (Mt = Rh, Pd, and Pt) in a basic solvent using cuprous iodide as a catalyst to obtain macroporous polystyrene resins containing organotransition metals. The distribution of the metal acetylide complexes in the modified macroporous resins was determined by an electron probe microanalyzer. A gradient in the transition metal distribution was observed in any case of the modified resins. The stability of the organotransition metal complexes in the polymer matrix could be compared with a low molecular weight analogous complex quantitatively.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Enantiomer separation ; Denopamine ; Derivatization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A reversed-phase high-performance liquid chromatographic (HPLC) method was developed to determine the optical purity of denopamine, which is a new cardiotonic agent having an asymmetric carbon in a molecule. The enantiomers were converted to diastereomeric thiourea derivatives using 2,3,4,6-Tetra-O-acetyl-β-D-glucopyranosyl isothiocyanate (GITC) reagent. Separation of the enantiomers of denopamine as diastereomers was successfully achieved by reversed-phase HPLC within 10 min using an ODS column and UV detection. Derivatization of denopamine proceeded rapidly under the alkaline conditions and the ambient temperature. This method was applied to the determination of the optical purity of denopamine drug substances and those in tablets. The favorable UV absorption of the derivatives enabled the optical antipode to be determined down to the 0.2% level.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Applied Polymer Science 45 (1992), S. 1463-1472 
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: The spherical tannin resin (STR) resulting from the reaction between Mimosa (Acacia Mollissima) tannin (condensed-type tannin) and formaldehyde was very porous. The specific surface area of the STR made from 37.5% of tannin was 139.2 m2/g (1 g of the resin in this is wet resin corresponding to 1 g of dried resin). Properties such as specific surface area and average pore radius could be controlled by adjusting the tannin concentration. The apparent activation energy of Cu2+ ion adsorption by STR was 3 kcal/mol, and that of Cr6+ ion was 2 kcal/mol. Since the energy was small, we concluded that the adsorption of metal ions was not influenced significantly by the adsorption temperature. The heat of adsorption for Cu2+ ions was only 1.6 kcal/mol, which suggests that the adsorption was a physical phenomenon. It was thought that the diffusion of heavy-metal ions into the porous resin was the rate-determining step of the adsorption since the elution profile of the column method was analogous to the profile of active carbon, which adsorbs physically, the heavy metal ions gradually leaking through the column. The surface and cross section of the STR were observed before and after Cu2+ ion adsorption with the scanning electron microscope. The pores of the spherical resin were clogged with adsorbed copper, suggesting that the Cu2+ ions were adsorbed during the formation of a multimolecular layer. The adsorption may therefore have been due to physical attractive forces. The rate of adsorption and adsorption isotherms of Cu2+ ions from copper salts having various anions was found to vary depending on the type of anion. These phenomena were not thought to be due to the properties of the spherical resin but to differences in the hydration state of copper ions.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
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