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  • Column liquid chromatography  (124)
  • Springer  (124)
  • Cambridge University Press
  • Frontiers Media
  • 2020-2022
  • 1985-1989  (124)
  • 1980-1984
  • 1975-1979
  • 1970-1974
  • 1988  (90)
  • 1985  (34)
  • 1970
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  • 2020-2022
  • 1985-1989  (124)
  • 1980-1984
  • 1975-1979
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  • 101
    ISSN: 1612-1112
    Schlagwort(e): Hydrolysis, high temperature ; Column liquid chromatography ; Ion-exchange ; Cellulose ; Oligomeric and monomeric sugars
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The hydrolysis of different cotton materials under hydrothermal conditions was investigated. For the analysis of the resulting reaction products high-performance liquid chromatography and gel-permeation chromatography were applied. HPLC columns with ion exchange materials as stationary phases (HPX 87P and Shodex S801) enabled the separation of monomeric sugars and degradation products. Oligomeric sugars were analyzed using a gel column (Bio-Gel P-2) as well as a HPLC column (HPX 42A). Through identification of additional reaction products the mass balance of the hydrolysis can be improved and the analysis of the distribution of the oligomeric sugars gives information for the selection of the reaction conditions.
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  • 102
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Analgesic peptides ; Opioids ; Glycopeptides ; Glycosylenkephalins
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary N 1.5-Glycosyl enkephalins are potent analgesics. Two enkephalin-related glycosyl peptides: [DMet2, Pro5] enkephalin (N 1.5 β-glucopyranosyl] amide and [DMet2, Pro5] enkephalin [N 1.5 β-galactosyl] amide have been prepared following the liquid phase procedure. The chromatographic behavior of both the final glycosyl enkephalins and their synthetic intermediates on reversed-phase columns has been tested. Semipreparative, reversed-phase, HPLC conditions have been developed in order to obtain a simple and rapid procedure for the purification of the two synthetic pentapeptides. Thus, using isocratic elution, injections of 10mg of crude material after gel filtration gave homogeneous (99.9%) glycosyl enkephalins.
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  • 103
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Acrylic acid ; Polyacrylic gelling agents ; Superabsorbent polymers
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary High-performance liquid chromatographic methods (reversed-phase and ion exclusion) for the determination of monomeric acrylic acid in polyacrylic gelling agents are described. Acrylic acid is extracted by two different methods. The methods were applied to samples containing acrylic acid from 1–1000 mg/kg.
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  • 104
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 919-922 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Nifedipine ; Normal phase ; Plasma ; Liquid-liquid extraction
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary For the determination of nifedipine in plasma a sensitive and selective method is required. The use of ‘on-line’ pre-column enrichment, followed by ‘reversed phase’ separation and UV-detection at 350 nm proved to be too susceptible. Therefore, detection was carried out after a post-column ‘on-line’ reduction and photoreaction step using a fluorescence detector. Although this method proved to be extremely sensitive (limit of detection 0.1 ng/ml plasma) and selective, a number of problems cropped up caused by the reduction agent which finally prevented the procedure being used in routine analysis. As a consequence, the following method was developed. After liquid-liquid extraction of nifedipine a 1/3 of the extract was chromatographed on a normal phase (diOH) system and detected at 235 nm, because detection at 350 nm was not sensitive enough. This method has a limit of detection of 1 ng nifedipine/ml plasma and the calibration curve is linear up to 320 ng/ml. The recovery lies around 82% and the standard deviation for the range 6–320 ng/ml is less than 5%. So far about 2000 plasma samples have been analysed by this method.
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  • 105
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 957-960 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Electrochemical Detection ; Ethinyloestradiol
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The analysis of ethinyloestradiol in tablets has been carried out by reversed phase high performance liquid chromatography (HPLC) using electrochemical detection. The drug was eluted with aqueous acetonitrile containing sodium acetate as background electrolyte. The mobile phase was used as extracting solvent, and 4-tertpentylphenol was used as internal standard.
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  • 106
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 969-973 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Carboxylic acid phase ; Addition reactions ; Synthesis of new bonded phases
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The allyl bonded phase is used as an intermediate in the synthesis of a weak cation exchange material. The double bond is first converted to an aldehyde by an ozonation reaction and then subsequent oxidation to the carboxylate group is accomplished with dichromate. Diffuse reflectance Fourier transform infrared spectroscopy (DRIFT) is used to monitor the conversion process. The presence of the aldehyde functional group is confirmed by reaction with 2,4-dinitrophenylhydrazine. ESCA spectra reveal no residual chromium on the silica surface. The product is tested chromatographically by the retention of alkylarylketones, the ion-exchange behavior of both monovalent and divalent cations, the retention of nucleosides and bases, and the separation of a mixture of hemoglobins.
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  • 107
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; UV detection ; Solubility ; Polystyrene ; Sample precipitation ; Gradient elution
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Gradient elution of polystyrene standards on reversed phase C18 columns by methanol/tetrahydrofuran or methanol/dichloromethane mixtures yielded a strange effect of the molecular weight of the sample on the specific peak are (mAUs per μg sample injected). The effect did not occur when pure dichloromethane was used as an eluent. Further to this, dependence of specific peak area on flow rate was observed in gradient elution with methanol/tetrahydrofuran mixtures. It was found that these effects were due to polymer elution at the verge of precipitation. Depending on the dwell time of the sample in the column, opalescence occurred that added to the UV signal used for monitoring the elution.
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  • 108
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Reversed-phase ; Ion-pair ; Red blood cells ; Tumour cells
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The determination of nucleotides, nucleosides, and nucleobases was carried out in cells of different metabolic complexity: in mature and immature red blood cells, in Ehrlich ascites tumour cells from different proliferation stages, and in other tumour cells. The maturation of reticulocytes to erythrocytes is accompanied by loss of organelles and energy-requiring processes as well as the switch from aerobic to anaerobic ATP production. The profile of purine nucleotides, nucleosides, bases, and pyridine dinucleotides, by reversed-phae HPLC, shows large concentration changes during the maturation of red blood cells. The concentrations of purine mono and triphosphates are two to four times greater in reticulocytes in comparison with erythrocytes; the difference in the concentrations of nucleosides and nucleobases between reticulocytes and erythrocytes is even greater. Application of ion-pair HPLC showed that the Ehrlich ascites cells loose major portions of purine mono-, diand triphosphates between the 7th and 11th day after inoculation. Fast growing solid sarcoma tumours of rats (MV 202 Ner) contain higher amounts of nucleotides than slowly growing tumours of identical cell type.
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  • 109
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 20 (1985), S. 96-98 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Phthalic anhydride ; Naphthoquinones
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A simple method of analysis of the 1,2 and 1,4 isomers of naphthoquinone in crude phthalic anhydride has been developed. The sample was first dissolved in water at 60°C to quantitatively hydrolyse the anhydride to phthalic acid. Analysis of the aqueous solution by reversed-phase HPLC using 75∶25 methanol:water mobile phase resulted in excellent resolution between the phthalic acid and the naphthoquinones and enabled quantitative measurement of each of the naphthoquinones to 0.1 % in crude phthalic anhydride.
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  • 110
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Micro enzyme-immobilized columns ; Separation of aldehydes ; Derivatization and fluorometric detection
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Aldehydes in liquors were analyzed by micro high-performance liquid chromatography with post-column derivatization on the enzyme-immobilized glass beads. β-nicotinamide adenine dinucleotide (NAD) was converted to its reduced form (NADH) on the enzyme-immobilized column in the presence of an aldehyde and a thiol, followed by fluorometric detection. A detection limit of 2.5 ppm (50 pg) was achieved for acetaldehyde.
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  • 111
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 526-530 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Doxycycline and Demeclocycline ; Plasma and urine samples ; Solid phase extraction
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A method for the selective quantification of doxycycline in human plasma and urine has been developed using HPLC with UV-detection at 350 nm. Analyte and internal standard were extracted from plasma by extraction columns filled with octadecylsilica. Urines were only mixed with diluted acid prio to injection. The influence of pH on peak shapes is discussed as well as comparative investigations on selectivity and peak symmetry on commerical octadecylsilica. The method was successfully applied to the samples of a clinical study with an oral single dose of 100 mg. Precision and accuracydata of the assay and calculated pharmacokinetic parameters are presented.
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  • 112
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Microcolumn ion chromatography ; Indirect photometric detection ; Monovalent cations
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Monovalent cations were indirectly detected via postcolumn suppressor ion replacement in microcolumn ion chromatography. The ion-repalcement column loaded by chromophoric ions was connected to the suppressor column. The eluent, nitric acid, was converted to water through the suppressor and anion-replacement columns, while the analyte cations were coeluted with the chromophoric anions. The analyte cations were indirectly detected by measuring UV absorptions of the chromophoric anions.
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  • 113
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 593-597 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Solid phase extraction ; Amiodarone in serum ; Addition of ammonia to eluent
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An improved liquid-solid extraction procedure for the purification and determination of amiodarone and desethylamiodarone in biological fluids is proposed. The sample is passed through a silica-C18 column, and after washing, the analytes are eluted with methanol. The determination is then accomplished by RP HPLC using an octadecyl silica column and a mobile phase of methanol containing 0.0015% of ammonium hydroxide. The effect of ammonia concentration on the capacity factors of the analytes has been used for estimating the acid dissociation constants of the investigated secondary and tertiary amines in methanol.
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  • 114
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Indirect photometric detection ; Signal intensity evaluation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary We have experimentally evaluated the equation representing the peak area of induced peaks in indirect photometric detection of nonelectrolytes as a function of the amount and concentration of the analyte and the visualizing agent and their capacity factor, the phase ratio of the column and the absorptivity and the pathlength of detection. Aliphatic alcohols and hydrocarbons were used as the test analytes. Most of the analytes behaved according to the relationship expressed by the equation.
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  • 115
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 685-690 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Adsorption on solid support ; Polar solutes
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The properties of chloroform as a liquid stationary phase in reversed-phase liquid chromatography have been investigated. Stable systems and complete pore filling of the support were obtained. Uncharged acids were slightly adsorbed by the support. Amines in the cationic form showed tailing, which can be attributed to adsorption on the support material. The influence of several reversed-phase supports on retention and peak symmetry has been studied. Little difference was found for uncharged acids, but retention and peak shape of the cations was dependent on the specific support. Also on the poly(styrene-divinylbenzene) copolymer PRP-1 cations gave tailing peaks. The results indicate that the surface of reversed-phase supports is heterogeneous. From this and other studies it can be concluded that only certain reversed-phase silicas, such as μ-Bondapak, are suitable supports for cationic solutes. In liquid-liquid chromatography polar solutes only obey a liquid-liquid distribution model if the liquid stationary phase molecules contains a hydrophobic group, as well as a polar function.
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  • 116
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Ligand exchange ; On-Line preconcentration ; Opiate pentapeptide
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary In order to study the occurrence of the opiate pentapeptide β-[D-Ala2,4, Tyr5] CM-5-NH2 in the 10−9–10−5 M concentration range, we have developed a new method consisting of extraction of the peptide from its buffered aqueous medium onto a reversed phase cartridge of 50 μL void volume, followed by on-line injection onto a Cu(II) modified silica gel column. The acetonitrile-rich mobile phase allows detection of the natural fluorescence of the peptide at the picomole level.
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  • 117
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Expert systems ; Optimization of operating parameters
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Given the mobile and the stationary phase and values for the physical parameters such as temperature and pH, a separation can be optimized by varying the so-calledchromatographic parameters. These include the column dimensions, particle size, operating conditions (e.g. flow rate, attenuation) and instrumentation (e.g. detector cell, time constant). Optimization of the chromatographic parameters implies finding the best possible set of values, which we define as yielding (i) sufficient separation and (ii) sufficient sensitivity in (iii) the shortest possible time. Finding the best possible conditions (the global optimum) is very difficult for chromatographers in practice. An expert system is described that allows chromatographic optimization to be performed for isocratic separations. An initial chromatogram is required to consult the system. In return, the system provides a complete set of chromatographic parameters, which represents the global optimum within the limits set by the required resolution and signal-to-noise ratio specified by the user. The tolerated flow and pressure ranges, the volume of the available detector cells and the time constant of the detection system are constraints during the optimization. A separate module of the system concerns the sample preparation for pharmaceutical formulations in solid dosages and aqueous solutions. Prototype expert systems have been successfully implemented in the expert-system shell Knowledge Craft on a MicroVAX workstation.
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  • 118
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Expert systems ; Selectivity optimization ; Optimization criteria
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Systematic procedures for the optimization of chromatographic selectivity require objective criteria to characterize the quality of separation in a chromatogram. Numerous criteria have been suggested. Different criteria yield different results and the choice will depend on a large number of factors. It is genuinely difficult to select the most suitable criterion in a particular situation. For these reasons, an expert system has been developed to assist chromatographers in the selection of optimization criteria. A structured representation of the required knowledge and its implementation in an expert-system shell are presented in this paper.
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  • 119
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 26 (1988), S. 300-304 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Column liquid chromatography ; Polycyclic aromatic hydrocarbons ; Phenolic compounds ; Air pollution
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An improved procedure for the determination of the less volatile air pollutants of recycled closed atmospheres by activated carbon-Soxhlet extraction is proposed. After total treatment of desorbate, PAH determination is then accomplished by RP-HPLC using both adsorptiometric and fluorimetric UV detection; phenolic compounds are determined by GC-MS. This technique is suitable for very low levels of PAH and phenolic compounds.
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  • 120
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Isotachophoresis ; Sample pretreatment
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary This study focusses attention on the possibilities of preparative isotachophoresis (ITP) as a sample pretreatment technique prior to liquid chromatographic (HPLC) analysis. The increased demand for accurate and less time consuming analysis necessitates that sample pretreatment procedures, should be develop in parallel with other improvements (e. g. in detection and separation) which can be observed. The preparation isotachophoresis was performed on gel slabs and the zones of interest were subsequently cut out, desorbed and the desorbates analyzed by HPLC. In this study satisfactory recoveries of between 85–90% with a standard deviation of 1–5% were observed for blank experiments. For spiked serum and urine samples the recoveries in general decreased with decreasing spiked drug concentrations. These observations are discussed in this paper.
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  • 121
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 26 (1988), S. 363-368 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Electrochemical detection ; β-Naphthoquinone sulfonate ; Labelling reagent ; Direct labelling in body fluids
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A new sensitive, high-performance liquid chromatography (HPLC) method using electrochemical detection (ECD) is reported for the determination of 21 amphetamine-like compounds such as amphetamine, methamphetamine, methoxyphenamine, phentermine, ephedrine, mescaline, STP and methylenedioxyamphetamine, in biological fluids. Primary and secondary amines in biological specimens were easily labelled with β-naphtho-quinone-4-sulfonate (BNQS) at 60°C for 30 min. Hydrodynamic voltamograms of BNQ-derivatives showed a maximum response at an applied potential of around zero V (against Ag/AgCl) in reducing model. BNQ derivatives of amines were analyzed by HPLC using a reducing ECD at zero V (Ag/AgCl). Separation was on a μ Bondasphere C18 with mobile phase: acetonitrile-methanol-0.01 M H2SO4. Good separations of twenty one amphetamine-analogs were obtained. Only 50 μl of biological fluid containing those drugs at a concentration of over 1 μg ml−1 were needed direct for determination with good accuracy. When extraction was carried out prior to the labelling reaction, the detection limits were much improved to less than 10 ng ml−1. This method was successfully applied to determination of methamphetamine in hair.
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  • 122
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 26 (1988), S. 13-18 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Hydrophobic interaction chromatography ; Proteins ; Salt effects ; Effect of MgCl2
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary It has been noted in the literature that certain salts enter into specific interaction with proteins. As a result of this, they may act as salting-in agents. We have investigated the effect of magnesium chloride which is known to possess such unusual properties on the retention of proteins in hydrophobic-interaction chromatography. First the retention behaviour of amino acids and small peptides having a wide polarity range was studied on reversed-phase columns using eluents containing (NH4)2SO4, MgSO4 or MgCl2, in wide the concentration ranges. For less polar eluites plots of the logarithmic retention factors against the salt concentration were found to be linear, whereas the more polar species showed irregular behavior. The retention of a wide range of proteins was measured on a TSK Phenyl-5-PW column using eluents containing (NH4)2SO4, MgSO4 or MgCl2 at different concentrations. The salt-mediated retention was regular with (NH4)2 SO4 and MgSO4 although MgSO4 showed a lesser effect than that predicted by the surface-tension increment. The effect of MgCl2 was quite irregular: the retention factors either increased or decreased or remained unchanged depending on the protein. These results corroborate earlier observations regarding the particular effect of MgCl2 and suggest the modulation of selectivity in hyrophobic-interaction chromatography by the addition of MgCl2 to the eluent.
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  • 123
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 26 (1988), S. 417-422 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Oligomeric series ; Separation selectivity ; Oligoethylene glycols ; Ethoxylated nonylphenols
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The simultaneous dependence of the retention in oligomeric series on the number of repeat structural units and on the mobile phase composition may be described by very similar equations for reversed-phase and for normal-phase systems. In reversed-phase systems, the separation selectivity of the individual oligomers is determined mainly by the size and by the polarity of the repeat structural unit, but the influence of a bulky and polar structural residue may also become important so that even reversed order of elution may be observed for oligomeric series with the same oligomeric units but significantly different end groups. For example, oligoethylene glycols are eluted in the order of increasing size of the oligomers, whereas ethoxylated nonylphenols are eluted in the order of decreasing size. In normal-phase systems, the separation selectivity in oligomeric series depends on the adsorption energy and on the adsorbed area of the oligomeric unit. If the oligomeric unit is small, the concentration of the polar solvent in the binary organic mobile phase has only a minor effect on retention and selectivity, which may be controlled by taking account of the nature of the adsorbent and of the polar solvent or by varying the proportion of two polar solvents in a ternary mobile phase.
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  • 124
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 26 (1988), S. 19-28 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Chiral LC and SFC phases ; Polymer coating ; Chemical bonding ; Polysiloxane pre-polymers
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Chirally substituted Si−H-containing polysiloxanes were synthesized, which can be immobilized on small particle silica gel as well as on the smooth surfaces of fused silica capillaries. Immobilization is achieved either by crosslinking or by chemical bonding to the surfaces via silanol groups; both reactions can only be performed by addition of H2PtCl6, which acts as catalyst for hydrosilylation and as stoichiometric reagent for crosslinking. Chiral substituents of systematically varied chemical structure were introduced into the polysiloxanes by hydrosilylation. The mechanism of immobilization was investigated by spectroscopic methods, notably29Si-NMR. Homogenous stationary-phase coatings of variable film thickness and corresponding retentivity can easily be achieved. The enantioselectivity of the phase systems was characterized in dependency on the chemical structure of the chiral selectors attached to the polysiloxane chain of the chiral stationary phases and also in terms of the functional groups introduced into the solutes by derivatisation.
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