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  • Column liquid chromatography  (54)
  • ASTROPHYSICS
  • Data analysis / ~ processing
  • Industrial Chemistry
  • Inorganic Chemistry
  • NOISE
  • Seismology
  • ddc:330
  • Springer  (55)
  • DGG  (1)
  • 1985-1989  (56)
  • 1950-1954
  • 1987  (56)
  • 1
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    Springer
    Chromatographia 23 (1987), S. 796-802 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Steroids ; Rat tissue ; Purification by extraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A high-performance liquid chromatographic method for analysis of steroids in the tissue of laboratory animals is described. A two-stage solid extraction procedure, utilizing Sep-pak C18 and graphitized carbon black, gives a purified product. Steroids in this extract were separated by multistep gradient elution with a reversedphase liquid chromatography system, using acetonitrilewater as solvent. Several columns with different geometry and phase loading were investigated. Optimum resolution was obtained with a medium covered and spherical particle. The applicability of this method was successfully demonstrated in the analysis of the testis and adrenal gland of rat.
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  • 2
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    Chromatographia 23 (1987), S. 814-817 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thin layer chromatography ; Ammonium tungstophosphate ; Aminoacids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The chromatographic behaviour of aminoacids on columns of silica coated with different percentages of ammonium tungstophosphate at several buffer phosphate concentrations is reported. The stationary phase shows a high selectivity towards aminobutyric acids and methyl derivatives of tryptophan due to the distance between the carboxylic group and the −NH 3 + group involved in the cation-exchange process and/or to the steric hindrance by a methyl substituent. A relationship between HPLC and HPTLC data has been verified and applied to the prediction of the separation of six aminoacids.
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  • 3
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    Chromatographia 23 (1987), S. 934-938 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Calibration ; Confidence interval ; Limit of determination ; Limit of calibration
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In HPLC calibration the expressions lowest calibration limit and determination limit are defined in statistical terms. The lowest calibration limit is the minimum mass in the measured series of calibration points. It is calculated from the confidence interval of the inverse of the calibration function as the lowest mass limit that may be differentiated from zero mass with a preset probability of error. If the calculated lowest calibration limit is lower than the actual data, points at lower concentration may be measured. The determination limit is the smallest concentration of an analysis that is differentiated from the concentration zero or an apparent blind value in the calibration curve with a given probability of error. Using two different UV-detectors (variable wavelength and photodiode-array) the lowest calibration limit is experimentally evaluated and compared with specific data for the detectors.
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  • 4
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Pre-column derivatization ; Ultraviolet detector sensitivity ; Dihydroartemisinin ; Diacetyldihydrofluorescein
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of diacetyldihydrofluorescein (DADF) for derivatization of dihydroartemisinin (dihydroqinghaosu, DHQHS) is proposed. The reaction between DHQHS and this reagent in the presence of 4-dimethylaminopyridine (DMAP) and N,N′-dicyclohexylcarbodiimide (DCC) was complete in 8 hours at room temperature giving about 80 per cent theoretical yield. The derivative showed intense UV absorption, thus providing a sensitivity of 0.1 nanogram by UV detection after column separation. The influences of the ratio of the reagents, reaction temperature, chromatographic conditions and the extent of detection linearity were investigated. The reaction gave consistent results and chromatographic separation was not affected by an excess of the reagent or side products.
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  • 5
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    Chromatographia 23 (1987), S. 395-400 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Photokinetic data ; Reaction mechanism ; (E)-1-phenylpropene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A combined method of high-performance liquid chromatography and UV-absorption spectroscopy is described for use in dynamic systems. It provides a way of obtaining detailed mechanistic information as well as quantitative data (rate constants, quantum yields), even though neither mechanism nor photoproducts are known. The kinetic treatment of the photoreaction of (E)-1-phenylpropene was successful, showing a photo-isomerization and a parallel step. Information on this additional step is obtained by using HPLC to observe the changes in the concentrations of the reactants' selectivity. The necessity of process control is demonstrated.
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  • 6
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    Chromatographia 23 (1987), S. 419-422 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fatty acid esters ; Particulate material in seawater
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method for the determination of fatty acids of the molecular weight range of propionic to erucic acid is reported. The acids are converted to either p-bromophenacyl-or p-phenylphenacylesters and the esters are separated by HPLC and detected by UV-absorption. Twentytwo esters, including saturated, monoolefinic and polyunsaturated ones were separated within one HPLC-run. The detection limit is about 5 pmol per fatty acid. The application of the method to particulate material is described.
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  • 7
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Anion-exchange stationary phases ; Polymer coating ; Cross-linking
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary PHEB=POLY(2-hydroxy, 3N-ethylenediamino)butadiene has been synthesized. This unsaturated pre-polymer can be immobilized on different, preferably inorganic supports of suitable porosity such as silica or alumina by cross-linking. Weak anion-exchange phase are obtained. Such phases do not have the disadvantages of organic polymeric phases, regarding pressure stability and swelling by solvent influence. The ion-exchange capacity and the retentivity of IE-separations can deliberately be varied via the thickness of the cross-linked polymer layer. Alumina can also be coated with PHEB applying the same cross-linking procedure. Such phases exhibit an exceptional chemical stability even when operated with mobile phases at very high pH-values. Separations of excellent selectivity are achieved for inorganic anions, as well as with mixtures of aliphatic and aromatic free acids also including hydroxy- (mono- or poly)carboxylic acids.
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  • 8
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase systems ; Stationary phase-solute interactions ; Polycyclic aromatics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Capacity factors of peropyrene-type polycyclic aromatic hydrocarbons were measured using 15 different liquid chromatographic reversed phase systems. On the basis of the retention data the electric interaction indices have been calculated. Application of these indices for structure-retention studies on peropyrene-type polycyclic aromatic hydrocarbons is demonstrated.
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  • 9
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    Chromatographia 23 (1987), S. 31-32 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gonadal steroids ; Epimers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Chromatographic separation of biologically active epimeric steroids was carried out using a combination of normal and reversed phases. Testosterone (17β-OH) was separated from its 17α-OH epimer epitestosterone using a normal phase silica column whereas their reduced 5α-metabolites were separated on a reversed phase system. The separation of other gonadal steroids including the epimers 20α- and 20β-hydroxypregn-4-en-3-one is also discussed. The technique is particularly useful for separating mixtures of naturally occurring steroid epimers prior to radioimmunoassay.
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  • 10
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ammonium acetate buffer eluent ; Chlorophylls and degradation products ; Marine phytoplankton
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An RP-HPLC procedure which separates chlorophylls and their degradation products is described. By employing an amonium acetate buffered mobile phase and a linear gradient elution, complex mixtures of chloroand phaeopigments are separated in less than 30 minutes. The method has been applied to the control of chlorophyll enzymatic degradation in cultures of two algal species, and has also been successfully used in the analysis of algal xanthophylls.
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  • 11
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Behaviour of metal complexes ; Solvophobic theory
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The chromatographic behaviour of Cu(II), Fe(II), Ni(II) and Co(II) complexes with 4-(2-pyridylazo)resorcinol was studied. The experimental results were very sensitive even to less obvious operational parameters like the kind of the cation (sodium or ammonium) of the phosphate salt used as buffer. The puzzling pattern of the data obtained was interpreted in terms of the equations formulated by Horvath's ‘olvophobic” theory which correlates the capacity factors of the solutes with the surface tension of the mobile phase. A satisfactory rationalization of the data was obtained together with qualitative information on the stoichiometry and charge state of metal complexes. Useful suggestions about the direction to address the experimental work in order to obtain the best results was also obtained.
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  • 12
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ligand Exchange ; Diethylenetriaminepentaacetic acid ; Transition metal ion separation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Basic alumina-bonded diethylenetriaminepentaacetic acid (DTPA) has been utilized for the separation and preconcentration of some transition metal ions on the basis of ligand exchange. Breakthrough capacity and rate of sorption have been studied. The distribution coefficients of 16 transition metal ions have been determined in demineralized water, 0.01 M sodium citrate and in four different pH systems. On the basis of differences in Kd values some quantitative separations of metal ions have been achieved. The greater selectivity behaviour (higher Kd values) of the adsorbent for Pt(IV)and Cr(III) has been utilized for their preconcentration in the presence of other metal ions. The method has been employed for the recovery of Pt(IV) and Cr(III) from tapwater and sea-water samples.
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  • 13
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gel permeation chromatography ; Cheese peptides ; Amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The nitrogen fraction from cheese, soluble in phosphotungstic acid has been analyzed by gel permeation and high performance liquid chromatography. Elution profiles of this fraction on Sephadex G-10 show that there are no peptides of molecular weight higher than 700 daltons. Six fractions have been obtained. The first one has the peptides and some amino acids. Fractions II to VI contains mostly free amino acids. Fraction I has been separated into many peaks by HPLC. Six or seven of these peaks are presumed to correspond to peptides.
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  • 14
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Small-bore packed columns ; Air pollutants ; PAH, nitro and oxy-PAH ; Aldehydes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of small bore columns (1 mm i.d.) packed with reversed-phase materials is described. High efficiency (Hmin=2 dp), coupled with a small C term (0.005 sec) have been obtained so that high speed can be combined with sufficient resolution for the separation of complex organic mixtures. These columns have been used for the separation of air pollutants dispersed in different matrices (air, particulate matter and rain water). Practical applications include the determination of aldehydes in air and emission samples, PAHs, nitrated and oxygenated PAHs in dust sampled from the stack of an industrial emission or collected in a urban area and the analysis of organic components dissolved in rain water collected at a rural site. Specific detection of these pollutants has been achieved by connecting small bore columns to UV absorbance, voltammetric and fluorimetric detectors. Mass spectra of some specific components have been recorded using the off-line technique.
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  • 15
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    Chromatographia 23 (1987), S. 825-828 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gasoline ; Single-ring aromatic hydrocarbons ; Polycyclic aromatic hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This work reports a rapid and easy procedure for the analysis of the aromatic fraction in gasoline. No sample pretreatment is required, since the gasoline is diluted in methanol and directly injected into a liquid chromatograph. A spectrophotometer detector and a spectrofluorimeter detector are used in series. The procedure has been applied to a large number of Italian and European refined gasoline samples.
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  • 16
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    Chromatographia 23 (1987), S. 109-111 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Normal and reverse phase ; Aldicarb ; Aldicarb sulfoxide ; Aldicarb sulfone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Aldicarb, aldicarb sulfoxide, and aldicarb sulfone were chromatographed on an octyl-silica bonded-phase column and on an unmodified silica column using acetonitrile/water mobile phases. The elution order of the analytes from the silica column was different from that using the octyl-silica bonded phase and allowed confirmation of residues of aldicarb sulfoxide in citrus nectar. Isocratic elution of the unmodified silica column allowed rapid sample throughput.
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  • 17
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ligand-exchange chromatography ; Chiral bonded phase ; Racemate resolution ; Amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The resolution of racemates on chiral chemically bonded silica gel by high-performance ligand-exchange chromatography is described. The stationary phase was prepared by bonding (−) trans 1,2 cyclohexanediamine to silica gel through the coupling agent 3-glycidoxypropyl silane. The resolution of several α-amino acids and of compounds of pharmaceutical interest is reported.
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  • 18
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    Chromatographia 23 (1987), S. 320-324 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Microbore capillary columns ; Polymer based octadecylsilica bonded phase ; Fat soluble vitamins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Separation behavior of fat soluble vitamins on various chemically bonded materials in non-aqueous reversedphases microcolumn liquid chromatography has been investigated. The best performance was found on a polymer-based octadecyl bonded phase. Optimization of separation for vitamins D2, D3, E and E acetate has been tried using this polymer-based column and it has been found that a binary mobile phase consisting of acetonitrile and methanol gave complete separation of fat soluble vitamins.
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  • 19
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    Chromatographia 23 (1987), S. 331-336 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Microbore columns ; Injection techniques
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This paper focuses attention on the potentially larger signal-to-noise ratios produced by microbore columns in comparison with conventional columns. The increased chromatographic signals by the application of microbore columns are due to the lower chromatographic dilution of elution profiles which are proportional to the square of the column inner radius. Generally less than 1μl sample should be injected into microbore systems to obtain the full benefit of the column performance. However, since more sample can be loaded on conventional columns compared to microbore columns the advantage of improved signal-to-noise ratio can only be realised in situations where very little sample is available. To inject more than 1μl sample, at the same time avoiding extra band-broadening effects, suitable injection techniques must be available. In this study three injection methods for microbore systems that meet this condition, are studied and compared.
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  • 20
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Anion-exchange chromatography ; Xylenol orange ; Separation of nickel and zinc
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A liquid chromatographic procedure for separating nickel and zinc has been developed. Xylenol orange, which is one of the sensitive and commercially available color-forming agents, was used as a component of the mobile phase. The two ions could be separated on weak anion-exchange gels within 10 min. The procedure was suitable for the determination of nickel and zinc in relatively pure solutions with fairly high sensitivity. The described liquid chromatographic analysis would be also potentially applicable for any aqueous sample containing trace levels of metal cations at 1–10 ppm.
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  • 21
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Oligosaccharides ; Interference by salts ; Complex biological samples ; Enzymatic assays
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the determination of oligosaccharides in samples of high salt content by RP-HPLC with water as eluent and refractive index detection. The samples, mussel processing wastes which are used as media for microfungus and yeast cultures and hence for enzymatic assays (amilolitic capacity) of these microorganisms that develop within the wastes, have been treated with ethanol to precipitate the macromolecular organic matter and desalted by a modified mixed bed resin before chromatographic analysis is carried out.
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  • 22
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    Chromatographia 23 (1987), S. 579-582 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Backflush technique ; Coal-derived procucts ; Separation of phenolic compounds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid method was developed for the direct extraction of phenolic compounds from coal-derived products and subsequent isocratic HPLC analysis in a reversed-phase system by using the backflush technique.
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  • 23
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Non-porous gel ; Alkaline-earth cations ; Arsenazo III
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A liquid chromatographic procedure for separating alkaline-earth-metal cations with a non-porous gel column has been developed. Arsenazo III, which is one of the sensitive and commercially available color-forming agents, was used as a component of the mobile phase. Magnesium and calcium could be separated on the nonporous gel column within 55 seconds. The procedure was suitable for the separation of alkaline-earth-metal cations in relatively pure solutions with high sensitivity. Because of its rapidity the described procedure is also potentially applicable for any aqueous sample.
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  • 24
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Biphenols ; Dihydroxyphenylpropanes ; Voltammetric detection ; UV photometric detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention behaviour of mono- and dihydroxy derivatives of biphenol and bis(hydroxyphenyl)propanes was studied on chemically bonded C-18, CN-, phenyl, phenoxypropyl- and NH2 stationary phases and on silica gel. The effects of the mobile phase, i.e., of the methanol content, the ionic strength, pH and the contents of cationic and anionic ion-pairing agents on the retention data were investigated. In the reversed-phase systems, all the substances are satisfactorily separated except for 3- and 4-hydroxybiphenyl; these isomers can be separated on silica gel, using a mixture of heptane and propanol as the mobile phase. Sodium dodecylsulphate, present at concentrations higher than the critical micelle concentration (about 10−2 M, depending on the methanol content), causes a decrease in the retention times and an improvement in the separation. UV absorption spectra, calibration curves and the detection limit values were obtained at two wavelengths and at various salt concentrations in the mobile phase. Hydrodynamic voltammograms of the solutes were measured in a carbon fibre detector and the calibration curves and detection limit values were measured at the optimal voltage (+1.2 V/Ag/AgCl) as a function of the mobile phase composition. For most test substances voltammetric detection is two to three times more sensitive than UV detection. The combination of a UV and a voltammetric detector in series has been utilized to identify the products of microbial degradation of biphenyl.
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  • 25
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thin-layer chromatography ; Ion pairing system ; Log P prediction ; Group contributions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A group of 17 β-carbolines was studied in HPLC and TLC systems in order to predict their partition coefficients (log P values). On account of the basic or acid character of some of these compounds, an ion pairing system gave the best results. Both HPLC and TLC data were comparable for log P prediction but severe pH conditions required the use of TLC plates. Retention data are quantitatively related to lipophilicity (expressed as the Hansch constant) and polarity (as the inductive constant) of the solute molecule.
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  • 26
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chitosan-coated silica gel ; Nucleotides ; Amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new stationary phase was prepared by immobilizing the chitosan, a natural hydrophilic polymer, on microparticolate silica gel. The effect of the polarity, pH and ionic strength of the mobile phase has been studied in order to find optimal conditions for the separation of nucleotides and aminoacids. The influence of the properties of the mobile phase on the retention was examined, allowing to employ the chitosan-coated silica gel both to anion exchange and adsorption, depending on the pH and the polarity of the eluent used.
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  • 27
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase systems ; Phases-solute interactions ; Molecular polarizability
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Variations in the electrostatic interaction have been studied using polycyclic aromatic hydrocarbons as standard compounds and different reversed-phase HPLC systems. Various methanol-water and acetonitrile-water binary mixtures were applied as the mobile phase. The stationary phases investigated consist of octadecylsilica and arenyl-silica. Using polarizability, dipole moment and ionization potential values of the solutes and mobile phase components as molecular descriptors an electrostatic interaction model is proposed.
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  • 28
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    Chromatographia 23 (1987), S. 93-96 
    ISSN: 1612-1112
    Keywords: Paper chromatrography ; Column liquid chromatography ; Copper-impregnated zinc silicate ; Separation of amines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Papers impregnated with Cu(II) sorbed on zinc silicate have been used to study the ligand exchange chromatographic behavior of amines. RF values of 16 amines have been studied in 6 different systems. On the basis of differences in RF values various analytically important qualitative separations of amines on impregnated papers and quantitative separations on columns of copper(II) sorbed on zinc silicate have been achieved.
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  • 29
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Linear isotherms ; Octadecyl bonded silica ; Styrene divinylbenzene ; Frontal analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two reversed-phase LC systems were investigated by frontal analysis for the determination of linear chromatographic conditions, as defined according to the isotherm concept. The Partisil ODS-3 bonded silica and the PRP-1 polystyrene-divinylbenzene resin were used as stationary phases together withtrans-2-hexen-al as test solute and methanol-water mixtures as mobile phases. Particular attention was paid to the respective influence of the two main parameters which may cause sorbent overloading, that is, the capacity factor (k′) and the solute concentration in the mobile phase (Cm). Provided that k′Cm≤10−2 M, linear chromatographic behaviour was observed for both sorbents, the maximum capacities of which were found greater than 1mmolg−1.
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  • 30
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    Chromatographia 23 (1987), S. 189-194 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Instrument bandbroadening by extrapolation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Methods to determine the contribution of the chromatographic equipment to the total band broadening which involve replacing the column by a union or a capillary tube are not suitable as they involve a fundamental change in the chromatographic system. The linear extrapolation method, based on the estimation of the relative influence of the instrument variance on solutes with different capacity factors, is a more attractive alternative method since the column remains in the chromatographic system. This method is only valid when a number of conditions are satisfied. By meeting these conditions the error in the instrument variance by using the linear extrapolation method was determined. At the same time, ways to minimise these errors were studied. Use of the linear extrapolation method in combination with conventional columns of 4.6 mm i.d. appears to yield inaccurate results. In combination with microbore columns the method can be used, provided the columns have a maximum length of 5cm and contain a packing material with a particle size of 2 or 3μm. The error in the determined instrument variance is then of the order of 2μl2.
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  • 31
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    Chromatographia 23 (1987), S. 209-214 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Review of triglyceride analysis ; Column temperature gradients ; Combined LC and other techniques
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The present review cites 54 papers dealing with reversephase HPLC analysis of triglycerides. The objective of the review was not merely to list the main contributions made in recent years but also to present a discussion of those papers representing qualitative advances and improvements helping to obviate the difficulties associated with this type of analysis. The use of mobile phase polarity and column temperature gradients and the combination of HPLC with other analytical methods such as mass spectrometry or GLC analysis of fatty acids are examples of such contributions.
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  • 32
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    Chromatographia 23 (1987), S. 254-256 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Synthesis of stationary phases ; Influence of surface pH ; Influence of temperature, concentration and reaction ; time
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new way to produce liquid chromatographic stationary phases is suggested. The method is based upon a solide-phase reaction between the silica surface and the adsorbed silane molecules. The role of surface pH is demonstrated. The influence of other reaction conditions (concentration of the silane solution, effect of temperature and reaction time) is discussed.
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  • 33
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral stationary phases ; Succinimido carbamate intermediates ; Amino acid enantiomers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Chiral stationary phases (CSPs) for liquid chromatography were prepared by the way of an activated carbamate intermediate. The amino group of aminopropylsilyl silica gel was first activated by carbamylation with disuccinimido carbonate (DSC). The obtained activated carbamate silica gel (ACsil) proved useful as an intermediate for the preparation of urea-type CSPs. The reaction of ACsil with (S)- of (R)-1-(α-naphthyl)-ethylamine gave naphthylethylurea type CSPs. These CSPs were also obtained directly from aminopropylsilyl silica gel by its reaction with optically active (S)- or (R)-succinimido 1-(α-naphthyl)ethyl carbamate (SINEC). Several phenylthiohydantoin amino acid enantiomers and p-bromophenylcarbamyl amino acid enantiomers were resolved on the CSPs by elution with aqueous mobile phase.
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  • 34
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography ; Bonded silica ; Residual silanol groups
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Silanol groups of chromatographic material surfaces were determined by chemical reaction with methyl-lithium. Evolved methane was measured by a gas chromatographic method using a column packed with molecular sieves. This chromatographic technique leads to very reproducible results, particularly for the control of the hydroxylation of a silica gel and for the analysis of residual groups at the surface of bonded silica.
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  • 35
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Aldehydes ; Annular denuder ; Environmental analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An improved procedure for the HPLC determination of C1−C3 aldehydes in environmental samples is described. These air pollutants are quantitatively collected on annular denuders coated with 2,4-Dinitrophenylhydrazine and analyzed as hydrazone derivatives by HPLC with UV absorbance and voltammetric detection. Collection efficiencies of aldehydes are reported and compared with other available methods. Practical examples of the application of the method are given.
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  • 36
    ISSN: 1612-1112
    Keywords: Estriol ; Urine ; Menstrual Cycle ; Column liquid chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A high-performance liquid chromatography (HPLC) assay for estriol in nonpregnancy urine is described. After Enzymic hydrolysis, the estriol is extracted from urine by the sorbent trap technique utilizing graphitized carbon black (Carbopack B). After some washing steps, estriol is desorbed by a suitable solvent system. After solvent removal, the sample is injected into an HPLC column for estriol quantification. Analytical recovery of estriol was 96.1%. The precision of the method was 2.6 and 4.9% respectively at 145 and 10.6ng/ml of urine. The limit of sensitivity was set at 0.8 ng/ml of urine. The mean contents of estriol in the follicular and luteal phases were respectively 11.3 and 38.8 ng/ml of urine.
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  • 37
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Isohydric solvents ; Butyrophenones ; Direct-silica gel
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The behaviour of butyrophenones in high performance liquid chromatography on silica gel using isohydric solvent systems has been studied. The influence of column temperature, water content, acidity and polarity of isohydric solvents on the retention, column efficiency and resolution of a series of butyrophenones have been investigated. Through the results obtained more insight has been gained into the theoretical aspects of the adsorption process on silica gel with isohydric solvent systems.
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  • 38
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed-phase separation ; Oligodeoxyribonucleotides ; Isolation of pure material
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A reversed-phase chromatographic column suitable for the purification of chemically synthesized large oligodeoxyribonucleotides (oligo-DNA) was prepared. The specifications of this column are; the selected silica (Toyo Soda silica) with large pore size (at least 150 Å) and small particle diameter (5 μm desired) should be grafted only with monochloro alkylating reagent of long alkyl chain (sufficiently C18) so that the carbon content of the resultant packing material is 15–16%. Using this column, we could isolate the targeted large oligo-DNA (up to 50mer) in a large scale (75 μg per one cycle) from the impurities in the reaction mixture formed during the automated synthesis by the phosphite method.
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  • 39
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    Chromatographia 23 (1987), S. 292-300 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Separation of sugars ; Review
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This contribution to the problems of carbohydrate (sugar) column liquid chromatography, evaluates several currently used systems (reversed phase octadecylated silica gel, amino modified silica gel, cation exchangers on polystyrene and on silica gel basis, polyol derivatised silica gel and anion exchange systems). The elution pattern, analysis time, column efficiency and column life time expectancy are considered to be the important points for this comparison. The application of silica gel-based cation exchanger and of polyol derivatised silica gel is new to this field. The comparison and/or evaluation tries to be critical and to come to a conclusion for the choice of a recommended system.
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  • 40
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Packings of octadecylated microporous glass ; Dimethadione and trimethadione in serum ; Pancreatic stones
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The liquid chromatographic determination of trimethadione (TMO) and its methabolite, dimethadione (DMO) were studied by high-performance liquid chromatography (HPLC) on octadecyl-modified microporous glasses, prepared with toluene solution containing octadecyl-dimethylchlorosilane, using two types of microporous glass with various mean pore diameters and/or specific surface areas. Using acetonitrile-water mixtures as eluents, TMO and DMO in human serum were separated on the glasses studied, but with different degrees of resolution. In this present study, we report the development of a rapid and selective HPLC method for the simultaneous analysis of TMO and DMO in human serum.
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  • 41
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Cross-linked polystyrene ; Characterization of surfaces
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The properties of the poly(styrene-divinylbenzene) copolymers PRP-1 and PLRP-S have been studied by infrared spectroscopy and chromatographic techniques. The following results were obtained: PRP-1 and PLRP-S are spectroscopically very similar. Their surfaces are chemically neither homogeneous nor stable during use. Retained nonpolar solutes should be eluted with a mobile phase containing tetrahydrofuran. Uncharged acids and anions can be chromatographed without difficulty. Cations of amines should be chromatographed only with a mobile phase of low pH. Uncharged amino-alcohols cannot be chromatographed without the addition of a competitor.
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  • 42
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemically bonded phases ; Kinetics of silanization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A wide-pore silica for HPLC with a particle size of 7.5 μm, specific surface area of 360m2/g, pore diameter of 20 nm and pore volume of 2.1 cm3/g was silanized with n-octadecyldimethyl-chlorosilane (ODMCS), n-octadecyldimethylmetoxysilane (ODMMS) and n-octadecyldimethyl-dimethylaminosilane (ODMAS), in sealed glass ampoules. The ligand density obtained with an excess of ODMCS and ODMMS was found to be limited by reaction equilibrium; at low (〈50%) conversion of the surface silanols, the reaction displays pseudo-first-order kinetics. Silanization with ODMAS, which seems to be sterically controlled at higher conversions, yields a relatively high concentration of bonded octadecyl ligands (4.24μmol/m2).
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  • 43
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    Chromatographia 23 (1987), S. 684-685 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Pentafluoroanilinopropyl silica gel ; Donor-acceptor complexes ; Aromatic hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of a new pentafluoroanilino-phase for HPLC is described. The retention times (tr) of about twenty aromatic hydrocarbons have been determinated. It has been shown that the aromatics were eluted according to the number of rings. The influence of water content in the mobile phase is commented.
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  • 44
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thiol drug analysis ; Derivatization by ethacrynic acid ; Pharmaceutical formulations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A high performance liquid chromatographic method has been developed for the determination of aliphatic thiol drugs, such as N-acetyl-L-cysteine, captopril and mercaptopropionylglycine in pharmaceutical formulations. The procedure involves a precolumn derivatization of the thiol drug with ethacrynic acid followed by reversedphase HPLC separation and UV detection. The conditions for a rapid and selective reaction of the thiols with ethacrynic acid have been investigated. The method proved to be suitable for a reliable and selective quality control of commercial dosage forms of the examined thiol drugs.
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  • 45
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    Chromatographia 23 (1987), S. 657-662 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Post-column derivatization ; Sugar analysis ; Wine characterization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A HPLC system with post-column derivatization for the quantitative analysis of sugars in complex matrices is described. As reagent a 0.2% solution of thymol in concentrated sulfuric acid has been used. The reaction is sensitive with reducing as well as non reducing sugars whereas sugar alcohols are discriminated. With this reagent and separation of sugars at high pH values with an anion exchange column it is possible to detect sugars in the ng range. Hence, it is possible to characterize wines not only by their fructose and glucose content but also by differences in the distribution of the other not fermentable sugars like trehalose, arabinose, galacturonic and glucuronic acid.
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  • 46
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    Chromatographia 23 (1987), S. 709-712 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polymer-based support ; Aldehydes ; Fluorescence detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The aldehydes were separated by reversed phase chromatography on a polymer-based support. Acid catalysis on the column was needed to obtain sufficiently fast equilibrium between acetaldehyde and its hydrate. Deuterium labeled acetaldehyde (D3) yielded complete separation from the nonlabeled compound, probably due to a difference in hydratization. Fluorescent products were obtained by reaction between the aldehydes and a mixture of ammonia and dimedone (5.5-dimethyl-1.3-cyclohexanedione). The fluorescence was detected at 460 nm after excitation at 390 nm. A reaction time of 42 seconds at 90°C in a knitted teflon capillary produced detection limits of 0.5 and 1 ng for acetaldehyde and formeldehyde, respectively. A method for preparation of a stable reagent with low background fluorescence is described.
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  • 47
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thiols and disulfides ; Fluorescence derivatization ; Monobromobimane
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The influence of reducing agents (sodium borohydride, tributylphosphine, dithioerythritol and dithiothreitol) on the conversion of disulfides into their parent thiols, with specific application to cysteine was investigated. Dithioerythritol and dithiothreitol were found to be most suitable for this reaction. A contact time of one hour at room temperature provided quantitative reduction as tested using cystine as a pure disulfide standard. A modified fluorescence labelling procedure with monobromobimane followed by reversed-phase HPLC allows quantitation of the parent thiol and the disulfide content when completing the labelling reaction with and without preliminary treatment with reducing agent. The effects of various bimane reducing agent ratios on the yield of the reaction are discussed. Precautions should be taken when dealing with complex matrices with respect to reagent concentrations and ratios.
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  • 48
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chrial separations ; Succinimido carbamate derivatives ; Propranolol
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A chiral derivatization reagent having activated succinimido carbamate moieties were developed for the optical resolution of enantiomeric amines by high-performance liquid chromatography. Succinimido R-(+)- or S-(−)-1-phenylethyl and R-(+)- or S-(−)-1-(α-naphthyl)-ethyl carbamates were synthesized by the reaction of optically active phenylethyl and naphthylethyl amines with discuccinimido carbonate (DSC). These reagents reacted with both primary and secondary amine enantiomers such as amino acids and β-amino alcohols to give the corresponding diastereomeric urea derivatives. These diastereomers were efficiently separated by reversed-phase liquid chromatography and detected by their absorption or the fluorescence of the chromophores. The chiral derivatization procedure was applied to the separation and determination of enantiomeric propranolol in serum.
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  • 49
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed phase operation ; Calculation of optimum solvent composition ; Polymethoxylated flavones
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An optimization procedure for the chromatographic separation of polymethoxylated flavones is described. A polyhedron working volume is drawn from a truncated tetrahedron constructed from the four solvents selected. The response function is an n'th degree polynomial the coefficients of which are calculated through the least squares method by means of B=(X′X)−1X′Y in which X′X is the information matrix (X′X)−1 the variance covariance matrix. X is the matrix of the model (polynomial built from the selected experiments) and X′ the transposed matrix. Y is the quality of the chromatogram defined by the resolution of each pair of solutes. An exchange algorithm matrix yields the minimum number of runs necessary to obtain a correct B. Isoresponses curves are drawn by intersection of a cubic volume which includes the polyhedron to give a better insight. An optimal zone is then determined and provides the solvent composition. An optimized chromatogram of 8 methoxylated flavones demonstrates the application of the method.
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  • 50
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    Chromatographia 23 (1987), S. 132-136 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column liquid chromatography ; Thin-layer chromatography ; Analysis of lactulose in carbohydrate mixtures
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Lactulose is a disaccharide with important implications in medicine, nutrition and dairy technology. It has to be determined usually as a minor component in complex matrices containing many other sugars. This paper describes the different chromatographic techniques (planar, liquid and gas chromatography) which have been proposed for the separation and quantification of lactulose in mixtures with other carbohydrates; the advantages of each technique are compared and some features where more research is necessary are outlined.
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  • 51
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    Chromatographia 23 (1987), S. 328-330 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Arylsulphonohydrazides ; On-column hydrolysis ; Fungicides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A number of fungicidally active arylsulphonohydrazides are examined by normal- and reversed-phase liquid chromatography. Although good separations are achieved by reversed-phase LC, difficulties are encountered due to analyte hydrolysis. On the other hand, satisfactory analyses are possible by normal-phase LC particularly on modified silicas.
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  • 52
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    Chromatographia 23 (1987), S. 377-378 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Solid phase extraction ; Codeine and morphine in blood
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid and efficient procedure is described for the extraction and analysis of codeine and morphine in whole blood. Red blood cells were fragmented by sonication and the blood sample extracted by passing through a bonded silica column (Bond Elute®). The adsorbed drugs were washed and eluted followed by analysis by HPLC. Recoveries were between 95–100% at 5 ng/ml concentrations.
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  • 53
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    Chromatographia 23 (1987), S. 651-652 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Metoclopramide ; Electrochemical detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple, reproducible liquid-chromatographic method for determination of metoclopramide anti-emetic and anti-spasmodic agent is described. Metoclopramide is extracted from alkalinized plasma into diethylether, then separated with a sperisorb CN column and measured through amperometric detection at +1,4 volt vs Ag/ AgCl. The average extraction recovery was 92%. Standard curves were linear and reproducible from 0.05 to 1.5 mg/ L. Within-day CV was better than 6%.
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  • 54
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    Chromatographia 23 (1987), S. 507-511 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Toluene Diisocyanate in air ; Collector for air sampling
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A useful method of sampling and measurement of toluene diisocyanate concentration in atmosphere is described. The sampler consists of glass-fibre filters impregnated with the reagent 1-(2-methoxyphenyl)piperazine1 so that the 2,4 and 2,6 isomers of TDI react to form urea derivatives which are analysed by high performance liquid chromatography in isocratic mode on cyan-amino and C18 bonded phases. A dynamic system was used to generate standard atmospheres of TDI and to validate the sampling method within the humidity range of 0% to 75%. A coated filter, a bubbling solution and an impregnated silica gel were compared as samplers requiring the piperazine reagent in performance experiments.
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  • 55
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    In:  Bull., Polar Proj. OP-O3A4, ASST'87, Berlin, Springer, vol. 81A, no. 16, pp. 347-350, (ISBN: 3-540-23712-7)
    Publication Date: 1987
    Keywords: Detectors ; Seismology ; Pattern recognition
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  • 56
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    In:  47. DGG-Tagung, Clausthal, DGG, vol. C 560, 183 pp., no. GL-TR-89-0143, pp. 235, (ISBN 3-933346-037)
    Publication Date: 1987
    Keywords: Data analysis / ~ processing ; Detectors ; ARR ; arc ; BUG ; Seismology ; Pattern recognition ; Seismic networks
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