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  • Column liquid chromatography  (86)
  • Springer  (86)
  • 1990-1994  (86)
  • 1985-1989
  • 1970-1974
  • 1992  (86)
  • 1972
Collection
Publisher
  • Springer  (86)
Years
  • 1990-1994  (86)
  • 1985-1989
  • 1970-1974
Year
  • 1
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porous polymer spherical packings ; Vinyl ether ; Alkali resistance ; No abnormal adsorption
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Spherical, porous-polymer particles for column packing in high-performance liquid chromatography were prepared by suspension copolymerization of alkylvinyl ether with triethyleneglycol divinyl ether. The hydrophobicity of the packings was easily adjusted by changing the monomer ratio. The packings showed the usual reversed-phase liquid chromatographic properties, but did not sho abnormal retention, tailing and broadening of peaks and irreversible adsorption of ionic and aromatic substances, owing to the lack of ionic or aromatic groups. In addition, the packings were stable in alkaline solutions because of the relative alkali stability of C−O−C bonds as compared with CO−O and Si−O−C bonds in conventional packings.
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  • 2
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polycyclic aromatics ; Water and sediment samples ; Coal washings
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Analytical methods for the determination in environmental samples, of some selected Polycyclic Aromatic Hydrocarbons (PAH's), which are included on the EPA Priority Pollutant list, have been developed and evaluated. The methodology involves the extraction of PAH's from water samples by solvent extraction with dichloromethane. Solid samples were ultrasonically extracted with acetone/hexane and the extract was cleaned up on a silica gel/alumina column. The concentrated and cleaned up extracts were analysed by HPLC on a polymeric C18 column using a gradient of acetonitrile/water as the mobile phase and fluorescence detection. Typical detection limits lie in the range of 1–30 ng ml−1 of the analytes, but after sample pretreatment detection limits of 10–300 ng l−1 were obtained. The extraction, clean-up and HPLC methodology was applied to the determination of selected PAH's in coal washings samples and the method was validated by the quantification of PAH's in a natural contaminated and a spiked sediment.
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  • 3
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Methoprene ; Tobacco
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid sample preparation procedure combined with a short reversed-phase HPLC separation for the quantitation of methoprene residue in tobacco samples is described. A ground tobacco sample of 0.5 g is mixed with 3 mL of 2-propanol. The mixture is extracted for twelve minutes with the aid of sonication at an elevated temperature (45–55°C) and then filtered through a 0.45 μm disposable filter prior to injection on HPLC. No sample cleanup or solvent evaporation step is required. Chromatographic analysis is performed on a C-18 column and the analysis time is 12.5 minutes. The detection limit for methoprene in tobacco samples is one part per million (μg/g).
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  • 4
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Diol silica gels ; Carbohydrates ; Evaporative light scattering detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Bonded silica columns have been evaluated for their ability to separate carbohydrates and polyols. Mobile phases consisting of dichloromethane/methanol produced the best separations in comparison with the acetonitrile/water mixtures commonly used with amino columns. Of all the bonded phases tested, LiChrospher Diol silica provided the best separations, and selectivities were not very different from those obtained on the most popular system using an amino bonded phase and acetonitrile/water as eluent. In addition, diol columns with a dichloromethane/methanol eluent offer excellent stability with no Schiff’s base formation of reducing sugars. Using an evaporative light scattering detector, low limit detection is obtainable (20 ng of glucose from a column) and gradient elution is quite feasible.
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  • 5
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; UV detection ; Pentafluorobenzyl chloride by UV detection ; Chloride in biological fluids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A reversed-phase high-performance liquid chromatographic method for the determination of chloride in plasma, urine, saliva, sweat and aqueous solution is described. Chloride, in solution in aqueous acetone, is converted by means of pentafluorobenzyl bromide into pentafluorobenzyl chloride. This derivative is separated on a ODS-5 μm reversed-phase column using isocratic elution with acctonitrile/water, 50/50, v/v, at a flow rate of 2.0 ml/min, and detected by a UV detector at 264 nm. The method is rapid, accurate and sufficiently sensitive for the determination of chloride in less than 10 μl sample volume of a biological fluid.
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  • 6
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral discrimination ; Guaran-borate complex ; Mandelic acid enantiomers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The Chiral discriminating properties of the legume seed (Cyamopsis tetragonalobus) polysaccharide, guaran, has been investigated by this laboratory. Due to the presence of cis-hydroxyl groups in its molecule, guaran a galactomannan, forms tetracoordinated polymeric complexes with boron, resulting in cross-linking and gelling. Ligand exchange between the polymeric boron complex and a low molecular weight chiral diol can take place with stereoselectivity. The principle has been applied for the resolution of (±) mandelic acid by using ligand exchange chromatography.
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  • 7
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion-pairing ; Furosine ; Pyridosine ; Milk
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An ion-pair, reversed-phase, liquid chromatographic procedure using UV detection for quantitation of furosine is described. The standard plot was linear (r〉0.999) over a 5 ng range. An authentic synthesised sample of furosine was used for calibration. Commerical milk samples were analyzed by the described procedure.
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  • 8
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; α1 glycoprotein ; Enantioseparation ; β-blocking agents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The enantioselectivity of the α1 glycoprotein chiral stationary phase, Chiral AGP® has been evaluated for a number of β-blocking agents. A correlation has been found between the retention behaviour on this stationary phase and the hydrophobicity of the compounds. The separation factor α is higher for compounds that are well retained. Retention, and thus α, are also controlled by pH and the percentage of organic modifier in the mobile phase.
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  • 9
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    Electronic Resource
    Springer
    Chromatographia 33 (1992), S. 478-484 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porous glass adsorbents ; Surface free energy ; Oriented adsorption of hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The relationship between the specific capacity factor (k/S, where k is the capacity and S is the surface area of the sorbent, in m2) in the liquid chromatography of aromatic hydrocarbons and the adsorption energy (-°GA) has been investigated. The previously published results, based on the calculation of the work of adhesion (WSA) from contact angles, were re-examined and a new hypothesis on interactions at interfaces was employed. Direct proportionality has been found between k/S and-°GA, which allows prediction of the chromatographic behavior of adsorbates on sorbents. The surface free energy components were calculated in order to determine-°GA in terms of the work of adhesion. The dispersion component of the surface free energy of glass was obtained from the adsorption isotherm of n-octane and it was found that the hydrocarbon molecules are adsorbed in an oriented position. The contact angles of liquids on the outer surface of porous solids do not yield reliable values of WSA and of the surface free energy components. A higher intermolecular attraction increases WSA and decreases the contact angle in pores.
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  • 10
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography-mass spectrometry ; Water analysis ; Triazine herbicides ; Chemical ionization mass spectrometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Mass spectra of 12 triazines were obtained by electron impact (EI), positive-ion chemical ionization (PCI) and negative-ion chemical ionization (NCI) using methane and isobutane as reagent gases. EI mass spectrometry is more sensitive than PCI and NCI, although the chemical ionization modes increase selectivity markedly. A pre-column packed with polymer stationary phase was employed to preconcentrate surface and drinking water samples. After desorption of the analytes with ethyl acetate, an aliquot was injected directly into the GC-MS system. Atrazine and simizine were found in these samples at 10–80 ppt levels. The limits of detection for both herbicides were below 10 ppt in drinking water.
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  • 11
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Diastereomer separation ; Chiral derivatizing agent ; Chiral oxazolidin-2-one
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Chromatographic separation of racemic amines, carboxylic acids and alcohols can be achieved with excellent resolution as measured in terms of the chromatographic separation factor α by derivatization with a homochiral oxazolidin-2-one easily prepared in three steps fromendo-borneol. The resolved materials can be isolated in excellent yields by cleavage of the resultant diastereomers using conventional methods, which also allow recovery of the chiral resolving agent for re-use.
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  • 12
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micellar mobile phase ; Direct injection of biological fluids ; Hexamethylene bisacetamide (HMBA)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This paper describes the direct injection analysis of the anti-cancer drug hexamethylene bisacetamide (HMBA) in biological fluids by an HPLC column switching technique. The first chromatographic column, which provides for sample extraction and cleanup, employs a micellar mobile phase with SDS as the modifier. The second column, coupled on-line to the first, utilizes reversed-phase conditions for analysis. UV detection is employed at 210 nm. 282 samples from 12 cancer patients were analysed and good pharmacokinetics curves obtained. The drug gives recoveries of 94.0–100.9% with a relative standard deviation of 1.88%. A sample analysis is completed within 15 minutes. This method should be satisfactory not only for the analysis of HMBA but also, probably for other drugs in biological fluids.
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  • 13
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Kalman filter ; Deconvolution ; Mycotoxins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The potential of a computational approach for the quantitative resolution of seriously overlapping chromatographic peaks when there is loss of collinearity between the pure component peaks and the mixture peak has been explored. The program makes iterative use of the Kalman filter algorithm for resolving the mixture peak with the component peaks aligned according to some values of the position parameters, and of a steepest descent minimization procedure to find the optimal alignment. This combined procedure has been applied to the quantitive resolution of the HPLC chromatograms of alternariol and altenuisol mycotoxins in synthetic mixtures and in real samples.
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  • 14
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Curcuminoid pigments ; Turmeric,Curcuma domestica Val
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid, simple and reproducible reversed-phase high-performance liquid chromatographic method was developed for the quantitative determination of curcumin, demethoxycurcumin and bis-demethoxycurcumin in ethanolic extracts of turmeric. The pigments were separated on a styrene-divinylbenzene copolymer column (Hamilton PRP-1), using an acetonitrile-water (55∶45, v/v) mobile phase. The pigments were monitored with a diode-array detector at 425 nm. The limit of detection was 10.2 ng curcumin, 11.1 ng demethoxycurcumin and 6.2 ng bis-demethoxycurcumin. Comparison of HPLC and spectrophotometric results for the determination of the total curcuminoid content for a number of turmeric samples, reveal that the spectrophotometric method invariably yielded higher results, indicating an overestimation of curcuminoids.
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  • 15
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Soybean lecithin ; Partial resolution ; Light scattering detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Using both synthetic phospholipids and soybean phosphatidylcholine (PC), it is shown that the retention of phospholipids during normal-phase chromatography is not only determined by the polar headgroup, but also by the fatty acid composition. Although fatty acid methyl ester determinations reveal that this effect only causes an enrichment of some fatty acids in subsequent fractions of the same phospholipid class, still a large influence on the peak shape is observed. As a further consequence, the evaporative light scattering detector output is greatly affected, so that accurate quantitation of phospholipid classes requires the availability of standards of the same origin.
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  • 16
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micelle-solute association constants ; Polynuclear aromatic hydrocarbons ; Octanol/water partition coefficients
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Sodium dodecyl sulphate, hexadecyltrimethylammonium bromide and polyoxyethylene(23) lauryl ether were investigated as mobile phases in the micellar liquid chromatography of polycyclic aromatic hydrocarbons of environmental concern. A wide range of surfactant concentrations were used and the retention parameters and distribution coefficients calculated. The trends in the retention data for the PAHs are discussed and several conclusions are presented concerning the partition coefficients when these surfactants are present in the mobile phase. Comparisons are made between the structural features of the compounds and their capacity factors, and the octanol/water partition coefficients are correlated with hydrophobicity for the PAHs studied.
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  • 17
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Post-column derivatization ; Light-scattering detection ; Carbohydrates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of post-column fluorescence derivatization and evaporative light-scattering detection to analyse saccharides selectively by LC was investigated. In order to compare the performances of these two detection systems, factors such as reproducibility, detection limits and linear calibrations were determined. Despite the derivatization reaction step, post-column derivatization is superior from the standpoint of sensitivity. The detection of saccharides in beverages is also described.
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  • 18
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Phenolic compounds ; Optimisation of isocratic separations ; River water samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Isocratic column liquid chromatographic systems with UV absorbance detection at 280 nm have been developed for the separation of 29 phenolics and related compounds. The selectivity was investigated on silica-, carbon- and polymer-based separation columns for the separation of phenolic type of components. The effects of various acetonitrile/buffer mixtures, and pH of the mobile phase, and their impact on the retention of the phenols was assessed. Tables of retention times on the four columns for the 29 phenols with two different acetonitrile/buffer mixtures, together with the retention times at three pHs from 6.5 to 2.3 with varying levels of organic modifier on the LiChrospher RP 18 column are presented. As an application, the analysis of real river water samples from the Ebro river is described using a solid phase extraction step prior to injection into the chromatographic system.
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  • 19
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 34 (1992), S. 182-184 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; C18 bonded phase ; Residual silanol groups ; Metal 5-Br-PADAP complexes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary If any residual (free) silanol groups remain at the surface of silica gel after bonding treatment, they may affect the retention of solutes since the dissociated groups (≡SiO−) will attract cations. The silanol group effect on the retention of cationic solutes will increase with increasing pH of the mobile phase but the effect will decrease with increasing hydrophobic-ion concentration at the C18 surface because such ions can mask the residual silanol groups. A method for the separation of metal complexes with 2-(5-bromo-2-pyridylazo)-diethylaminephenol (5-Br-PADAP) has been developed. The hydrophobic ion in the MeOH/H2O mobile phase was tetrabutylammonium (TBA).
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  • 20
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 34 (1992), S. 431-432 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thin-layer chromatography ; Porphyrine ether glycerides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Efficient TLC and HPLC conditions for the separation of a newly synthesized class of compounds, porphyrine ether glycerides, have been established. Supplementary physico-chemical characteristics are given for this group of solutes.
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  • 21
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Flow injection analysis ; Combined methods ; Transition metal ions ; Aqueous samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An automatic method based on the combination of a flow injection (FI) manifold with a liquid chromatograph has been developed for the enrichment and determination of transition metal ions in water samples. Alternatively, the FI configuration can be used as a screening system for the determination of the total concentration of heavy metals. Two-parameter expressions for calibration graphs involving preconcentration time and concentration of the analytes were established for both the FIA and the integrated FIA/HPLC methods. The preconcentration time depends on the concentration level of the analytes in the samples. The method is linear in the range 2–200 ng/ml, with r.s.d. values between 1.5 and 5.0. It has been applied to the determination of copper, lead, zinc, nickel, cobalt, cadmium and manganese in synthetic water samples.
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  • 22
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Precipitation chromatography of polymers ; Block copolymers of styrene-butyl methacrylate ; Association phenomena
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Block copolymers of styrene andt-butyl methacrylate can be analysed by methanol/tetrahydrofuran gradients on C18 or phenyl bonded phase columns. On both of these columns, retention increases with styrene content of the samples. At 50°C, the retention of PS or a block copolymer containing 45% styrene was longer on the phenyl than the C18 columns. This indicates the contribution of adsorption to retention on phenyl bonded phase columns. Lowering the temperature from 50 to 30°C caused earlier elution of part of the sample from the phenyl phase. On a C18 phase the same drop in temperature improved the shape of the peak, which also started later than at 50°C. This effect of temperature is generally observed in polymer retention due to an adsorption mechanism, whereas increasing retention with decrease in temperature is characteristic of a precipitation mechanism. The block copolymer investigated contained 15% free polystyrene precursor which could not be separated from the block copolymer under the conditions employed. The addition of 20% PS homopolymer with a molecular weight similar to that of the styrene block in the copolymer showed that the polystyrene eluted together with the block copolymer, whereas the addition of PS homopolymer with a much higher molecular weight caused an extra peak at the expected elution time.
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  • 23
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fatty acids and bile acids ; Fluorogenic precolumn derivatization ; 2-Bromoacetyl-6-methoxynaphthalene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of 2-bromoacetyl-6-methoxynaphthalene as a fluorogenic labelling reagent in pre-column derivatization for the HPLC separation of biologically active carboxylic acids (fatty acids and bile acids) has been investigated. The compound reacts (30 min. at 70°C) with carboxylic acids to give fluorescent esters that can be separated by reversedphase HPLC and detected at λ ex. 300 nm, λ em. 460 nm. The experimental conditions for the derivatization and chromatographic separation are discussed. Applications to the determination of valproic acid and chenodeoxycholic acid in pharmaceutical formulations are described.
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  • 24
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ultrafiltration ; Fermentation monitoring ; Sugars
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An automated on-line monitoring system for low-molecular-weight compounds (e.g. sugars) during fermentation processes is described. The applicability of cross-flow ultrafiltration, coupled on-line with high-performance liquid chromatography, is evaluated. Various detection modes for the determination of the test compounds lactose, glucose and fructose) in a complex fermentation broth are compared. In addition, the influence of some system parameters on the performance of several ultrafiltration modules for the removal of cellular and macromolecular broth constituents is investigated. A method for the fully automated determination of sugars during anE. coli batch culture in a brain-heart infusion medium is presented. With the present system five analyses can be performed every hour, using only 35μl of sample, without significant deterioration of the ultrafiltration process. Contamination by external micro-organisms was not observed and good correlation with an off-line method was found.
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  • 25
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Benzodiazepines ; Human serum albumin chiral stationary phase (HSA-CSP) ; Quantitative structure-enantiospecific retention relationships (QSERR) ; Structural descriptors ; Submolecular polarity parameter
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Quantitative structure-enantiospecific retention relation-ships (QSERR) have been derived for a series of 1,4-benzodiazepines. The compounds were chromatographed on a human serum albumin based HPLC chiral stationary phase (HSA-CSP). Molecular modeling of the solutes allowed the determiantion of various structural descriptors. Among these descriptors, a submolecular polarity parameter, PSM, was identified which was able to characterize enantiospecific interactions of benzodiazepines with the HSA-CSP. Combining PSM with the retention parameter of the less retained enantiomer permitted precise prediction of the retention of the second eluting enantiomer. Highly statistically significant regression equations were also derived which described the retentions of both enantiomers in terms of nonempirical molecular descriptors. The calculated enantioselectivity correlated well with the experimentally observed values. A significant conclusion from this study is support for the existence of two different binding sites for chiral benzodiazepines on HSA.
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  • 26
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; 2′-Deoxyuridine ; Anomer separation ; Isomer separation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A liquid chromatographic assay method was developed to separate 2′-deoxyuridine from its anomer and pentopyranosyl isomers. The influence of the pH of the mobile phase, the type of organic modifier and the column temperature on the chromatographic parameters was systematically investigated. Using a Hypersil C18 (5 μm) column at 10°C, the following mobile phase was found suitable: tetrahydrofuran −0.2 M potassium phosphate buffer pH 4.0-water (0.1∶5∶94.9, v/v).
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  • 27
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion-pair system ; Gossypol analysis ; Chicken liver ; Plant toxin residues
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An ion-pair, liquid chromatographic method for the determination of total gossypol in chicken liver has been developed. It involves hydrolysis of bound gossypol in the presence of ascorbic acid, partitioning into chloroform and isocratic separation on Spherisorb ODS2, 10 μm, column with a methanol-water mobile phase containing octane-1-sulfonate. Precision data based on within-day and between-days variation suggested an overall relative standard deviation of 8.1%, while overall recovery was 81.1%±3.
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  • 28
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Octadecyl modified silica ; Hexamethyldisilazane treated silica ; Calcination ; Heat-treated silica
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The effect of silanol groups on three types of octadecylmodified column gels using heat-treated silicas by calcination has been studied by high-performance liquid chromatography. After heat-treating at 180°C, 500°C and 950°C, the silicas treated with octadecyldimethylchlorosilane were used for the measurement of physical and chemical analysis. From elemental carbon analysis data, the reactive silanol group concentrations, αOH(s), were determined to be 2.0 in the 180°C treated silica, 2.1 in the 500°C treated silica and 1.6 in the 950°C treated silica, respectively (original silica: mean pore diameter 116 Å, specific surface area 298 m2/g, pore volume 1.22 ml/g, particle size 5.0 μm). The separation factors, α, of pyridine versus phenol were measured to be 0.79 on 180°C treated silica, 0.91 on 500°C treated silica and 1.98 on 950°C treated silica, using acetonitrile-water mixtures as the eluent. And then, on the basis of the physico-chemical and chromatographic data, the three types of octadecyl modified column gels using heat-treated silicas by calcination have been compared.
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  • 29
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Diode array detection ; Principal component analysis ; Evolving factor analysis ; Pesticide mixtures
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A recently developed self-modeling curve resolution method based in different factor analysis techniques has been applied for the first time to the study of liquid-chromatography-diode array data under situation where the separation of two components is not achieved. Two applications are reported: the resolution and quantitation of a coeluted mixture of carbamate pesticides pirimicarb and 1-naphthol, and the estimation of the concentration profiles of the double peak obtained in the elution of the triazine metabolite chlorodiamino-s-triazine. Different methods of quantitation are compared, including Evolving Factor Analysis and Rank annihilation. Quantitation from the area of the elution profiles once the component spectra have been transformed for their area contribution to the signal, gives a relative composition for pirimicarb and naphthol pesticides which agrees with the known sample composition. In the case of the unknown triazine mixture, an approximate quantitation of the two peaks obtained for this metabolite is obtained by assuming equal signal contribution or equal maximum absorbance of the individual spectra of the two detected components.
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  • 30
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Hydrophobic solutes ; Enthalpy and entropy changes ; Eluent composition effects ; Surface area effects
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Chromatographic retention of several nonpolar solutes by three reversed-phase liquid chromatography (RPLC) supports was measured at several temperatures with binary mixtures of methanol/water and acetonitrile/water as the mobile phase. These data were used to estimate enthalpy and entropy changes (ΔH sorp o and ΔS sorp o ) associated with solute retention. The dependence of these two thermodynamic parameters on organic solvent content (θ) in the mobile phase, solute hydrophobic surface area (HSA), and bonded n-alkyl chain length (Nc) of the RPLC support was evaluated. The differences noted in the two solvent mixtures were attributed to: (1) the manner in which solvent surface tension changes with increasing θ, and (2) the differences in the interaction of methanol and acetonitrile with the bonded alkyl chains.
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  • 31
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fluoropyrimidine drugs ; Pharmacokinetics of doxifluridine ; Chemotherapy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A reversed phase high performance liquid chromatographic method has been developed for the simultaneous determination of the pro-drug 5′-deoxy-5-fluorouridine (5′-dFUR), its metabolite 5-fluorouracil (5-FU) and some fluorinated pyrimidines involved in the metabolic activation process of 5-FU. The method has been used to monitor the bioavailability of 5′-dFUR and 5-FU in patients undergoing anticancer chemotherapy. Serum sample treatment involves addition of internal standard (5-bromouracil), protein precipitation with saturated ammonium sulphate solution and liquid-liquid extraction with ethyl acetate-isopropanol (90 ∶ 10 v/v). Urine is simply diluted with mobile phase and injected. The average recovery from serum (at 0.5 μg/mL level) was 95.0%±1.4 for 5′-dFUR and 86.3%±3.5 for 5-FU. A linear response extending over four decades of concentration was observed. Detection limits in the low ng/ mL range were obtained using a 250 μL sample size and a 20 μL injection volume. Within-day and between-day coefficients of variation were below 4 and 10%, respectively.
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  • 32
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Flow injection analysis ; Combined flow injection/HPLC ; Carbamate pesticides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An integrated flow injection (FI)/HPLC system for the total and individual determination of carbamate pesticides (propoxur, carbofuran and carbaryl) is proposed. The determination is based on the alkaline hydrolysis of the analytes and subsequent coupling with diazotized sulphanilic acid to yield the monitored dyes with or without a prior separation step by HPLC in a C18 column. The calibration curves obtained are linear in the μg/ml range and r.s.d. values are between 0.5 and 3.7% in all instances. Injection of the sample into the FI manifold allows the total pesticide content in the sample to be screened. The manifold thus acts as a post-column reactor/detector of the chromatograph for samples with high overall carbamate content, which are also injected into the HPLC instrument. The performance was checked with contaminated water samples.
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  • 33
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion-pairing ; Temperature effects ; Organic modifier concentration
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention behavior of phenylamine and naphthylamine sulphonic acid was evaluated in reversed-phase ion-pair liquid chromatography as a function of organic modifier concentration and column temperature. It has been observed that the logarithm of capacity factors decrease linearly with organic modifier concentration, and there is a good linear relationship between the intercept and slope for this relationship. Phenylamine and naphthylamine sulphonic acid retention decreases with increase in column temperature. A linear dependence of lnk ip ′ on the reciprocal of the absolute temperature, the Van't Hoff plot, was observed over the column temperature range studied, and the standard enhalpic change (ΔHo) for these sulphonic acid transfers from the mobile phaser to the stationary phase was determined. ΔHo was dependent on the solute structure and in the range from 2.5 Kcal/mol to 5.5 Kcal/mol, which is close to that observed in RP-HPLC. The enthalpy/entropy compensation effect was evaluated by plotting lnk ip(T) ′ vs. −ΔHo, and the apparent differences in retention mechanisms between the analytes were observed, which may arise from the significant differences in their configuration, hydrophobicity and the charges of the solutes as well as the complex retention processes of RP-IPC.
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  • 34
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral mobile-phase additive ; Inductive adsorption ; Enantiomer resolution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Separation of lactic acid enantiomers by inductive adsorption has been studied on silica columns using (S)-(+)mandelic acid as the chiral mobile-phase additive. The lactic acid peak is not very strongly retained, broad, strongly tailing and splits in two at loadings lower than 60 μmol cm−2 column cross-section and at mandelic acid concentrations higher than 10−4M. The splitting indicates partial separation of enantiomers: enantiomerically enriched fractions are obtained but not enantiomerically pure. Lactic acid retention strongly decreases with increasing concentration of both hydroxy-acids; mandelic acid acts by displacement and lactic acid acts by an overloading effect.
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  • 35
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thermospray MS detection ; GC/MS identification ; Epoxy resins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The need to determine the migration of toxic unreacted compounds in bisphenol diglycidyl ether epoxy resins prompted us to investigate the HPLC properties of bisphenol F diglycidyl ether and its hydrolysis products in the water-based food simulants 3% (w/v) acetic acid, distilled water and 15% (v/v) ethanol. Peaks were identified by reversed-phase HPLC thermospray mass spectrometry and gas chromatography/mass spectrometry.
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  • 36
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Oxindole alkaloids ; Uncaria tomentosa
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The main oxindole alkaloids from the root bark ofUncaria tomentosa were separated by reversed phase HPLC with an acetonitrile/methanol/phosphate buffer solvent gradient. UV detection was carried out at 245 nm. The chromatographic parameters for the separation of the alkaloids were optimized by studying the impact of the pH value of the mobile phase and the column temperature on the separation efficiency of the analytical system. The best separation was achieved with a mobile phase pH of 6.6 and a column temperature of 15°C. The method developed is suitable for the qualitative characterisation and quantitative determination of oxindole alkaloids in crudeUncaria tomentosa extracts and phytopharmaceuticals.
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  • 37
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemically bonded phases (CBP) ; Surface heterogenity ; Surface purification
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The surface chemistry of eight silica-gels with different siliceous matrix structures have been described. The influence of surface impurities on the chemical modification process (coverage density) with monooctadecylsilane has been studied. The surfaces of the adsorbents, before chemical modification, were cleaned by extraction with 20% HCl. Bare and modified materials were characterized using different physico-chemical methods e.g.: SIMS, CP/MAS NMR, porosimetry, pH measurement, elemental analysis and chromatography (GC & HPLC). The presence of trace amounts of different metallic elements creating new adsorption centers on the surfaces of the packings, have been demonstrated. Moreover, it has been shown that washing of silica gel adsorbents increases the coverage density of alkylsilyl ligands and improves the chromatographic properties of prepared packings.
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  • 38
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Zone-electrophoretic sample treatment ; Basic and acidic compounds ; Biological samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A modified valve arrangement for zone-electrophoretic sample treatment (ZEST)-which is coupled on-line with column liquid chromatography — is used to pretreat biological (plasma) samples. Carry-over of plasma proteins depends on the pH of the electrophoresis buffer. The determination of propranolol, metoprolol, cromolyn and salicylic acid demonstrates that both basic and acidic analytes can be isolated from the plasma matrix with high selectivity. Analogous piperazines, with different protein binding properties, were used to study the influence of protein binding on the recovery. It is shown that high protein can cause a decreased recovery.
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  • 39
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Suppressed ion chromatography ; Eluent composition and concentration ; Oxyanions in soils
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Methods based on simultaneous determination of oxy-anions in soil extracts are needed for studies of competitive adsorption of oxyanions by soils. We studied the effect of NaHCO3/Na2CO3 and NaOH/Na2CO3 concentrations on ion chromatographic (IC) determination of PO 4 3− , AsO 4 3− , SeO 4 2− , SeO 3 2− , WO 4 2− , and MoO 4 2− in a 10-mM NaCl matrix equilibrated with soils by using a Dionex 2002i IC unit. The eluent, 6.0 mM NaOH+4.5 mM Na2CO3, resolved the 10 mM Cl− from the six oxyanions. Elution times for Cl−, SeO 3 2− , SO 4 2− , NO 3 − , SeO 4 2− , PO 4 3− , WO 4 2− , MoO 4 2− , and AsO 4 3− were 1.7, 2.7, 5.2, 6.1, 7.8, 10.5, 14.3, 17.7, and 21.2, respectively. The recovery of 0.2-mM oxyanion standards added to the soil solutions ranged from 93.0 to 106.8%, with coefficients of variation ranging from 0 to 14.3%. The detection limits of the oxyanions studied ranged from 0.3 μM for SeO 3 2− to 9.0 μM for AsO 4 3− .
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  • 40
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Normal phase separations ; Chloro-substituted polycyclic aromatic hydrocarbons ; Coupled column system ; Environmental samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention behaviour of chloro-substituted PAHs on several commercial normal bonded phase HPLC columns has been investigated. Chloro-substitution was shown to generally decrease the retention on stationary phases like amino-, diol- and nitrophenylpropyl-modified silica. Dimethylaminosilica exhibited more complex retention characteristics towards chloro-substituted PAHs. On this stationary phase, the position of the chlorine substituents on the aromatic solute seemed to be of greater importance for retention than on the amino-, nitro- and diolsilica. For some chloro-PAHs, the retention was shown to increase with the number of chloro-substitutions, probably due to the large affinity of the electron-rich nitrogen in the stationary phase for the electron deficient π-system of the chloro-PAHs. Chloro-substituted PAHs were strongly retarded on the electron donating 2-(1-pyrenyl)-ethylsilica (PYE) stationary phase. However, the molecular shape of the chloro-derivatives had a large influence on retention, which was considerably decreased for some nonplanar chloro-derivatives of chrysene and benz(a)anthracene. A two-dimensional back-flush HPLC method, consisting of a combination of a nitrophenylsilica column and a PYE column of matched lengths, was shown to be useful for clean-up of chloro-substituted PAHs in environmental samples.
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  • 41
    ISSN: 1612-1112
    Keywords: Supercritical fluid chromatography ; Column liquid chromatography ; Microbore columns ; Octadecylsilyl silica ; Selectivity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The influence of column temperature and pressure on the planarity selectivity of encapsulated and polymeric octadecylsilane-modified silicas was examined using carbon dioxide mobile phase in supercritical fluid and liquid chromatography. The use of liquid carbon dioxide was found to enhance remarkably the molecular planarity recognition capability of the polymeric stationary phase compared with supercritical conditions. The influence of pressure and temperature on selectivity was seen to be significant with the polymeric phase but less with the encapsulated. It seems that pressure and temperature change the morphology of the polymeric phase to a greater extent than the encapsulated one.
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  • 42
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Retention ; Crown ethers ; Actinomycin D ; Metal cation complexation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Retention of crown ethers in reverse-phase HPLC has been determined by their bonding ability with cations present in the eluent. The dependence of retention of crown ethers on cation concentration exhibits an inflection and makes it possible to calculate stability constant for the crown ether-cation complex. It is shown that in 75% MeOH retention of antitumor antibiotic, actinomycin D, depends on [Na+] and not on [K+] at concentrations of K+ from 5×10−7 to 10−1 mol l−1. Hence, actinomycin D may be classified as an ionophore-antibiotic.
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  • 43
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Synthesis of bonded stationary phases ; Acceptor ligands ; Normal phases ; PAHs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The synthesis of several electron-acceptor stationary phases has been reviewed the materials evaluated for their capacity to separate polyaromatic hydrocarbons (PAHs). Chemically bonded phases were obtained by the same procedure; the organosilane moiety is monofunctional and the HPLC behaviour is compared under identical conditions. Examples of PAHs separations are given.
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  • 44
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Solid phase extraction ; PCBs in cod-liver oil ; GC/MS identification
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A group of non-planar PCBs (IUPAC nos. 28, 52, 101, 118, 138, 153, and 180) was identified in a cod-liver oil product by using high resolution gas chromatography-mass spectrometry (HRGC/MS) in electron impact (EI) and negative chemical ionization (NCI) modes. The cod-liver oil samples were prepared either in a cyano column by high performance liquid chromatography (HPLC) or by a solid phase extraction (SPE) clean-up procedure that included e.g. purified charcoal treatment. The two methods of sample preparation were evaluated on the basis of the detectabilities of the congeners. The GC/MS-SIM method allowed quantitative monitoring of congeners nos. 52, 101, 118, 138, 153, and 180 at low concentration levels. Detection limits were 1.2 pg and 130 fg (m/z 292.00) in EI and NCI modes, respectively. The determination levels in EI and NCI were 1.8 pg and 290 fg in HPLC followed by HRGC/MS and 170 pg and 27 pg in SPE followed by HRGC/MS. The linear range was from 5.0 pg/μl to 1.0 ng/μl and from 1.0 pg/μl to 1.0 ng/μl in EI and NCI modes, respectively. In addition, the co-planar PCBs, PCDDs, and PCDFs were also screened and two of the chlorinated furanes were identified by HRGC/MS-NCI after separation from non-planar PCBs by SPE. In this case the only congeners that could be quantified were 2,3,4,7,8-PCDF and 1,2,3,4,6,7,8-HCDF, the detection limit for them being 740 fg (m/z 351.90) with NCI. SPE allows the separation of the planar and non-planar compounds, but LC separation is more effective for separation of the compounds of interest from the matrix. LC clean-up is easier and faster to perform than SPE clean-up.
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  • 45
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Calix[4]arenes ; Host-guest chemistry ; Separation of stereoisomers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A high performance liquid chromatographic procedure on 5 μm RP-18 was developed for the separation of the four possible cis-trans isomers of tetramethyl-calix[4]arenoctol, and of their octaacetates, and their octamethyl ethers.
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  • 46
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Sphingomyelin ; Molecular species separation ; Experimental design and optimization ; Chemometrics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An improved method has been developed for the separation of molecular species of intact sphingomyelins from natural sources (chicken egg yolk, bovine brain, and bovine milk) by high performance liquid chromatography with light-scattering detection. The method was developed and optimized using a novel multivariate optimization strategy.
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  • 47
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Valproic acid ; Simultaneous determination of anticonvulsants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The derivatizing procedure of Moody et al. [20] for valproic acid has been simplified and applied to the simultaneous HPLC determination of valproic acid (VPA), barbital (B), primidone (PRM), phenobarbital (PB) and carbamazepine (CBZ) in serum or plasma of epileptic patients. The sample is deproteinized with acetonitrile containing esterification agents and an aliquot of the supernatant is heated to 70°C for 15 min with 4-bromophenacyl bromide. The reaction mixture is analysed on a C18 column at ambient temperature, with gradient elution and with detection at 205 nm. The time required for the chromatographic analysis is 13 min; identification is based on retention time and quantification is by peak area determination with an internal standard. The calibration curves show good linearity in the range 6.25 to 100 mg/L. The detection limits at a signal: noise ratio ≥3, ranged from 1 mg/L for B and CBZ to 2–3 mg/L for PRM, PB and VPA. The method described for the simultaneous determination of the five drugs in the same plasma pool, correlated well with isocratic HPLC methods specific for each drug. The simultaneous procedure described allows a reproducible (CVs≤6.5% within run) and rapid (25 min for sample preparation: 13 min for chromatographic run) therapeutic monitoring of patients treated with VPA and two or more antiepileptic drugs.
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  • 48
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Anion exchange ; Indirect photometric and direct conductivity detection ; Naphthalenesulfonate ; Inorganic anions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Indirect photometric and unsuppressed direct conductivity detection modes are examined using naphthalene mono-, di-, and tri-sulfonate as mobile phases for the separation of several anions such as F−, Cl−, NO2 −, Br−, NO3 −, SO4=,I−, and SCN− using a commercial anion exchange column. With all three mobile phases, conductivity detection shows better sensitivities and detection limits than indirect photometry. Conductivity detection is 5 to 16 times more sensitive than indirect photometry for all analytes. Detection limits achieved using these mobile phases are, for example, 0.04 ng and 0.1 ng for chloride ion with conductivity and indirect photometry, respectively. Both detection modes give wide linear ranges extending from at least 100 ppm to the detection limit of each anion which is generally about 0.02 ppm. Sulfur oxide anions such as dithionate and tetrathionate are separated using flow programming with naphthalenetrisulfonate as the mobile phase in less than 20 minutes. With both detection modes, desired chromatographic performance of these three eluents is achieved without pH adjustment of the mobile phase.
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  • 49
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micellar bile-salt mobile phase ; Enantiomeric resolution ; Retention model
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention mechanism involved in enantiomeric separation of binaphthyl compounds by HPLC with micellar bilesalt mobile phases is discussed. A new model for the equilibrium is proposed, in which a heterogeneous stationary phase comprising solvated and micelle-adsorbed portions is considered. The experimental data supported the adsorption of the bile salt micelles on the octadecylsilica stationary phase which could recognize the chirality of binaphthyl compounds.
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  • 50
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Pre-derivatization ; Catecholamines ; 9-fluorenylmethyl chloroformate (FMOC-Cl)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Optimum conditions for the separation of 9-fluorenylmethyl chloroformate derivatized catecholamines by HPLC are described; three catecholamines (noradrenaline, adrenaline and dopamine) and an internal standard (epinine) were separated in less than 20 minutes under isocratic conditions. This method is 17 to 350 times more sensitive than electrochemical detection, depending on the test compounds. It has been applied to the analysis of catecholamines in urine. The sample was extracted by a metal-loaded silica prior to separation.
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  • 51
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Affinity chromatography ; (Na,K)-ATPase β-subunit ; Wheat germ agglutinin ; Protein purification
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Wheat germ agglutinin (WGA) affinity chromatography was examined as a method for the purification of the glycosylated beta subunit from SDS solubilized (Na,K)-ATPase. This lectin, WGA, bound quantitatively all of the beta subunit from SDS solubilized (Na,K)-ATPase whether or not the sample was reduced and/r alkylated. The combination of affinity and high performance size exclusion chromatography purified the beta subunit to a single band on SDS-PAGE electrophoresis. Compared to other methods of isolation this two step procedure utilizing wheat germ agglutinin was superior in terms of yield and purity for the beta subunit of (Na,K)-ATPase.
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  • 52
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Isotachophoresis ; On-line sample pretreatment ; Pesticide analysis ; Bentazone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The analysis of compounds which are present in low concentrations in complex sample matrices is often hampered by the lack of adequate sample pretreatment methods. In this study isotachophoresis (ITP) is presented as a selective sample pretreatment technique for ionic substances prior to HPLC analysis. It is shown that the ITP sample treatment and the HPLC analysis step can easily be operated in an on-line mode, which greatly facilitates automation.
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  • 53
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Official methods of analysis ; Method evaluation ; Minocycline
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The liquid chromatographic methods laid out for the analysis of minocycline hydrochloride in the British Pharmacopoeia 1988, the United States Pharmacopeia XXII and the Pharmacopée Française 10 were examined. The major difference between these methods lies in the adjustment of the pH of the mobile phase. The analyst has to obtain the right pH of the mobile phase for his available column. This was found to be a less than easy task for the occasional analyst. Other disadvantages observed were poor solubility of the components of the mobile phase, reduced sensitivity due to UV absorbance by the mobile phase, rather high back pressure, the elution order for 9-minocycline depending on the brand of stationary phase, and above all, poor stability of the stationary phase.
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  • 54
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Arsenic compounds ; Polymeric styrene divinylbenzene phase ; Ion-pairing
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The resolving power of an ion-pair reversed-phase liquid chromatography method, on a polymeric stationary phase (PRP-1) with an alkaline aqueous mobile phase (pH=9) containing tetrabutylammonium cation as ion-pairing agent, is compared with a traditional ion-pairing system using an octadecyl-modified silica column and a neutral aqueous mobile phase (pH=7.3). This chromatographic system (PRP-1 column) provides a rapid means for the determination of two of the most important arsenic species, arsenobetaine and arsenite. Addition of methanol (5%) to the aqueous mobile phase allows the differentation of arsenobetaine from the system peak when using UV detection.
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  • 55
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gravity-flow column chromatography ; Provitamin A determination
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The provitamin A content of some food samples was determined by methods involving MgO: Hyflosupercel gravityflow column chromatography (GFCC) and reversed phase high performance liquid chromatography (HPLC), the quantitation being done by external standardization (HPLC-ES) or internal standardization (HPLC-IS) with Sudan. The results obtained with α- and β-carotene in carrots, β-carotene and β-cryptoxanthin in papaya and β-carotene in tomato and kale agreed well, showing that any of the these techniques can be used, provided the analysis is done under optimum conditions. Good separation of the different provitamins using GFCC depends on the analyst's skill and visual acuity. HPLC-ES required a constant supply of provitamin standards, thus the varying purity of commercially available standards and the high instability of these compounds could pose grave problems. Due to the stability of Sudan, HPLC-IS appeared to be the method of choice although passage of the extract through a MgO: Hyflosupercel minicolumn was required prior to injection to separate chlorophylls, dihydroxy- and polyoxycarotenoids which would otherwise elute with Sudan. Nonconformity of the Sudan structure to those of the provitamins did not effect the quantitative results. The chromatographic separation, identity and quantification of the provitamins could be more easily established by using HPLC-IS, complemented with GFCC.
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  • 56
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 33 (1992), S. 344-346 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Charge-transfer chromatography ; Carbon clusters ; Fullerenes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A comparison of three binary mobile phases in LC separation of C60 and C70 fullerences on chemically bonded 2,4-dinitroanilinopropyl (DNAP) stationary phase was carried out, n-Hexane-benzene has been found to be the best mobile phase for efficient separation of the all-carbon molecules permitting high loads in preparative LC.
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  • 57
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Trichlormethiazide ; Electrochemical detection ; Diuretics in plasma and urine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This paper describes a high-performance liquid chromatographic (HPLC) assay method for the determination of trichlormethiazide (TCM) in human plasma and urine. After extraction and separation on an ODS column TCM from plasma was detected by oxidation in an electrochemical detector (ECD) by a porous graphite electrode. The sensitivity was better than HPLC with UV detection, enabling the determination of 2 ng ml−1 TCM in human plasma. This method also allows determination of TCM at higher concentrations by exchanging the UV for the electrochemical detector. To study the pharmacokinetics, TCM in plasma and urine was assayed with coefficients of variation in the range 2–3%. The method has the advantages of high sensitivity for plasma assay and high precision with a simple procedure for both plasma and urine samples. Small samples of 0.5 ml plasma per assay also reduced the total volume of plasma needed.
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  • 58
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porous graphitized carbon ; Ring-substituted aniline derivatives ; Electronic interactions ; Principal component analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention characteristics of 22 aniline derivatives were determined on a porous, graphitized-carbon column in unbuffered acetonitrile-water and methanol-water mixtures. Each aniline derivative gave symmetrical peaks in each eluent without buffers. Good linear correlations were found between the log k′ and the concentration of the organic component in the eluent. The slope and intercept values differed according to the type of organic modifier and the charcter, number and position of substituents, indicating the different selectivities of methanol and acetonitrile and the good separating power of the column. Multivariate mathematical-statistical calculations proved that the retention of ring-substituted aniline derivatives is mainly governed by electronic parameters and the hydrogen acceptor capacity of substituents.
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  • 59
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 33 (1992), S. 377-384 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gel permeation chromatography ; Synthetic resin analysis ; Quality control of resin manufacture
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The article gives a brief survey of the use of liquid chromatography in characterizing different kinds of synthetic resins and presents several examples of the application of this technique for analysis of such materials.
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  • 60
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Perfluoroalkylated polymer-gel packings ; Aromatic and fluorine-containing compounds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Porous, perfluoroalkylated polymer-gels for column packings in high-performance liquid chromatography (HPLC) were prepared by suspension polymerization of heptadecafluorodecyl arcylate and ethylene glycol dimethacrylate. The packings showed no abnormal retention for ionic or aromatic compounds, due to the lack of ionic or aromatic groups. In addition, the packings showed no excessive retention for strongly hydrophobic compounds which is often the case with long-chain, alkylated silica gels and polymer gels. This is due to the extremely low surface energy of perfluoroalkyl groups. Therefore, perfluoroalkylated polymer gels enable isocratic HPLC separation of solutes with significantly different hydrophobicity.
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  • 61
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Solid phase extraction ; 1,4-Benzodiazepines ; Drugs in plasma and urine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new method to predict the most suitable conditions for the solid phase extraction of 1,4-benzodiazepines and related compounds using C18 Sep-Pak carridges is proposed. The composition of the washing and elution solvents for the solid phase extraction of a test compound can be obtained from its capacity factor on a C18 HPLC column and an equation which relates capacity factors and solid phase extraction data of other similar compounds. The solid phase extraction data given in this paper can be used by others, there by saving considerable time and effort in the development of sample preparation methods. The suitability of the method was checked with two test compounds, showing good results.
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  • 62
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Heat-treated milk ; Milk quality indicators ; 5-Hydroxymethyl-2-furfuraldehyde
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An enhanced method of HPLC for the determination of 5-Hydroxymethyl-2-furfuraldehyde (HMF) in fluid milk was perfected. Its resolving capacity permitted the specific separation of this compound. The real concentration (μmol/l) of HMF was determined and not the HMF value, as in the colorimetric analysis, where an intermediary coloured compound (HMF-TBA) is utilised. The optimum pH condition (pH=4.0–4.2) for the mobile phase to prevent overlapping between the HMF peak and the peaks of the other compound (α and β) that coeluted with the HMF and also the optimum organic solvent content (3% or 7%) were established. This is a sensitive, quick and safe method for the determination of HMF in fluid milk.
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  • 63
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Enantiomeric separation ; Micellar bile-salt mobile phase ; Binaphthyl compounds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Optical isomers of substituted binaphthyl, compounds such as 2,2′-dihydroxy-1,1′-dinaphthyl and 1,1′-binaphthyl-2,2′-diyl hydrogenphosphate are, separated by HPLC using micellar bile-salt mobile phases. Operating conditions which affect the optical resolution of these enantiomers are examined. The largest separation factor achieved for these enantiomers is 2.74. The elution order of the latter enantiomers changes with mobile phase composition.
    Type of Medium: Electronic Resource
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  • 64
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography/mass spectrometry ; Ligand exchange ; Dipeptides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A two step process is described for the separation and identification of trace amounts of dipeptides in an hydrolysed brain extract. Peptides were first separated from the amino-acids by ligand exchange chromatography (LEC) on an iminodiacetate bonded polymer in the Cu(II) form. After elution from the LEC column, peptides were transformed into volatile derivatives and separated by gas chromatography (GC). This method presented many advantages in comparison with the liquid chromatography (LC) commonly used for peptide separations: a better efficiency due to the utilization of a capillary column, a better selectivity between the amino-acids and peptides and less interference from non-peptidic substances. Combination of GC with mass spectrometry allowed the sequence determination of twelve dipeptides in the extract. Three of them were quantitatively determined.
    Type of Medium: Electronic Resource
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