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  • Column liquid chromatography  (82)
  • Springer  (82)
  • Oxford University Press
  • 1995-1999  (82)
  • 1980-1984
  • 1975-1979
  • 1995  (82)
  • 1981
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  • 1995-1999  (82)
  • 1980-1984
  • 1975-1979
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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 40 (1995), S. 99-101 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; High temperature open-tubular columns ; Solvent make-up ; Acetophenone oxidation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Acetophnone, a substance stable at room temperature, is readily oxidizes in a high temperature open tubular liquid chromatographic system by the residual oxygen in the mobile phase. The oxidation product is less UV absorptive and detection sensitivity decreases greatly. To prevent the oxidation, through degassing of the mobile phase is necessary.
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  • 2
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Endotoxins ; Lipopolysaccharide ; Aminated poly(γ-methyl L-glutamate) ; Bovine serum albumin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the selective removal of endotoxins from various protein solutions using columns packed with aminated poly (γ-methyl L-glutamate) (PMLG-NH2) spheres. The PMLG-NH2 adsorbents showed a high adsorbing activity for endotoxins which had an ionic strength of μ=0.05–1.0 and pH 5.0–9.0. The endotoxin-adsorbing capacity per millitre of the wet adsorbent increased from 0.40 to 1.35 mg (E. coli O111: B4 LPS) at μ=0.2 and pH 7.0 while the aminogroup content of the adsorbent increased from 0.8 to 3.5 meq g−1. The PMLG-NH2-3.5 has an amino-group content of 3.5 meq g−1. This column packing selectively adsorbed endotoxins, without loss of the protein, from a γ-globulin or cytochromec solution which contained endotoxins at μ=0.05 and pH 7.0. On the other hand, when bovine serum albumin (BSA) was present in solution with endotoxins, both the endotoxins and the BSA were adsorbed by the column. The BSA-adsorbing activity increased with increasing amino-group content of the adsorbent. However, this undesirable adsorption was suppressed with increasing ionic strength of the buffer. As a result, when the packing which had an amino-group content of 1.5 meg g−1 was used in conditions of μ=0.2 and pH 7.0, the endotoxins were removed from a BSA-containing solution without affecting the recovery of the BSA.
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  • 3
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    Chromatographia 40 (1995), S. 51-57 
    ISSN: 1612-1112
    Keywords: Column electrophoresis ; Column liquid chromatography ; Phenolic lignin degradation compounds ; Sugar degradation products ; Quantitative analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method for the quantitative analysis of phenolic lignin degradation products by capillary electrophoresis (CE) with on-column UV detection has been developed. The liquid biomass solutions contain low molecular hemicellulosic sugars and phenolic lignin degradation products with various degrees of polymerization. Special attention has been paid to the monomeric phenolic components of lignin degradation fragments, e.g. derivatives of phenolic acids, aldehydes, and alcohols. Uncoated fused silica capillaries and borate-phosphate buffer systems at moderate pH conditions were used in order to separate the compounds of interest. To provide validation of the method, the same samples were analyzed independently by HPLC using gradient elution on a RP-C18 column. As sugar degradation fragment, furan-2-carboxylic acid was detected.
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  • 4
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    Springer
    Chromatographia 40 (1995), S. 85-90 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Phenolic compounds ; Ion-pair solid phase extraction ; On-line trace enrichment
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two packing materials, C18 and PLRP-S, are studied for on-line trace enrichment of phenolic compounds in water. Various precolumns of different internal diameter are also tested and the addition of an ion-pair reagent to increase retention and thus, breakthrough volumes of phenolic compounds, is studied. Best results are obtained when a PLRP-S precolumn is coupled on-line with a C18 analytical column and DAD detector. Addition of TBA considerably increases breakthrough volumes. In contrast, when a C18 precolumn is used, breakthrough volumes are lower and it is impossible to determine TCP and PCP, under the experimental conditions used, because of interference of other nonpolar compounds in the samples. The performance of the system is evaluated with river and tap water and the preconcentration of 10 ml of sample in a PLRP-S precolumn involves a linear range between 1 μg 1−1 and 20 μl−1 and limits of determination between 0.5 μg l−1 and 1 μg l−1 are obtained.
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  • 5
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    Chromatographia 40 (1995), S. 631-637 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Trace analysis ; Pesticides in tap water ; Aromatic sulphonates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Methodology and instrumentation are described which allow chromatographic screening of water samples under substantially simplified conditions and at reduced cost. A single column is used to accomplish sample extraction, trace enrichment, and separation. The performance of such a system is demonstrated, and the results compared with conventionally used concepts.
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  • 6
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Transchelation ; Zinc pyrithione and related compounds ; Antidandruff formulations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An analytical procedure has been developed for the determination of zinc pyrithione in antidandruff formulations. Zinc pyrithione was converted into a stable copper complex and then analysed by reversed-phase HPLC. The proposed method allows the separation of the analyte from related pyrithiones and therefore is able to verify the compliance of cosmetic preparations with current legislation.
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  • 7
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Benzodiazepines ; Solvent effects ; ACN clusters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two different methods were used to determine the separation factor α at different temperatures and the Gibbs-Helmholtz parameters (Δ(ΔH), Δ(ΔS)) of two adjacent benzodiazepines on a chromatogram were obtained from plots of lnα versus 1/T. We first studied each factor (fraction of water ϕ in the ACN/water mixture and column temperatureT), which controls the retention mechanism, and then we examined the simultaneous variation of all these factors. The changes in Δ(ΔH) and Δ(ΔS) in relation to a volume fraction of water ϕ in an ACN/water mixture were examined. In the ACN/water system, Δ(ΔH) was fairly constant in the acetonitrile region of ϕ≤0.52 and appears to be a roughly linear function of ϕ for ϕ≥0.52. In this system Δ(ΔS) is approximately a parabolic function of ϕ with an optimum at ϕ≅0.52. The retention mechanism of ten benzodiazepines was found to be significantly different in the methanol/water and ACN/water mixtures. The separation optimization of these ten benzodiazepines was then considered. A fraction of water of 0.43 in the ACN/water mixture and a column temperature of 44°C gave the most efficient separation conditions in the ACN/water mixture.
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  • 8
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polyurethane degradation products ; 2,4- and 2,6-toluendiamine ; Urine analysis ; Breast implants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A reversed-phase HPLC method has been developed for the urinary determination of mutagenic 2,4- and 2,6-toluendiamines. These amines are degradation products of polyurethane, a material used to cover textured silicone breast implants. FMOC-Cl was used as fluorescent derivatising agent in order to obtain a limit of detection of 15 ng/ml in urine. Pre-treatment of urine samples was by liquid/liquid extraction and urine specimens of patients after surgury were analysed.
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  • 9
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    Chromatographia 41 (1995), S. 657-660 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polyphenols ; Flavonoids ; Phenolic acids and aldehydes ; Eucalyptus spp.
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Standards of the polyphenols occurring in wood, bark and leaf extracts ofEucalyptus spp. (i.e. flavonoids and phenolic acids and aldehydes) have been analyzed by HPLC using reversed phase columns, gradient elution and diode-array detection. The conditions used are reported.
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  • 10
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    Chromatographia 40 (1995), S. 657-661 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed phases ; Polyencapsulated silica ; Polyacrylates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary By copolymerization of silica modified with vinyl groups and acrylic acid esters in suspension highly efficient, polymeric-encapsulated stationary-phases can be prepared. The suspending liquid has to be selected such that the monomers are at least partially adsorbed on the surface and the polymer formed does not precipitate. Under these conditions stationary phases capable of speedy mass transfer can be prepared, where the reduced plate heights are between 2 and 3. The silica surface shielding is optimized so that basic and acidic solutes elute with symmetrical peak.
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  • 11
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral resolution of amino acids ; Pre-column derivatization ; Fluorescent chiral tagging reagents ; Stereochemical purity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Derivatization of amino acid enantiomers with fluorescent chiral Edman-type reagents, 4-(3-isothiocyanatopyrrolidin-1-yl)-7-nitro-2,1,3-benzoxadiazole [R(−)- and S(+)-NBD-PyNCS] and 4-(3-isothiocyanatopyrrolidin-1-yl)-7-(N,N-dimethylaminosulfonyl)-2,1,3-benzoxadiazole [R(−)-and S(+)-DBD-PyNCS], yields corresponding diastereomers separable by reversed-phase HPLC on normal achiral columns. The resolved diastereomers were detected fluorometrically at 530 nm with excitation at 490 nm for the NBD-PyNCS derivatives and at 560 nm with excitation at 450 nm for those derived from DBD-PyNCS reagents. This HPLC-derivatization method was used for evaluation of stereochemical purity for some synthetic commercial peptides. The enantioanalysis was reliable down to 0.05% racemization of the amino acid residues and a quantity of 100 μg peptide sample was usually enough for the analysis. Two acid hydrolysis methods, i.e. the standard procedure with constant-boiling hydrochloric acid (HCl) and a rapid vapor-phase procedure with HCl-trifluoroacetic acid (TFA) mixture, were compared. The later was found to be unsuitable owing to increased racemization of the amino acid residues during the hydrolysis. Judging from the results obtained for proline and leucine residues, most of the tested peptides including biologically active peptides, such as neurotensin, [d-Ala2,d-Leu5]-enkepharin and morphine tolerance peptide, possessed stereochemical purities higher than 98%. Influence of structural features of the peptides on the racemization of the amino acid residues was found to be significant.
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  • 12
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Mass spectrometric detection ; Fast atom bombardment ionization ; Serum bile acid ; Rat bile
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In order to analyse bile acids in biological matrices, e.g. rat bile and human serum, high performance liquid chromatography (HPLC) was coupled to continuous-flow fast atom bombardment mass spectrometry (CFFAB-MS). A gradient elution system which had already proved to be well suited for the quantitative determination of conjugated bile acids in bile was modified to allow HPLC-CFFAB-MS-coupling. Due to the sensitivity of this coupling method it is possible to obtain more information about the biliary bile acid pattern and species-specific secondary bile acids. Furthermore, we were able to identify obviously unknown bile acid species in rat bile which most likely classify as mono-oxo and di-oxo-taurocholates (MW 513 Da, 511 Da) and mono-oxo-glycocholates (MW 463 Da). In the present study we show that using this system it is possible to determine both conjugated and unconjugated as well as sulfated bile acids, without time consuming group separation and derivatization, from rat bile and human serum. In addition, it is suggested that the method presented here should be considered for use in routine analysis.
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  • 13
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fluorescence enhancement ; Bovine serum albumin ; Dansylamino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The effects of acetonitrile and bovine serum albumin (BSA) concentrations on the signal intensity and retention behavior of dansylamino acids have been examined by using γ-cyclodextrin-bonded silica gel as the stationary phase in microcolumn liquid chromatography. Fluorescence intensities of dansylamino acids were enhanced by BSA as a mobile phase additive, e.g., detection limits of dansyl derivatives of L-Ala and L-Phe were improved by a factor of 12–18.
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  • 14
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micellar liquid phases ; Octanol-water partition coefficient ; Benzene and naphthalene derivatives
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary It is shown that the logarithm of the capacity factor (log k′) for fifteen benzene and naphthalene derivatives in micellar liquid chromatography with forty nine different mobile phases generally correlates better with the logarithm of the octanol-water partition coefficient (log Pow) than the capacity factor (k′). Optimum conditions are established to obtain the best linear correlations of log k′-log Pow.
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  • 15
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Photolysis ; Electrochemical detection ; Drugs with chlorinated aromatic rings
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Pharmaceuticals containing a thiazide ring or chlorinated aromatic ring were investigated with respect to enhanced selectivity in determination. Oxidative electrochemical detection coupled with HPLC was used to study the influence of the pH of the mobile phase under conditions of photolysis. To cover a pH range 3.9–12, the employment of a polymer column stable in alkaline media was necessary. The method offers the great advantage of derivatization without chemicals at low operating potentials, thereby providing high selectivity.
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  • 16
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    Chromatographia 40 (1995), S. 296-302 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Structural isomer separation ; Cyclodextrin ; Polymers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Several β-cyclodextrin (CD)-bonded stationary phases for high performance liquid chromatography (HPLC) were prepared, based on silica beads coated with a poly(alkylamine), [poly(ethyleneimine)(PEI)]. In order to obtain stationary phases with a high content of CD and maximum accessibility of the CD cavity, the functionalization was carried out after the coating, using the mono-tosyl derivative of CD as the intermediate. The ability of these supports to separate ortho, meta and para isomers of some disubstituted benzene derivatives was examined. The contribution of the amino groups of the polymer and of the CD cavity to the separation process is discussed. The resolution is mainly based on the difference in the stability of the complexes of the various isomers with CD. The influence of the amount of CD on the height of the theoretical plate is also studied.
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  • 17
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Reversed phase ; Polystyrene ; Pellicular ; Ultra high molecular mass
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Ultra high molecular mass (〉 7 million dalton) polystyrenes are prone to degradation in size exclusion chromatography. In gradient elution reversed phase HPLC they do not elute visibly on small particle size porous supports. However, large diameter C18 pellicular particles were successfully employed for reversed phase study of ultra high molecular mass (15 million dalton) polystyrenes without polymer degradation during elution. Although retention for the lower molecular mass polystyrenes was lower than on small diameter porous particles, the medium high molecular mass polystyrenes (0.5–1 million dalton) showed similar retention. The addition of small diameter porous particles in small quantities, to the large diameter pellicular particles, increased the amount of retention of the low molecular mass polystyrenes without affecting the higher molecular mass polystyrenes.
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  • 18
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Methyl ethyl ketone in urine ; Derivatization ; 3-Methyl-2-benzothiazolinone hydrazone ; Comparison with GC-MS
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A HPLC method for the determination of methyl ethyl ketone (MEK) in urine after derivatization with 3-methyl-2-benzothiazolinone hydrazone is proposed. The calibration curve for the ketone was linear, ranging between 0.23–10 mg/L, with a detection limit of 0.025 mg/L. The results were compared to those obtained by GC-MS, coupled to the headspace technique. MEK derivatization and the derivative purification processes were verified with respect to the main variables such as reaction temperature, reagent concentration, probable interferences and enrichment phase. The method is simple and reliable and shows a good sensitivity.
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  • 19
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    Chromatographia 40 (1995), S. 382-386 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Sulfonamides in foodstuffs ; Honey ; Milk ; Eggs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A procedure for the simultaneous determination of several sulfonamides in different foods, such as honey, milk and eggs is proposed. The analysis is carried out using reversed phase liquid chromatography with spectrophotometric detection. Optimization of the mobile phase led to good separation and a short analysis time when an initial isocratic step with a 3∶97 acetonitrile: water mixture was used for 5 minutes, followed by a linear gradient up to a 40∶60 mixture over 15 min. The proposed method is suitable for routine quality control analysis to ensure the absence of sulfonamides in foods. Recovery studies yielded good results for all food samples because there were no interferences from the matrices.
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  • 20
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    Chromatographia 40 (1995), S. 411-416 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Particle beam LC/MS interface ; Capillary columns for LC ; Mycotoxins ; Peanut meal
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new method for the analysis of aflatoxins in food extracts, based on liquid chromatography/mass spectrometry interfacing, is presented. The chromatographic separation was performed with a reversed phase packed capillary column coupled with a modified particle beam interface capable of handling microliter per minute flow rates. This system allows higher overall sensitivity and easier operation procedures. The method has proved to be particularly suitable for the analysis of the toxins in very complex matrices. The specificity of electron impact ionization allowed positive identification of the aflatoxins with an excellent response linearity for accurate quantitation.
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  • 21
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thin-layer chromatography ; Reversed phase ; 2-benzoylbenzoic acids ; Anionic and cationic counter ions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The 2-benzoylbenzoic acid series was investigated by reversed-phase, high-performance, thin-layer and column chromatography using various alkylammonium salts and di(2-ethylhexyl)orthophosphoric acid as polar associating reagents. The effects of the individual substituents on retention were quantified by Δlog k′ and ΔRM values. The compounds investigated differing in molecular structure (hydrophilic and hydrophobic substituents) commonly occurring groups in drugs and biologically active substances provide information on molecular interaction in these ion-pair systems. The combined effects on retention of organic modifier and ion-pair reagent concentration were investigated.
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  • 22
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Two-dimensional separation ; D- and L-amino acids ; Enantioseperation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A two-dimensional, column liquid chromatographic system is used for the determination of the D- and L-enantiomers of amino acids in biological samples. Separation of the amino acids is first on ion-exchange column by gradient elution with a sodium citratesodium chloride buffer. Enantioseparation is by subsequent injection of 3 μl heart-cuts of the individual amino acids onto a second column with a chiral crown ether stationary phase. Finally, fluorescence detection is after post-column labelling of the amino acids using ano-phthalaldehyde-2-mercaptoethanol reagent solution. The high separation power and selectivity of the system allow processing of complex samples with hardly any additional treatment and the determination of small quantities of D-amino acids in the presence of excess L-form. Applicability of the system is illustrated by the determination of D- and L-aspartate, serine, glutamate and alanine in various complex biological samples, such as protein hydrolysates, urine and biotechnological and food samples. Data are given on detectability, repeatability and linearity.
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  • 23
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion pair LC ; Sweeteners, preservatives and antioxidants ; Food additive analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A paired-ion, reversed-phase high-performance liquid chromatographic method was developed for the simultaneous determination of sweeteners (dulcin, saccharin-Na and acesulfame-K), preservatives (sodium dehydroacetate, sorbic acid, salicyclic acid, benzoic acid, succinic acid, methyl-para-hydroxybenzoic acid, ethylpara-hydroxybenzoic acid, n-propyl-para-hydroxybenzoic acid, isopropyl-para-hydroxybenzoic acid, n-butyl-para-hydroxybenzoic acid, and isobutyl-para-hydroxybenzoic acid), and antioxidants (3-tertiary-butyl-4-hydroxyanisole and tertiary-butyl-hydroquinone). A mobile phase of acetonitrile-50 mM aqueous α-hydroxy-isobutyric acid solution (pH 4.5) (2.2 ∶ 3.4 or 2.4 ∶ 3.6, v/v) containing 2.5 mM hexadecyltrimethylammonium bromide and a C18 column with a flow rate at 1.0 mL/min and detection at 233 nm were used. This method was found to be very reproducible with detection limits ranged from 0.15 to 3.00 μg. The retention factor (k) of each additive could be affected by concentrations of hexadecyltrimethylammonium bromide and α-hydroxyisobutyric acid, and pH and ratio of mobile phase. The presence of additives in some food samples was determined.
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  • 24
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Limit of detection ; Precision ; Uncertainty prediction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The precision of integration over noisy instrumental output for quantitative analysis is studied. A probability theory is developed to predict the relative standard deviation (RSD) of integration results over an integration domain from one-point integation (peak height measurement) to entire area integration in HPLC. Common integration modes of horizontal zero line and oblique zero line are taken into account, but no peak overlap is assumed. The question of the analytical superiority of peak height measurement or integration for quantitation is answered. In the HPLC apparatus used, the minimum RSD of measurements is found in the integration domain of ca. ±0.5 σ for analytes [peaks are approximated by the Gaussian signal of width, σ (standard deviation)]. The RSD of integration measurements is also shown to depend on the stochastic properties of back-ground noise (uncorrelated noise and correlated 1/f type noise). The theoretical conclusion is verified by Monte Carlo simulation and HPLC experiments for some aromatic compounds.
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  • 25
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion-pair and GPC separations ; Amoxicillin oligomers ; β-Lactam ring polymers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Polymeric substances formed from concentrated sodium amoxicillin in an aqueous solution have been separated using two high-performance liquid chromatographic methods. We used a C18 reversed-phase column with tetrabutylammonium chloride as an ion-pairing agent with an acetonitrile gradient and a TSKgel G2500PWxl column with water as the solvent for gel permeation chromatography. The separated materials, ranging in size from the monomer to the tetramer, have been characterized by functional-group chemical analysis, while the identification of the piperazine-2,5-dione was done using a pure standard. A greater number of peaks which were also better defined were obtained using the ion-pair reversed-phase method, and open and closed beta-lactam ring polymer forms could be distinguished. Using the gel permeation method, only a few monomer, piperazine-2,5-dione, dimer, trimer and combined amoxicillin trimer and tetramer peaks were obtained with water, although those obtained were quite well defined. The data on the time-course of formation of the oligomers and the amoxicillin degradation product were virtually identical by both methods.
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  • 26
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; On-column fluorimetric detection ; Gradient elution ; Dansyl amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Fluorimetric detection in the presence of a stationary phase has been applied to gradient elution of dansyl amino acids in liquid chromatography. A 1.5 mm ID quartz tube packed with the same materials as the separation column was employed for the flow cell. Conventional-size columns were employed. The peak height of analytes increased with increasing retention owing to focusing and environmental effects of the stationary phase, leading to improvements in sensitivity, which was pronounced for analytes eluting late. The lower the gradient, the larger the improvement in sensitivity achieved. Detection limits were improved by a factor of up to 5.1 by fluorimetric detection using the packed flow cell, compared with those achieved using a common empty flow cell.
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  • 27
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; LC-MS ; Cinchona alkaloids ; New column packing materials
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A major problem in the HPLC analysis of alkaloids is the poor peak shape and consequently low resolution, due to the interactions of the basic alkaloids with the residual acidic silanol groups of most reversed phase materials. The performance of new packing materials specially designed for the separation of basic compounds has been studied using mobile phases without the special additives commonly applied in the analysis of alkaloids. Strongly basic Cinchona alkaloids were used as test compounds. Retention characteristics and selectivities of each material were studied, after mobile phase optimisation for the column. The influence of the major factors (nature and content of the organic modifier, pH value, salt concentration) affecting resolution was studied. The mobile phases were chosen so that they could be used in thermospray LC-MS. The addition of salts to the mobile phase improves separation but in general the modification of the mobile phase gave little change in selectivity. The performance of silicabased C18 material proved superior to the polymer materials tested.
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  • 28
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Diode-array detection ; Retinol acetate ; Pharmaceutical preparations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A very simple high-performance liquid chromatographic method for determination of Vitamin A in pharmaceutical preparations without the need for saponification was developed. A reversed-phase (Nova-Pack C18, 4 μm) column was used with a mobile phase of acetonitrile-tetrahydrofuran-water (55∶37∶8) and a flowrate of 1.5 ml/min. Sample treatment only consisted of the extraction of retinol acetate content from capsules or tablets with methanol. Total extraction was achieved by shaking vigorously with the aid of magnetic stirring for three hours at room temperature. No change of solvent is necessary to introduce the sample in the chromatographic system. This method is suitable for routine quantification of Vitamin A.
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  • 29
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    Chromatographia 40 (1995), S. 193-196 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemometric methodology ; Elution order ; Simplex optimization ; Benzodiazepines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Using a rapid chemometric methodology to determine the separation factor, α, at different temperatures, Gibbs Helmholtz parameters (Δ (ΔH), Δ (ΔS), Δ (ΔG)) of two adjacent benodiazepines on a chromatogram were obtained from ln α versus T−1 plots. A temperature dependent reversal of the elution order was studied and the mobile phase composition and column temperature were optimized to obtain the best separation. A flow rate of 0.80 ml min−1 with 52.6% methanol in the methanol-water mixture and a column temperature of 48°C gave the most efficient separation of ten benzodiazepines.
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  • 30
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    Chromatographia 40 (1995), S. 237-246 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Mixed mode stationary phases ; Indirect photometric and fluorometric detection ; Conductimetric detection ; Alkyl-sulphates, and sulphonat-phosphates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Separation of three classes of anionic surfactants (alkyl sulfates, alkanesulfonates, and alkyl phosphates) are achieved on a mixed-mode reversed phase (RP) phenyl/-anion exchange column using a naphthalenetrisulfonate (NTS)-acetonitrile (ACN) mobile phase via indirect photometric, indirect fluorometric, direct or indirect conductivity detection. Mixtures of C5−C18 sulfates, C6−C18 sulfonates, and C1−C4 phosphates (mono- and di-ester) can be separated in less than 20, 24, and 20 min respectively. Although hydrophobic effects are more pronounced in mixed-mode chromatography, equivalent-per-equivalent exchange of analysis and eluent ion is still required for sensitive indirect photometric, fluorometric, or conductivity detection. The detection limits of alkyl sulfates and alkanesulfonates are in the range of 3–15 pmoles which are at least an order of magnitude better than suppressed conductivity detection. The determination of surfactants in a variety of real samples is also presented.
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  • 31
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    Chromatographia 40 (1995), S. 287-295 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Capillary zone electrophoresis ; Enantioseparation ; Carnitine ; Derivatization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Carnitine is an essential component in tissues of animals, higher plants and many microorganisms. Whereas the L-carnitine enantiomer plays an important role in the metabolism of long chain fatty acids, D-carnitine has a considerable toxic influence on biochemical processes. The analytical separation of D-and L-carnitine depends upon derivatization with UV-or fluorescently active substances, e.g. FMOC and (+)/(−)-FLEC. The separation of diastereomeric (+)- and (−)-FLEC carnitine esters was performed successfully with capillary zone electrophoresis (CZE) and HPLC, after optimization of the derivatization process and of the composition and pH of the buffer, using UV- and fluorescence detection. With HPLC separation a detection limit of the carnitine esters of 5 μmol/l when using fluorescence detection was achieved. With both separation systems baseline resolution and short analysis times could be obtained. The enantiomeric FMOC derivatives could be separated using the electrophoretic system and acidic buffers with high concentrations of an osmotic flow modifier together with γ-cyclodextrine as chiral selector. The applicability of the optimized separation conditions are demonstrated in the analysis of agar culture medium inoculated withPseudomonas putida and of pharmaceutical formulations. In all samples very low amounts of D- or L-carnitine could be determined in the presence of the other enantiomeric form. Problems caused by the impurity of the carnitine standards or the derivatization agent (+)/(−)-FLEC are discussed.
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  • 32
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fullerenes ; Retention vs NMR spectra ; C18 phases ; Low temperature separations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The temperature effect on the retention of fullerenes in the range 80°C to −70°C in liquid chromatography (LC) has been examined using octadecylsilica stationary phases (ODS). It has been found that the maximum retention temperature lies around −10°C with a highly carbon loaded ODS phase. Solid state CPMAS NMR measurements on the stationary phases indicated that the relaxation time at the 30 ppm methylene signal changes with the temperature and has a minimum relaxation time at the temperature which closely matches the maximum retention temperature observed in chromatography. The interpretation of both NMR spectroscopic and LC chromatographic data are discussed.
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  • 33
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    Chromatographia 40 (1995), S. 601-606 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Amino acid analysis ; Chirality ; Diastereoisomers ; Dipeptides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Using a robotic autosampler, free DL-amino acids were derivatized with highly reactive, urethane-protected, L-α-amino acidN-carboxyanhydrides (NACs) with structures: Boc-Phe-NCA, Boc-Asn(Trt)-NCA, Fmoc-Lys(Boc)-NCA, Fmoc-Met-NCA, Fmoc-Ala-NCA, Z-Ala-NCA, Z-Val-NCA and Z-Leu-NCA (Boc=tert-butyloxycarbonyl, Trt=trityl, Fmoc=9-(fluor-enylmethyl)oxycarbonyl, Z=benzyloxycarbonyl). Using sodium borate buffer and acetonitrile solvent, derivatization was complete in 3.5 min at room temperature. By selection of an appropriate reagent, the resulting diastereomeric,N-protected dipeptides were separated on an octylsilica stationary phase using mixtures of sodium acetate buffer and acetonitrile as eluents.
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  • 34
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Dihydroxyacetone ; 2,4-dinitrophenylhydrazine ; Tanning creams
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid and simple HPLC method for the identification and determination of dihydroxyacetone, a tanning agent widely used in a variety of preparations, is presented. The method consists of the analysis of the formulated products after a derivatization reaction which enhances the response and the detection limit of the chromatographic analysis. The characterization and the elucidation of the spacial geometry of the synthesized derivative are described.
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  • 35
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    Chromatographia 41 (1995), S. 431-434 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Thin-layer chromatography ; Patent Blue V in cheese
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The HPLC method developed for the analysis of the dye Patent Blue V in extracts from cheese is sufficiently sensitive to detect and measure concentrations above 0.1 ppm with a standard deviation of 3%. The extraction procedure described gives a recovery from cheese of about 80%. The method has been applied to commercial samples of cheese and a concentration of the dye of about 0.12 ppm was measured in one case.
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  • 36
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micellar liquid chromatography ; Neural networks ; Retention modelling
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Multi-layer feed-forward neural networks trained with an error back-propagation algorithm have been used to model retention behaviour of liquid chromatography as a function of the composition of the mobile phases. Conventional hydro-organic and micellar mobile phases were considered. Accurate retention modelling and prediction have been achieved using mobile phases defined by two, three and four parameters. With micellar mobile phases, the parameters involved included the concentrations of surfactant and organic modifier, pH and temperature. It is shown that neural networks provide a competitive tool to model varied inherent nonlinear relationships of retention behaviour with respect to the mobile phase parameters. The soft models defined by the weights of the networks are capable of accommodating all types of linear and nonlinear relationships, neural networks being specially useful when the relationships between retention behaviour and the mobile phase parameters are unknown. However, to train neural networks more experimental points than with hard-modelling methods are required, hence the use of the networks is recommended only for those cases where adequate theoretical or empirical models do not exist.
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  • 37
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Diltiazem hydrochloride stereoisomers ; Chiralcel OF ; Chiral inversion ; Epimerization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The simultaneous stereospecific assay of four stereoisomers of diltiazem hydrochloride in bulk drug and aqueous solution was developed using HPLC on a Chiralcel OF column. The four isomers were quantitated with good precision by the internal standard method. The chiral inversion of (+)-cis-diltiazem hydrochloride in vitro, stability of its (2S, 3S) configuration in the solid and aqueous states was examined by HPLC. Chiral inversion of (+)-cis-diltiazem hydrochloride was not observed in the solid state, and its (2S, 3S) configuration was stable to heat, humidity and light. Chiral inversion of (+)-cis-diltiazem hydrochloride (2S, 3S) was observed in aqueous solution under UV, but not in aqueous solution stored at 80°C for 5h nor under visible light for 10 h. The (+)-cis-diltiazem hydrochloride (2S, 3S) epimerized to (+)-trans-diltiazem hydrochloride (2R, 3S) with a half-life of 5h in aqueous solution under UV but the reverse chiral inversion of (+)-trans-diltiazem hydrochloride (2R, 3S) to (+)-cis-diltiazem hydrochloride (2S, 3S) was not observed.
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  • 38
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    Chromatographia 41 (1995), S. 488-491 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Acetonitrile disposal ; Acetonitrile hydrolysis ; Degradation kinetics ; Waste solvent management
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Acetonitrile is one of the most frequently used solvents in column liquid chromatography. Because of its toxicity, safe disposal of the waste solvent is essential. Combustion in a hazardous waste plant, if available, is recommended. Otherwise the waste can be degraded in the laboratory to acetic acid and ammonia by treatment with sodium hydroxide. The addition of hydrogen peroxide is not necessary. The waste needs to be diluted to 10% acetonitrile in water in order to prevent the formation of a two-phase system on addition of concentrated sodium hydroxide. This reagent must be added in excess; 2.5 mols of sodium hydroxide per mol of acetonitrile are recommended. It was found that the kinetics are of second order, with an activation energy of 89 kJ mol−1 and a frequency factor of 9×109. Therefore even at room temperature degradation is possible, although a hydrolysis time of approximately 15 days is needed under these conditions. At 80°C, where refluxing is not necessary, hydrolysis is complete after, e.g., 2 h, depending on the amount of sodium hydroxide added.
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  • 39
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion-pair LC ; 5-Sulphoquinoline-8-ol ; Metal complexes
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    Topics: Chemistry and Pharmacology
    Notes: Summary The reversed-phase ion-pair liquid chromatographic behaviour of several metal complexes with 5-sulphoquinoline-8-ol (HQS) on an octadecyl-modified silica column was investigated by using a fluorescence detector. The aluminum complex gave two peaks on the chromatograms when eluents containing phosphate buffer were used. The effects of the pH of the eluent, HQS concentration, the nature of anions in the eluent, and the column temperature on the retention behaviour of the aluminum complex are discussed on the basis of the equilibria and the kinetics of the complexation of the aluminum ion with HQS and anions in the eluent. The equilibrium constant for the interconversion reaction between the two Al(III)-HQS species which correspond to the two peaks observed and the second stepwise formation constant for the Zn(II)-HQS complex were evaluated from the HPLC data obtained.
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  • 40
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fluorescamine derivatives ; Aniline and aniline derivatives ; Environmental waters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Fluorescamine (fluram) has been used as a fluorogenic compound for pre-column derivatization of aniline and some derivatives. Anilines were derivatized with fluram in citrate buffer media (pH 5.5) to form pyrrolinones. The highly fluorescence pyrrolinones were isolated and pre-concentrated by solid phase extraction. A reversed phase, Spherisorb RP-8 column and tetrahydrofuran: water:formic acid (42∶56∶2) mobile phase was used for separation. Detection method was by a sensitive fluorimetric method and quantitation was at 395 and 495 nm. The various parameters such as reaction conditions between anilines and fluram, solid phase extraction and chromatographic separation were optimized. Calibrations were linear over the range considered with excellent correlation coefficients (r〉0.999). Relative standard deviations are less than 2.5% and detection limits for aniline,p-toluidine, 4-chloroaniline and 4-bromoaniline were 6, 30, 6 and 8 ng L−1, respectively. This method has been used successfully for the determination of anilines in environmental waters.
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  • 41
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Nauclea diderrichii (de Wild) Merr ; Saponins ; Alkaloid glycoside ; Chrysanthelline A
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    Topics: Chemistry and Pharmacology
    Notes: Summary A reversed-phase HPLC determination of 11 saponins and an alkaloid glycoside inNauclea diderrichii bark is described. Quantitative analysis of quinovic acid 3-O-α-L-rhamnopyranoside which is one of the main saponins was determined, using Chrysanthelline A as internal standard. The complete separation was achieved in 47 minutes. The method of quantification was validated.
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  • 42
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column liquid chromatography ; Polychlorinated biphenyls ; Cod liver oil
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    Topics: Chemistry and Pharmacology
    Notes: Summary By application of a chromatographic column filled with Supelclean ENVI-Carb/Celite and elution with three solvents of different polarity three PCB fractions were obtained. Fraction A contained poly-ortho PCBs, Fraction B mono-ortho PCBs, and Fraction C non-ortho PCBs. The Supelclean ENVI-Carb/Celite column was used in combination with a sample preparation procedure for pre-cleaning of acid-stable chlorinated hydrocarbons such as DDT and its metabolites, HCH isomers, and regulation-relevant PCB congeners. The method was optimized using standard solutions of 55 PCB congeners, 8 chlorinated pesticides and contaminated cod liver oil samples. The influence of traces of remaining matrix on the elution profile of the organochlorine compounds on Supelclean ENVI-Carb/Celite was observed. Quantitation was carried out by GC-ECD with fused silica capillary columns of different polarity.
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  • 43
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Capillary electrophoresis ; Enantiomer separation ; Trimetoquinol ; Denopamine ; Timepidium
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two methods for the direct separation of the enantiomers of trimetoquinol hydrochloride, denopamine and timepidium bromide were investigated, namely capillary zone electrophoresis (CZE) using cyclodextrins (CDs) (CD-CZE) and high-performance liquid chromatography (HPLC) using chiral stationary phases (CSPs). By CZE, separation of the enantiomers of trimetoquinol was successfully achieved when using β-cyclodextrin (β-CD), heptakis(2,6-di-0-methyl)-β-cyclodextrin (DM-β-CD) and β-CD polymer, but direct HPLC separation of the enantiomers was not successful. The enantiomers of denopamine were successfully separated by both CZE, employing DM-β-CD under acidic conditions, and HPLC, with cyclodextrin immobilized CSPs (CD-CSPs). Timepidium bromide, which is a racemic drug, was successfully enantioseparated by both CD-CZE and HPLC with CD-CSPs. The CD-CZE mode was selected as the optical purity testing method for trimetoquinol and denopamine because of the superiority of capillary electrophoretic (CE) techniques. Method validation results obtained clearly show that the CE method would be useful as an quality control method for assessing the optical purity of the drugs.
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  • 44
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Microbore columns ; Column packing ; Slurry viscosity ; Surfactants
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    Topics: Chemistry and Pharmacology
    Notes: Summary The kinematic viscosity of the slurry used for the packing of microbore columns for liquid chromatography has been correlated with the packing efficiency. The columns were packed into polyetheretherketone (PEEK) tubing with an internal diameter of 0.5 mm using unbonded and bonded spherical silica gels under constant pressure conditions. Higher efficiencies were obtained using slurries suspended in aqueous solutions of surfactants, such as polyoxyethylene sorbitane monolaurte (Tween-20) and sodium dodecyl sulphate, in comparison with organic solvents usually used for column packing. The concentration dependencies of the relative kinematic viscosities of six slurries were compared using capillary viscometry. The slurries with low relative viscosities possessed rheological properties which enabled high packing densities, typical of a stable dense random packing arrangement, to be obtained at moderate packing pressures. The unusually low relative viscosities are discussed in terms of a “porous hydrodynamic bearing” model. The techniques used should also be generally applicable to the slurry packing of conventional columns.
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  • 45
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Preservatives-antioxidants ; Eluent pH ; Retention and separation factors
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In this paper the dependence of eluent pH on the efficiency of separation in RP-HPLC is described. Preservatives-antioxidants, esters ofp-hydroxybenzoic acid (methyl, ethyl, propyl and butyl parabens), sorbic acid, butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT), propyl gallate (PG) and L-ascorbic acid (Vitamine C) were investigated by reversed-phase high-performance liquid chromatography, utilising isocratic elution with UV detection. The mobile phase composition (methanol-water v/v containing 1% acetic acid), was varied in order to obtain the best separation. For all substances analysed the pH, pKa and the fitted pKa values were calculated in different mixtures of mobile phases using the graphical method of Charlot and Trémillon [1]. The retention factors (k) and the separation factors (α) were also calculated.
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  • 46
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    Chromatographia 40 (1995), S. 680-683 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral stationary phase ; Preparative chromatography ; Benzodiazepines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary High performance liquid chromatography chiral stationary phases based on immobilized proteins are well known and commonly used. This work reports on an evaluation of a Human Serum Albumin stationary phase in the preparative separation of benzodiazepines.
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  • 47
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Isoniazid in milk ; SPE preconcentration ; Diode array UV spectra
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple, fast, accurate and highly sensitive (5 ng/ml) method for the detection of sionicotinic acid hydrazide (isoniazid) in cattle milk is described, based upon an RP-HPLC system, equipped with a C18 column and a UV detector. Milk was deproteinized with trichloroacetic acid and treated with cinnamaldehyde, before being injected into the HPLC system. Preconcentration of samples on an SPE phenyl cartridge allows the sensitivity of the method to be increased to 0.05 ng/ml using a UV detector. The presence of isoniazid can be confirmed at concentrations as low as 0.4 ng/ml, through a diode-array UV spectrum of isoniazid hydrazone. The analytical procedure here described is routinely applied to investigate the illegal administration of isoniazid to cattle, as it provides a means of screening that can be carried out in a very short time.
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  • 48
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micellar liquid phases ; Hybrid mobile phases ; Retention behaviour
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two methods for the description of the retention behaviour of solutes in micellar liquid chromatography are compared. One of them divides the parameter space into triangular subspaces, fitting a different equation in each subspace. The second method makes use of a unique equation, valid in the whole parameter space. In both cases, equations of the type log k=f (μ, ϕ), and 1/k=f (μ, ϕ), (μ and ϕ are the concentration of surfactant and alcohol, respectively), were used to describe the retention. The use of the hyperbolic function, 1/k=c0+c1μ+c3μϕ, to describe the whole parameter space yielded the best prediction. When a small portion of the parameter space was modelled, a simpler hyperbolic function, lacking the μϕ term often led to good results. The logarithmic equations usually gave the poorer predictions.
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  • 49
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; High speed LC ; Pharmaceutical drugs ; Routine analysis ; Fast HPLC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary High performance liquid chromatography (HPLC) is widely used in drug development and quality control. The main objective is to obtain dependable results in the shortest time in order to reduce the time taken to develop drugs and to ensure better quality of the final compound. High speed liquid chromatography (HSLC) helps us to reach this objective. In this paper pratical aspects of HSLC are discussed mainly in terms of instrument requirements and the practical needs of users. Comparison between HPLC and HSLC separations of pharmaceutical preparations are given and discussed. The contribution of HSLC to decrease solvent consumption and consequently analysis cost and its role in reducing environmental pollution, are also mentioned.
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  • 50
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Indirect photometric detection ; Anthraquinone-disulfonate ion ; Inorganic anions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Disodium salts of several anthraquinone-disulfonic acids, which possess large molar absorptivity, were employed as the visualization agent for microcolumn ion chromatography with indirect photometric detection. Detection limits of inorganic anions were improved, e.g., concentration detection limits of chloride, nitrate and sulfate were 0.91–1.6 μmol L−1 at S/N=3, corresponding to mass detection limits of 18–32 fmol. The present system was applied to the determination of inorganic anions in tap water.
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  • 51
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    Chromatographia 40 (1995), S. 404-410 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Solid-phase extraction ; Wine ; Biogenic amines ; Phthalaldehyde
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A suitable method for the determination of 16 biogenic amines in wine has been developed. The method involves clean-up of wine samples using ion-exchange cartridges and a preconcentration step, under controlled vacuum, before derivatization of the amines by treatment with phthalaldehyde (PA) and reversedphase HPLC with gradient elution and fluorimetric detection. Linearity of response was obtained for all the biogenic amines from 100 μg L−1 to mg L−1. Limits of detection for the amines were similar for all PA-derivatives (25–50 μg L−1) and the quantitation limits were about 0.1 mg L−1. After clean-up and preconcentration, the concentration levels increased 10-fold for all amines except putrescine and cadaverine, which gave poor recovery by this method unlike the rest which gave recoveries of almost 90%. The overall process was successfully applied to identify and quantify biogenic amines in several red wines from the Tarragona region.
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  • 52
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Mixed-bed stationary phase ; Anion and cation exchange resins ; Retention mechanism of anions and cations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention mechanism of anions and cations on a mixed-bed column packed with a mixture of strong anion and cation exchange resins has been studied. Organic acids and inorganic anions have showed the same elution behaviour on the mixed-bed column as on a single anion exchange column. In contrast, different elution behaviours for cations have been observed between the mixed-bed column and a single cation exchange column. On the mixed-bed column, cations would be eluted by a mixed retention mechanism. The primary retention mechanism is ion exchange with eluent cation (H+) for all cations. The ion exchange mechanism on the sites occupied by anion exchange groups makes a greater contribution for monovalent cations. A partition mechanism between the stationary phase and mobile phase contributes to the separation of Mg2+ and Ca2+ by forming neutral compounds.
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  • 53
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Open tubular columns ; Cross-linked polyacrylate stationary phases ; Photopolymerization ; PTH-amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Fused silica capillaries with an internal diameter of 5 μm were coated with polyacrylate films containing either alkyl or ether functionalities. Polymer networks were created byin situ photopolymerization of acrylic monomers. Capillaries with phase ratios up to 1.3, having excellent separation efficiencies, could be prepared. The performance of these capillaries was demonstrated by the separation of various solute mixtures. Nineteen phenylthiohydantoin (PTH) amino acid derivatives could be separated in less then 10 minutes when using UV detection. Laser Induced Fluorescence detection was used for the separation of polycyclic aromatic hydrocarbons, dansyl (Dns) derivatized amino acids ando-phthalaldehyde (OPA) derivatized aliphatic amines which could be separated with approximately 310,000 plates in less than 3.5 minutes corresponding to around 1500 plates per second.
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  • 54
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    Chromatographia 41 (1995), S. 178-182 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Solid-phase extraction ; Triazine herbicides ; Milk
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary High-performance liquid chromatography with UV detection was used to determine eight triazine herbicides in milk. Solid-phase extraction was performed using a double trap; first, a nonspecific adsorbent (Carbograph), and then a cation exchanger (SCX). Eluate from the SCX was evaporated to dryness under reduced pressure and redissolved in mobile phase. An aliquot was injected into the chromatography, which was operated isocratically in the reverse-phase mode with UV detection at 225 nm. Analytical recoveries for the eight triazines ranged from 73.0% to 92.4%. The limit of sensitivity of this method was about 0.09 ng mL−1 of milk. The method was validated and evaluated by comparison with a method reported in literature.
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  • 55
    ISSN: 1612-1112
    Keywords: Supercritical fluid extraction ; Column liquid chromatography ; Aromatic compounds on silica
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An SFE-HPLC system has been tested with a simple model aromatic mixture on spiked silica. The spiked silica was extracted with pure CO2 and the extract retained in a trap packed with C18 material. Quantitative separation and reproducity have been investigated and are reported.
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  • 56
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    Chromatographia 41 (1995), S. 445-449 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion chromatography ; Alkylsulphonic acids ; Conductivity detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An ion chromatographic (IC) method has been developed for the separation of alkylsulphonic acid. Two different stationary phases, silica-based and polymer-based ion-exchange resins, were studied using pure ion exchange and/or hydrophobic interaction mechanisms. Correlations between analyte hydrophobicity and eluent polarity were made in order to investigate the possibility of changing the dominant separation mechanism by varying the eluent composition. The alkyl chain lengths of the sulphonic acids analysed ranged from C1 to C9. Detection limits in the submicromolar range were obtained by suppressed conductivity detection.
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  • 57
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polymeric bonded phase ; Anion-exchange chromatography ; Pulsed amperometric detection ; Carbohydrates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This paper reports the results of a study on the use of a new polymer-based, strong anion-exchange, stationary phase for rapid and selective separation of carbohydrates and related compounds by high-pH, anion-exchange chromatography with pulsed amperometric detection. The new adsorbent has been obtained by direct nitration of 2.8 μm, spherical non-porous highly crosslinked, styrene-divinylbenzene copolymer beads, followed by reduction of superficially introduced nitro groups with nascent hydrogen and quaternization of the resultant amino groups with iodomethane. It is reported that by optimizing the ionic strength of the mobile phase, columns packed with the new anion-exchanger can be successfully employed to separate, either in isocratic or gradient elution mode, oligosaccharides, positional isomers of gluco-disaccharides, as well as uronic acids and sugar monophosphates.
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  • 58
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Analytical and preparative scales ; Soybean phospholipids ; Mass detector
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary To enable the study of the functional properties of pure soybean phospholipids, a chromatographic method was developed for the preparative fractionation of soybean lecithin. A coarse and irregularly shaped silica gel was used as the stationary phase, whereas the mobile phase consisted of three mixtures of hexane, 2-propanol and water of increasing polarity. These solvents were included in a step gradient, formed by an isocratic pump connected to a solvent changer. To reduce solvent consumption, the procedure was optimised using a method development column. The solvent program and the sample load were shown to affect mainly the purity and recovery of phosphatidylinositol.
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  • 59
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    Chromatographia 41 (1995), S. 521-526 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Phenolic compounds ; Ion-pair solid phase extraction ; On-line trace enrichment
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Modifying the most common design for the on-line coupling of a precolumn to reversed phase LC with diode array detection has resulted in reduction of the broadening of the peaks which results when the compounds of interest are strongly retained by a highly hydrophobic sorbent. The modification consists of the desorption of the analytes trapped on the precolumn solely by the organic solvent used to modify the solvent strength of the mobile phase. Results obtained using this design were compared with those obtained with the conventional design, with C18 and PLRP-S precolumns. The performance of the system was also tested with a highly cross-linked styrene-divinylbenzene copolymer (ENVI-chrom P) precolumn for the determination of phenolic compounds in real samples. The advantages and disadvantages are discussed. Ion-pair solid phase extraction is used in order to increase the breakthrough volumes of more polar compounds, mainly phenol. The use of the new design enables phenolic compounds to be determined at the low μg L−1 level with limits of detection ranging between 0.1 and 2 μg L−1 in tap water when a 10 mL sample was analyzed.
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  • 60
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    Chromatographia 41 (1995), S. 553-560 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography ; Experimental design ; Modelling
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Experimental Design methodology allows the modelling and optimization of the chromatographic separation of similar pesticides (triazine family) by GC and HPLC. The GC separation of simazin and atrazin is well modelled by a first degree equation, involving injected volume, carrier gas pressure and rising oven temperature. The LC is modelled by a second degree equation, depending on injected volume, eluent flow and composition. These calculated models allow easy optimization of the separations, using isoresponse curves.
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  • 61
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    Chromatographia 41 (1995), S. 573-580 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Mobile phase optimization ; Steroids ; Solvatochromic parameters ; Retention prediction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The proportion of organic modifier and pH of the hydroorganic mobile phase were optimized to separate a series of nine important steroids by LC. It has been shown that linear plots of logk′ against Reichardt'sE T N parameter for the mobile phase is observed over the whole range of compositions of practical importance. Data from these plots summarize an approach for optimization of resolution from only two retention measurements for each compound. pH is shown to be irrelevant. This behaviour could be extrapolated to other steroids and drastically reduce the number of retention values needed for mobile phase optimization for screening analysis of steroids in doping investigations.
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  • 62
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Cation ion-exchange resins ; Lactose, lactulose and galactose
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A strong acid cation-exchange resin, Dowex AG50W-X8 in potassium, calcium or sodium form, with water as eluent, has been used to separate three sugars (lactose, lactulose and galactose). The linearity of lactulose equilibrium isotherms was verified. Thermodynamic and kinetic parameters were thus determined by the moment method. Evaluation of the parameters revealed in this work can be considered as the first step in scaling up the process towards industrial use. On the other hand, the equilibrium stage model, which takes mass transfer resistance into account, is shown to provide a fair representation of the system's behaviour.
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  • 63
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    Chromatographia 40 (1995), S. 9-14 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porous graphite ; Chiral stationary phase ; Copper complexation chromatography ; Amino acids ; Hydroxy acids ; Adsorbed stationary phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new type of chiral stationary phase has been prepared by coating porous graphite with a near-monolayer of an adsorbed enantiomeric modifier which then acts as an adsorbed stationary phase. The most effective modifiers are L- or D-isomers of N-(2-naphthalene-sulphonyl)-phenylalanine (NS-Phe). Conveniently 80% of monolayer coverages, corresponding to 1.2 μmol m−2, are achieved by adsorption of NS-Phe from methanolic solution. Enantiomeric separations by complexation with cupric ion show base-line resolution of α-amino and α-hydroxy acids with separation factors up to 2. Identical separations are achieved with chiral phases made from the L- and D-isomers of NS-Phe except that the elution orders of enantiomers are inverted. Reduced plate heights are around 5 and the adsorbed chiral phases are extremely stable, retention ratios being unchanged after passage of 7000 column volumes of eluent. A mechanism of retention is proposed, which fits the experimental observations.
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  • 64
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Enantioseparation ; ChiralcelR OJ ; Anti-HIV agents ; Thiazolo-benzimidazoles
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A series of enantiomeric 1H,3H-thiazolo[3,4-a] benzimidazoles with anti-HIV activity has been stereospecifically analyzed. The enantiomeric resolution has been carried out by means of an HPLC method using a column of cellulose tris-(4-methyl-phenylbenzoate) ester adsorbed on macroporous silica gel (ChiralcelR OJ).
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  • 65
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Structure vs. retention ; Principal component analysis ; Multiple linear regression ; Molecular descriptors
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The mechanism of the retention in HPLC when using a non-polar solvent with a very low content of polar modifier as mobile phase is outside the scope of the classical interpretations. We have used quantitative structure-retention relationships (QSRR) to interpret the retention of a series of 36 compounds on 18 chromatographic systems (3 stationary phases and 6 mobile phases). Principal Component Analysis (PCA) was used to reduce the complexity of the data and to obtain the most significant axis; molecular modeling (molecular mechanics and molecular orbital calculations) was used to obtain structural information on the solutes, and multiple regression to correlate coordinates and descriptors. We have shown that the coordinates of the solutes on the first PCA axis are related to three molecular descriptors: the calculated logarithm of the partition coefficient in an octanol/water system (Log P), the polarisability (pol) and the energetic level of the highest occupied molecular orbital (HOMO). We have found the same equation with a similar coefficient for the three different stationary phases. These results prove the dominant role of the polar modifier in such chromatographic systems.
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  • 66
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Sugars ; Amperometric detection ; Chemically modified electrodes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A chemically modified electrode was applied as a working electrode for the amperometric detection of sugars in liquid chromatography. A mixture of cuprous oxide and conductive carbon cement was used as electrode material. Cuprous oxide acted as a catalyst for the oxidation of sugars. Cyclic voltammetry was used to examine the oxidation of the sugars at the electrode surface. The stability and sensitivity of a cuprous oxide/conductive carbon cement (20/80 %, w/w) electrode were tested in flow injection analysis experiments. For liquid chromatography, sugars were separated on an ion-exclusion column with 0.01 M H2SO4 as mobile phase. After the separation, 0.2 M NaOH was added post-column and the sugars were determined at 550 mV vs. Ag/AgCl. Calibration was linear in the range of 10−6·10−3 M with limits of detection of approximately 1·10−6M. The application of the modified electrode for the determination of sugars in fruit beverages and dairy products following chromatographic separation is shown.
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  • 67
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    Chromatographia 40 (1995), S. 129-133 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Digalactosyldiacylglycerols ; Solid phase extraction ; Oats ; Experimental design
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A convenient method for the isolation of digalactosyldiacylglycerols from plant material has been developed using solid phase extraction. Commerical cartridges were utilized to prepare 100 mg fractions of galactolipids containing more than 97% of digalactosyldiacylglycerol. The purity of the fractions was monitored by an isocratic normal phase analytical HPLC procedure, which was optimized using factorial design. The optimized system was successfully scaled up to a semi-preparative HPLC system with a capacity of about 10 mg/injection which was used to further purify the digalactosyldiacylglycerol fraction.
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  • 68
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Benzalkonium chloride ; Tramadol ; Ophthalmic solution
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    Topics: Chemistry and Pharmacology
    Notes: Summary A high-performance liquid chromatographic procedure employing ultraviolet detection for the analysis of benzalkonium chloride in 0.5% Tramadol ophthalmic solution is reported. The method requires minimal sample pretreatment and is sensitive, accurate, and reproducible. The peak area versus BAK concentration is linear over the range of 50–150% of its label claim of 0.05 mg/mL. The mean absolute recovery of BAK using the described method is 100.2±1.2%, (mean ±SD, n=10). A stress study with heat, acid, base and UV radiation indicates that the method is stabilityindicating with no interference from drug or degradation products.
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  • 69
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    Chromatographia 40 (1995), S. 204-206 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Stability-indicating method ; 17β-Estradiol-3-phosphate ; Ophthalmic solutions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A reversed-phase high-performance liquid chromatographic (HPLC) procedure using ultra-violet (UV) detection for the analysis of 17β-estradiol-3-phosphate in an ophthalmic solution is reported. The method is selective, accurate, and reproducible. The peak area versus 17β-estradiol-3-phosphate concentration is linear over the range of 50–150% of its label claim of 1.0 mg/mL, with a detection limit of 20 ng/mL. The mean absolute recovery of 17β-estradiol-3-phosphate using the described method is 99.8±0.6% (mean ±SD, n=10). A stress study with heat, acid, base and UV radiation indicates that the method is stability-indicating with no interference from excipients or degradation products.
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  • 70
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column liquid chromatography ; On-line coupling ; Ion-exchange membrane ; Ion-pair reagent
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In order to enable the coupling of reversed-phase liquid chromatography (RPLC) with capillary gas chromatography (GC), the performance of an anion-exchange micromembrane device has been studied to remove the ion-pair reagent methanesulphonic acid from an acetonitrile/water LC eluent. The regenerant in the membrane was tetrabutylammonium hydroxide dissolved in acetonitrile/water, which effects an anion-exchange of methanesulphonate ions for regenerant hydroxide ions. The efficiency of the exchange process was found to be 99.9%. This enabled the direct introduction of the LC eluent, free of ions and with the proper acetonitrile/water ratio, into the GC. The applicability of the on-line LC-micromembrane-GC system has been illustrated for the potential drug eltoprazine, which is quantitatively recovered with a coefficient of variation for standard solutions of 3% at the 150 μg/ml analyte level.
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  • 71
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Optimal mobile phases ; Enantiomer separation ; Pesticide enantiomers
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    Topics: Chemistry and Pharmacology
    Notes: Summary A computer-assisted method is described for optimization of multi-component, mobile phase selection for separating enantiomers of four pesticides in normal-phase HPLC. The method is based on the triangle, solvent-selection concept using a statistical scanning method. The optimization of the separation over the experimental region is based on a special polynomial estimation from seven experimental runs, and resolution (Rs) is used as the selection criterion. Excellent agreement was obtained between predicted and experimental data.
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  • 72
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Multicomponent mobile phases ; Retention prediction ; Binary and multicomponent phases, comparison
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    Topics: Chemistry and Pharmacology
    Notes: Summary Using the concept of an effective concentration a method is proposed for predicting retention in liquid chromatography with multicomponent mobile phases based on experiments with corresponding binary ones. The method is verified for normal and reversed-phase systems with ternary mobile phases and agrees closely with experimental data.
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  • 73
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    Chromatographia 40 (1995), S. 545-549 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fluorimetric detection ; Packed flow cell ; Dansyl amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Fluorimetric detection with a packed flow cell has been applied to dansyl amino acids in liquid chromatography using conventional size columns (4.6 mm ID). The same packing as for the separation column was used in the 6×1.5 mm ID cylindrical flow cell, where analytes were detected in the presence of the stationary phase. Both peak height and peak area of analytes increased with increasing retention owing to focusing and environmental effects of the stationary phase, leading to dramatic improvement in the sensitivity for analytes eluting late. The detection limits for analytes eluting in around 1 h were improved by a factor of 28 compared with those achieved with a normal empty flow cell.
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  • 74
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Solid-phase extraction ; Solvent effects ; Solvation parameter model ; Cyanopropylsiloxane-bonded, silica-based sorbent
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The solvation parameter model is used to characterize the retention properties of a cyanopropylsiloxane-bonded, silica-based sorbent with methanol, acetonitrile, tetrahydrofuran, and isopropanol in water as mobile phases. The system constants over the composition range 1 to 50% (v/v) organic solvent indicate that retention occurs because of the relative ease of cavity formation in the solvated stationary phase compared to the same process in the predominantly aqueous mobile phase as well as from more favorable stationary phase interactions with solutes containing π- and n-electrons. The capacity of the solute for dipole-type interactions is not important whereas all hydrogen-bond-type interactions result in reduced retention. Graphing the system constants as a function of mobile phase composition provides a simple mechanism for interpreting the change in capacity of the chromatographic system for retention in terms of changes in the relative weighting of fundamental intermolecular interactions. A comparison is also made with the retention properties of an octadecylsiloxane-bonded, silica-based sorbent with 30% (v/v) methanol in water as the mobile phase and the extraction characteristics of a porous polymer sorbent with 1% (v/v) methanol, acetonitrile, tetrahydrofuran, and isopropanol in water as the sample processing solvent. Changes in sorbent selectivity due to selective uptake of the processing solvent are much smaller for the cyanopropylsiloxane-bonded sorbent than the results found for a porous polymer sorbent.
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  • 75
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    Chromatographia 41 (1995), S. 66-74 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Limit of detection ; Precision ; Uncertainty prediction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method to determine the limit of detection (LOD) in high performance liquid chromatography (HPLC) is described. The power spectral density of instrumental baseline variation is fitted by the simplex least squares methods with a mixed random process of white noise and Markov process as a model. The white noise is characterized by standard deviation (SD), ∼w; the Markov process by the SD, ∼m, and auto-correlation degree, ρ. All required parameters for calculating the LOD signal are obtained by experiment without repeat measurements. No arbitrary constants are needed. The LOD signal is uniquely determined and is characterized by 33.3% relative standard deviation (RSD) of analyte measurements and 0.13% of the error of the first type. This signal also specifies that the signal-to-noise ratio=3, using the definition of noise originating from the white noise and Markov process. The theoretical conclusion is verified by the Monte Carlo simulation using real baseline and peaks. The LOD concentrations for naphthalene, acenaphthene, pyrene and perylene are given.
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  • 76
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Hydroxycinnamic derivatives ; Photodiode-array detection (DAD)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The present paper describes the development of a method for the differentiation of hydroxycinnamic acid derivatives by HPLC with photodiode-array detection. Furthermore spectral data of the compounds under investigation are given. Whereas p-coumaric acid derivatives are distinguishable from caffeic and ferulic acid derivatives by the positions of their spectrum maxima and their convexity interval value, it is not possible to distinguish between caffeic and ferulic acid derivatives because of overlapping spectrum maxima and convexity interval values.
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  • 77
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fluoroquinolones ; Quinolizines ; Impurity Profile ; Abbott compound 086719.1
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The purity of the investigational antibacterial Abbott-086719.1 (I) which is 8[(3S)-3-amino-1-pyrrolidinyl]-1-cyclopropyl-7-fluoro-9-methyl-4-oxo-4H-quinolizine-3-carboxylic acid hydrochloride is determined using gradient elution HPLC. The chromatographic separation was optimized and the chromatographic parameters critical to separation are discussed in detail. Most acceptable separations were achieved using an Alltima C18 column (5 μm) measuring 4.6 mm I.D.×15 cm with 0.01M–0.03M citrate eluents which were modified with acetonitrile or with mixtures of acetonitrile and methanol. Related substances in I were determinable to 0.05%. Repeatability (RSD values) for determining related substances at levels of 0.50 to 0.06% ranged from ±1.9 to ±10%. Determinations of I in 5% dextrose in water and in hydroxypropyl methylcellulose were made using the same column and a simple isocratic system. The determination of I was stability indicating with precision (RSD values) of ±0.5% to ±2.0% and good agreement with theory for formulations containing I at 1.0 to 95 mg/mL concentrations. Recoveries of I from the vehicles were quantitative and linearity of the detector response of I was demonstrated to at least 0.10 mg/mL.
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  • 78
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    Chromatographia 41 (1995), S. 204-206 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; p-tert-Butylcalixarenes
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    Topics: Chemistry and Pharmacology
    Notes: Summary Thep-tert-butylcalix[n]arenes (n=4,6,7,8) andp-tert-butyldihomooxacalix[4]arene have been separated by reverse phase liquid chromatography. Optimum conditions have been obtained on a Spherisorb ODS1, 5 μm C18 column by isocratic ambient elution with acetonitrile-methyltert-butyl ether. Calibration plots have been obtained from purified calixarenes and the reliability of the method is confirmed from test mixtures of calixarenes of known composition.
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  • 79
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Solid phase extraction ; Enzyme-based biosensor detection ; Tyrosinase ; Phenols
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A fully integrated screening system for phenolic compounds was developed incorporating on-line solid phase extraction, fractionation and biosensor detection. Two different types of biosensors, solid graphite and carbon paste electrodes incorporating the enzyme tyrosinase, were compared and used in the screening system. Interfacing of the solid phase extraction and fractionation with the biosensor detection was given special attention since the biosensors were not compatible with the organic modifier used for desorption of phenols from the solid phase extraction step. The system was validated with conventional analytical techniques. Surface water samples from the Ebro river were spiked with 1,10, and 25μg L−1 of catechol, phenol,p-cresol, respectively. Three out of seven samples were spiked and the correct samples were identified, containing phenols equivalent to the spiked concentrations.
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  • 80
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Amino acids ; Hydrophobicity ; o-Phthalaldehyde-N-acetyl-L-cysteine derivatives ; Phenylthiohydantoin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Hydrophobic character is usually expressed in terms of the partition coefficient in 1-octanol-water (log PO/W). However, measurement of this coefficient is often problematic. Retention in micellar liquid chromatography is mainly due to hydrophobic interactions and can also be used as an index of hydrophobicity. A hydrophobicity scale was established with retention data foro-phthalaldehyde (OPA)-N-acetyl-L-cysteine (NAC) amino acid derivatives, using the glycine derivative as reference. Since the OPA-NAC derivatives only differ in the nature of R1 in the amino acid (R1CH(COOH)NH2), in the absence of electrostatic interactions the hydrophobic character of the substituent was responsible for retention. Linear relationships were obtained between log of the ratiok′ of amino acid derivatives:k′ of the glycine derivative for a given mobile phase, and logP O/W for the R1 substituent. Good correlations were also found for phenylthiohydantoin amino acid derivatives.
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  • 81
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    Chromatographia 41 (1995), S. 462-470 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Solid-phase microextraction (SPME) ; Headspace solid-phase microextraction (HSPME) ; Environmental analysis ; Water analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Solid-phase preconcentration coupled on-line with liquid chromatography, and solid-phase microextraction coupled with gas chromatography have been applied to the determination of trace-level concentrations of benzene and sulfur compounds (tetrahydrothiophene (THT),t-butyl mercaptan (TBM), andn-butyl mercaptan (nBM)) in aqueous media. The first technique uses a microcolumn packed with a styrene-divinylbenzene copolymer. Retention values for THT, TBM, and benzene on this sorbent, expressed as the capacity factors, are 1100, 1600, and 4000, respectively. It is, therefore, possible to preconcentrate them efficiently and this method enables minimum concentrations of 0.05, 0.7, and 0.8 μg L−1, respectively, to be reached. In microextraction, a fine silica fiber coated with a thin layer of polydimethylsiloxane is used. The partition coefficients of the analytes between the polymeric coating and water have been determined to be 40, 115, and 110 for THT, TBM, and benzene, respectively. When sampling is performed from the liquid phase, partition equilibrium is reached within 5 to 20 minutes, or more quickly when the solution is agitated. Using a flame ionization detector, detection limits for THT, TBM, and benzene were 3, 5, and 0.2 μg L−1, respectively. Extraction of volatile or semi-volatile analytes can also be performed from the headspace with very similar detection limits. In addition, the extraction time is shorter since equilibrium is reached within 1 to 1.5 minute, which can again be reduced by agitation of the sample. The advantages and drawbacks of both techniques are gathered and discussed in this paper, which also underlines their complementarity.
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  • 82
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Divinyl chlorophyll a and b (chl a2 and chl b2) ; Polymeric ODS phases ; Prochlorophytes ; Temperature step gradients
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Divinyl chlorophyll a (a2) and divinyl chlorophyll b (b2) are chemotaxonomic marker pigments for the marine prochlorophytes, and can be used to study their distribution in marine samples. In this paper we report a baseline resolution of mono- and divinyl forms of chlorophylls a and b employing polymeric ODS stationary phases at sub-ambient temperatures. The simultaneous resolution of mono- and divinyl forms of chlorophylls a and b, chlorophylls c1, c2, c3, Mg 3,8-divinylphaeoporphyrin a5 monomethyl ester (MgDVP), and phytol-substituted chlorophylls c was achieved when a temperature step gradient was employed during the analysis. An example is given of the utility of the protocol in oceanic field samples.
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