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  • Digitale Medien  (602)
  • Loseblatt
  • 1995-1999  (602)
  • 1930-1934
  • 1925-1929
  • 1998  (602)
  • 1933
  • Physics  (299)
  • Analytical Chemistry and Spectroscopy  (163)
  • Capillary electrophoresis  (140)
Materialart
  • Digitale Medien  (602)
  • Loseblatt
Erscheinungszeitraum
  • 1995-1999  (602)
  • 1930-1934
  • 1925-1929
Jahr
  • 1
    Digitale Medien
    Digitale Medien
    Springer
    Zeitschrift für Lebensmittel-Untersuchung und -Forschung 206 (1998), S. 246-250 
    ISSN: 1431-4630
    Schlagwort(e): Key words Histamine ; Capillary electrophoresis ; Photometric determination ; Liquid liquid extraction ; Solid phase extraction
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Werkstoffwissenschaften, Fertigungsverfahren, Fertigung
    Notizen: Abstract  To determine levels of histamine, two methods were used, photometry in conjunction with two sample clean-up procedures, and capillary zone electrophoresis (CZE). The two sample clean-up procedures used were liquid liquid extraction (LLE) with n-butanol and solid phase extraction (SPE). Using CZE, the separation of histamine from the matrix was good. The other method, photometry, represents a classic and simple method, that can be employed for in situ measurement of histamine. We found that it was necessary to clean up the samples prior to photometry; if this was not done, the recorded levels of histamine were higher than those determined by CZE. In order to determine levels of histamine, both of these rapid tests were applied to ten different foodstuffs. The levels of histamine measured using photometry following either LLE or SPE were compared. The results indicated that photometry is a suitable method for the measurement of histamine, although the sample solutions have to be purified by either LLE or SPE. Samples do not need to be cleaned up before CZE because there is no interference between histamine and attendant material. Both sample clean-up procedures were applied to the following foodstuffs: tomatoes, sauerkraut, tuna, leaf spinach, cream spinach, white wine and mackerel. The differences of the measured values vary between 3% and 18% for LLE and 6% and 27% for SPE. For the other foodstuffs, such as beef, beer and non-alcoholic beer, only one sample clean-up procedure is suitable. LLE used for beef and beer leads to differences in measured levels of histamine between 18% and 50%, respectively, whereas SPE used for non-alcoholic beer leads to differences of 20%.
    Materialart: Digitale Medien
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  • 2
    Digitale Medien
    Digitale Medien
    Springer
    European radiology 8 (1998), S. 849-857 
    ISSN: 1432-1084
    Schlagwort(e): Key words: Ultrasound ; Physics ; Vascular studies ; Vascular pathologies ; Ultrasonic contrast agents ; Clinical applications
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract. The choice of the optimal ultrasonic frequency for vascular studies is determined by the required resolution and penetration. Anatomical real-time two-dimensional imaging and blood flow studies provide complementary information. Intravascular scanning allows high-frequency ultrasound to be used, with correspondingly good spatial resolution. Contrast resolution is degraded by beam side lobes and the limited dynamic range of the ultrasonic pulse. The physics of ultrasonic scattering by blood, pulsed Doppler and duplex scanning and colour flow imaging performances determines the limits of clinical applications. Contrast agents enhance the echogenicity of blood, improving sensitivity and, through second harmonic detection, suppressing solid tissue echoes. Three-dimensional display, with segmentation by the presence of the flow signal, facilitates spatial perception. Clinical applications in vascular pathologies are summarised.
    Materialart: Digitale Medien
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  • 3
    ISSN: 1612-1112
    Schlagwort(e): Capillary electrophoresis ; Airborne particles ; Humic-like substances
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A considerable fraction of the refractory organic carbon in airborne particulate matter is to be attributed to humic-like substances (HULIS). Such atmospheric HULIS isolated from different air dust samples by a microscale extraction procedure were characterized by capillary electrophoresis (CE). For fractionation of HULIS the working conditions of the CE system were optimized using a borate buffer (pH 8.2), polyacrylamide (PAA) coated, fused-silica capillary and polyethylene glycol as sieving modifier. Using CE under optimized conditions, HULIS produced electropherograms showing well resolved and reproducible signals.
    Materialart: Digitale Medien
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  • 4
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 47 (1998), S. 249-256 
    ISSN: 1612-1112
    Schlagwort(e): Capillary electrophoresis ; Cyclodextrin mobile phase additives ; Synthetic food colorants ; Selectivity
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A high-performance capillary electrophoresis method with diode-array detection has been developed for analysis of synthetic food colorants. The influence of buffer composition on the separation of the food colorants was examined, as were the effects of α-, β- and γ-c-yclodextrins on analyte migration behavior. Eight food colorants were completely separated within 10 min using pH 9.5 borax—NaOH buffer containing 5 mM β-cyclodextrin. Experimental results indicate that the relative standard deviations of analyte migration times were〈0.88% under the optimized separation condition. Correlation coefficients of the linear calibration plots of the analytes exceeded 0.998. The method was suitable for determination of the quantities of synthetic food colorantsi in ice cream bars and fruit soda drinks.
    Materialart: Digitale Medien
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  • 5
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 48 (1998), S. 355-359 
    ISSN: 1612-1112
    Schlagwort(e): Capillary electrophoresis ; Cathodic flow electrode ; Electrolyte buffer depletion ; Reproductibility and precision
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The effects of electrolyte buffer depletion is well recognised and regular replacement of the electrolyte can prevent poor reproducibility. We have further investigated the effect of electrolyte depletion and produced a modified cathodic flow electrode to improve reproducibility using minimal volumes of electrolytes.
    Materialart: Digitale Medien
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  • 6
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 48 (1998), S. 395-401 
    ISSN: 1612-1112
    Schlagwort(e): Capillary electrophoresis ; Enantiomers ; Epinephrine ; Experimental designs ; Optimization
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A capillary electrophoretic method using a chiral selector was optimized by experimental design for the enantioresolution of epinephrine enantiomers. Two β-cyclodextrins derivatives, namely heptakis-2,6-di-O-methyl-β-cyclodextrin and carboxy-methyl-β-cyclodextrin, respectively neutral and charged, were used as chiral selectors employing an uncoated capillary. By using a statistical experimental design in which all factors are varied at the same time, it was possible to optimize the method with regard to the resolution between peaks and the two migration times. A fractional factorial design and a central composite design were used. A compromise between conflicting goals, such as maximization of resolution and minimization of analysis time, was found by means of a desirability function D. Balancing these goals against each other, the most acceptable solution to the problem was found and the optimized method gave a fast separation with complete resolution between the adrenaline enantiomers. The response surfaces obtained confirmed the robustness of the method.
    Materialart: Digitale Medien
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  • 7
    ISSN: 1612-1112
    Schlagwort(e): Capillary electrophoresis ; pK A determination ; Indirect UV detection ; Alkyl-alkyl phosphonic acids
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Capillary electrophoresis (CE) has proved to be a fast and convenient method for the determination of the dissociation constants of non-UV absorbing solutes in the acidic pK A range (2.0–2.5). The electroosmotic flow was reversed by washing the capillary with 0.2% polybren aqueous solution. A series of background electrolytes was prepared with phenylphosphonic acid (pK A=1.29) and β-alanine (pK A=3.55) with the same ionic strength and a high buffer capacity in order to improve the repeatability (0.1–0.2 %) of the electrophoretic mobility and to determine the values of pK A accurately. This procedure was applied to the determination of the dissociation constants of several alkyl-alkylphosphonic acids whose pK A values have not yet been published in the literature. In this work, their dissociation constants have been found to vary between 1.91 and 2.34 for alkyl-methylphosphonic acids and between 2.10 and 2.38 for alkyl-ethylphosphonic acids.
    Materialart: Digitale Medien
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  • 8
    ISSN: 1612-1112
    Schlagwort(e): Capillary electrophoresis ; Aldehydes ; Hydrazino benzene sulfonic acid ; Water analysis
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A method has been developed for the analysis of environmentally important aldehydes in rain water. The method is based on the derivatization of the aldehydes with hydrazino benzene sulfonic acid, separation of the hydrazones formed by capillary electrophoresis and UV detection at 280 nm. Derivatization was shown to be complete in 15 min at 50°C. The aldehyde derivatives could be separated from each other and from the excess of reagent using a pH 9 borate buffer as background electrolyte, with an analysis time of less than 6 min. The repeatability was better than 0.5% for the peak mobilities and in the order of 2–5% for the peak areas. Detection limits of 0.8–3 μmol L−1 (0.02–0.2 ppm) were obtained. The method was applied for the determination of formaldehyde and acetaldehyde in rain water samples.
    Materialart: Digitale Medien
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  • 9
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 48 (1998), S. 569-575 
    ISSN: 1612-1112
    Schlagwort(e): Capillary electrophoresis ; Oligonucleotides ; Dextran ; Polymer solution ; Purity testing
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Capillary gel electrophoresis (CGE) has been recognized as an effective method for the analysis of oligonucleotides. CGE using polymer solutions is especially useful and effective compared with that using crosslinked gels, because of easy change of media. Replacement of media leads to the reproducible separation of analytes. We have investigated CGE analysis of oligonucleotides of less than 20 bases employing various kinds of polymers. Polyacrylamide, dextrin, dextran, pullakin, and poly(ethylene glycol) were used as sieving matrixes at concentrations of 0–30 %. Polydeoxythymidylic acids [p(dT)11–20] were used as a test sample. These small oligonucleotides were successfully resolved on the basis of their base number by CGE using some of these polymer solutions. In particular, dextran was found to be effective and baseline separation was observed when a 30 % dextran solution was employed. Some validations such as linearity and reproducibility were also established and this method was found to be an adequate quality control method for small oligonucleotides. Finally, CGE using a 30 % dextran solution was successfully applied to impurity profiling of some synthetic oligonucleotides.
    Materialart: Digitale Medien
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  • 10
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 48 (1998), S. 739-744 
    ISSN: 1612-1112
    Schlagwort(e): Capillary electrophoresis ; Nucleotides ; Inorganic cations ; Complexation with Mg and Ca
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The complexation equilibrium between nucleotides (ATP, ADP) and inorganic cations (Mg2+, Ca2+) has been studied by capillary electrophoresis. The equilibrium constant and the stoichiometry of nucleotide-inorganic cation complexes can be deduced from the dependence of the electrophoretic mobility of each nucleotide on the negative logarithm of the inorganic cation concentration. The experimental values of complexation constants determined by CE compare favorably with those in the literature. As expected, Mg2+ forms more stable complexes with ATP (logK=2.30 and 4.10 at pH 5 and 8, respectively) than with ADP (logK=1.92 and 3.15 at pH 5 and 8, respectively). In the pH range 4–8, the stoichiometry of ADP-Mg2+ and ADP-Ca2+ complexes is always 1∶1 whereas that of the complexes between these cations and ATP depends on pH-hence ATP-Mg2+ and ATP-Ca2+ complexes have 1∶1 stoichiometry at pH 5 and 1∶2 at pH 8.
    Materialart: Digitale Medien
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  • 11
    ISSN: 1612-1112
    Schlagwort(e): Capillary electrophoresis ; Conductivity tuning ; Chiral separation ; Peak symmetry ; Resolution expression
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Different approaches how to handle the electromigration dispersion process that occurs in separation and determination of enantiomers are presented. The use of cyclodextrins as chiral selectors in resolution enantiomers involves the possibility to tune the conductivity of the sample band in order to obtain symmetrical and efficient peaks. Determination of impurities that migrate in the rear part of an overloaded main peak can be accomplished if the conductivity of the background electrolyte (BGE) is adapted to the conductivity of the sample band. This strategy was shown in determination of the content of D-sotalol in a mixture of L and D-sotalol. The efficiency and the symmetry of the overloaded L-sotalol peak was substantially improved by substitution of tetrabutylammonium ions for tetrapentylammonium ions as co-ions in the BGE. In this system it was possible to determine 0.2% w/w of the chiral impurity D-sotalol. A resolution model is presented and used qualitatively in the study where the complexation between the tetraalkyllammonium ions and the cyclodextrins is taken into account.
    Materialart: Digitale Medien
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  • 12
    ISSN: 1612-1112
    Schlagwort(e): Capillary electrophoresis ; Succinic and levulinic acid ; Indirect UV detection ; Standard addition method
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary This paper describes an capillary electrophoresis (CE) method used to quantify both succinic acid and levulinic acid in an industrial production process. Measurement was performed by CE with indirect UV detection, using potassium hydrogen phthalate as the UV-absorbing additive. The electrolyte composition used was 5 mM potassium hydrogen phthalate at pH 7.0 containing 0.25 mM cetyl trimethylammonium bromide (CTAB) as an electrosmotic flow (EOF) modifier to reverse the EOF. The method provides for improved sensitivity by employing an extended path length capillary, and for identification and quantification by the use of a standard addition method.
    Materialart: Digitale Medien
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  • 13
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 47 (1998), S. 219-224 
    ISSN: 1612-1112
    Schlagwort(e): Capillary electrophoresis ; Beta-blockers ; Protein separation ; Drug separation ; Guaran ; Buffer modifier
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Guaran, a neutral polysaccharide, has been used as a buffer modifier to improve the separation of basic proteins and drugs. Migration reproductibility, peak shape and efficiency were improved when 0.1% guaran was added to the buffer. The concentration of guaran, ionic strength, and pH of buffer solution were optimized to obtain the optimum separation of proteins. Possible separation efficiencies of 700,000 plates per meter were obtained for test proteins. The relative standard deviation (% RSD) of the migration time of all test proteins was less than 0.5%. Improved separation of β-blockers was also observed when guaran was added to the buffer.
    Materialart: Digitale Medien
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  • 14
    ISSN: 1612-1112
    Schlagwort(e): Capillary electrophoresis ; DNA fragments ; Cellulose derivatives ; Sieving cellulose matrix
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A rapid, robust and reproducible method providing excellent separation performance and simplicity using a 0.5% MC-4000 methyl cellulosic sieving medium in DB-1 coated capillaries has been developed. The method is suitable for qualitative comparison of DNA restriction profiles for fragments in the size range 100–1000 base pairs (bp). Efficiencies up to 8.5 million plates/m (1057 bp fragment) were recorded. Peak resolution of 6 bp (291/297 bp, 335/341 bp) and 4 bp (238/242 bp, 341/345 bp) was achieved. In addition, 1 bp partial resolution of 123/124 bp and 298/297 bp was obtained. Run-to-run (n=15), day-to-day (n=4), and capillary-to-capillary (n=3) variations of 0.1–0.2% RSD, 0.3–0.5% RSD, and 0.1–0.3% RSD, respectively, were observed. The MC-4000 sieving matrix was found to be better than hydroxypropyl methyl cellulose and hydroxypropyl cellulose, in terms of both performance and stability in the DB-1 coated capillaries. The efficiency and resolution in DB-WAX capillaries were inferior to those obtained in DB-1 capillaries. The commercially available DB-1 capillaries were stable for months in the sieving medium at pH 8.3 and could be regenerated to provide high efficiency after accidental current breaks.
    Materialart: Digitale Medien
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  • 15
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 48 (1998), S. 331-346 
    ISSN: 1612-1112
    Schlagwort(e): Peak integration ; Baseline determination ; Quantitation ; Capillary electrophoresis ; Chromatography
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Peak integration is still a major source of error in analytical techniques such as chromatography (LC and GC), aapillary electrophoresis (CE), spectrosocpy, and electrochemistry. If the baseline is complex, e.g. because of matrix effects, or if the peak shape is irregular, e.g. because of peak tailing, the results are often not satisfactory when classical procedures are used. These shortcomings arise because of the stepwise appearance of the chromatogram. An algorithm that copies the human method of considering baseline and peaks as a whole has already been introduced. Here the use of a straight line as a baseline model led to an improvement in several instances. The baseline is, however, usually not exactly straight and rigid. A baseline model with flexible properties is more advantageous. Thus the smoothing cubic spline function is applied in this work. Here the rigidity can be controlled by use of a parameterp k. The prediction interval of the spline is used for iterative distinction between baseline and peak regions. Afterwards straightforward optimization of the peak boundaries is applied. More than 50 series of consecutive injections of the same sample (n=40 on average) were used to test the performance of this procedure. The same raw data have been integrated by means of the algorithm described here and by use of commercially available software. The reproducibility of the main component peak are within the series was taken as a measure of integration quality. Typically the new procedure reducesRSD % by approximately 33% (e.g. from 1.5% to 1.0%). The improvement is even more impressive for difficult samples with complex matrices, e.g. blood plasma or polymer excipients. for such samples improvements of up to a factor of 6 are obtained.
    Materialart: Digitale Medien
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  • 16
    ISSN: 0935-6304
    Schlagwort(e): Epoxytriacylglycerols ; high temperature gas chromatography ; hydroxytriacylglycerols ; ketotriacylglycerols ; lipids ; negative chemical ionization mass spectrometry ; SOP-50 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Five seed oils consisting of unusual triacylglycerols have been examined by high temperature gas chromatography using glass capillary columns coated with the stationary phase SOP-50 (50%-diphenyl-50%-dimethylpolysiloxane, methoxy-terminated). The investigated hydroxy, epoxy, and ketokonjuene triacylglycerols were first derivatized in order to permit analysis by high temperature gas chromatography. Structural elucidation of the intact triacylglycerols was performed with high temperature gas chromatography/negative chemical ionization-mass spectrometry using NH3 as a reagent gas. Individual derivatized lipid species with a molecular weight up to 1176 g/mol could be identified.
    Zusätzliches Material: 10 Ill.
    Materialart: Digitale Medien
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  • 17
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 169-174 
    ISSN: 0935-6304
    Schlagwort(e): CZE ; detection limit ; signal-to-noise ratio ; correlation chromatography ; reproducibility ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Poor signal-to-noise ratios and analytical reproducibility in capillary electrophoresis were improved by application of multiple injections of the same sample at (pseudo) randomly chosen time moments. One order of signal-to-noise ratio improvement was achieved in practice using an in-house developed computer-controlled pneumatic sampler. However, it is demonstrated here that better implementation of the capabilities of multiple input requires that the detector signal noise be “pre-whitened”, i.e. spikes, baseline drift, oscillations etc. must be removed from the detector signal before transforming it to the electropherogram in the common form. Such filtering of the detector signal was realized by implementing iterative, menu-driven software written in Matlab, a high-level programming language.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 18
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 181-184 
    ISSN: 0935-6304
    Schlagwort(e): Trace analysis, atmospheric ; digital signal processing ; signal to noise reduction ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 19
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 189-192 
    ISSN: 0935-6304
    Schlagwort(e): Chiral stationary phases ; pyrethroic acids ; enantiomer separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 20
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 193-196 
    ISSN: 0935-6304
    Schlagwort(e): capillary electrophoresis ; dissolving solvent selection ; optimization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 21
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 201-208 
    ISSN: 0935-6304
    Schlagwort(e): PAN ; peroxyacetyl nitrate ; alkyl nitrate ; chlorinated hydrocarbons ; halocarbons ; capillary GC-ECD ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A cryogenic preconcentration/high-resolution gas chromatographic technique has been developed for the rapid, simultaneous quantitation of C1-C4 organic nitrates and halocarbons in ambient air. Whole-air samples are collected in TedlarTM bags by an evacuated-chamber method. Samples were stable in 0.010-cm-thick bags for 24 h if they were immediately stored in a freezer at -25°C. Analytes in a 50-cm3 air sample were efficiently preconcentrated on fused-silica beads at -180°C and thermally desorbed at 30°C. High-resolution gas chromatography with a cross-linked polydimethylsiloxane fused-silica capillary column and an electron-capture detector were used for separation and quantitation of the analytes. An analysis time of about 12 min was facilitated by sample cryofocusing at -180°C and oven temperature programming. Recoveries of the analytes by the evacuated-chamber method were better than 95%. The sensitivity of the technique for sample volumes of 50 cm3 is in the sub-parts-per-trillion by volume (ppt[v]) range for many of the analytes, with an average precision of about ±5% for analytes at levels of about 10 ppt(v).
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 22
    ISSN: 0935-6304
    Schlagwort(e): capillary electrophoresis ; enantiomer separation ; hydroxypropyl-β-cyclodextrin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Following an extended screening project, 86 racemic drugs were investigated by capillary zone electrophoresis in the presence of the chiral solvating agent (CSA) hydroxypropyl-β-cyclodextrin. A total of 42 drugs out of 86 tested was thereby separated into enantiomeric pairs. Statistical analysis of the numerous experiments performed un der identical conditions reveals a loose correlation of the migration separation factor (αm) with the migration retardation factor (Rm). For a subset of 23 drugs, a drop in the concentration of the CSA was also studied, showing the way to further optimization.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 23
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 253-257 
    ISSN: 0935-6304
    Schlagwort(e): Edible oils ; lipids in foods ; HPLC ; Polycyclic Aromatic Hydrocarbons (PAHs) ; off line LC-LC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 24
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 234-240 
    ISSN: 0935-6304
    Schlagwort(e): Micellar electrokinetic capillary chromatography ; electroosmotic migration ; electrophoretic migration of micelle ; retention mechanism ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---In the present work, four organic modifiers, viz. urea, dioxane, methanol, and tetrahydrofuran, were comparatively and systematically studied in terms of their effects on electrokinetic migration behavior and the retention mechanism of homologous solutes in MECC. The results showed that the electroosmotic mobility, μeo, and the electrophoretic mobility of a micelle, μep,mc, decrease linearly with increasing organic modifier concentration. The ability of organic modifiers to lower μeo is greater than their ability to lower μep,mc. The negative values of the slopes of these linear relationships, Deo and Dep,mc, increase along the series the order urea 〈 methanol 〈 dioxane 〈 tetrahydrofuran. The logarithm of the capacity factor (ln k′) of uncharged homologous solute, which is mainly determined by the hydrophobic interaction, decreases linearly with increasing organic modifier concentration, due not only to the decrease in the partition coefficient but also to the decrease in the phase ratio. A linear relationship was observed between the slope of the plot of ln k′ vs. organic modifier concentration and the carbon number of homologous compound. The slope of such a relationship can characterize the hydrophobicity of the organic modifier. The hydrophobicity of such organic modifiers is also found to increase along the series urea 〈 methanol 〈 dioxane 〈 tetrahydrofuran.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 25
    ISSN: 0935-6304
    Schlagwort(e): Fluoroquinolone ; ASTED ; HPLC fluorescence ; sarafloxacin ; flumequine ; oxolinic acid ; chicken liver ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A recently introduced programmable fluorescence detector was compared with a single wavelength fluorescence detector for quantification of fluoroquinolone (FQ) antibacterial agents, which have widely varying spectral characteristics. The two detectors were connected in parallel to an HPLC system to test their performance characteristics. With single wavelength detection, two FQs, flumequine and oxolinic acid could be detected at an emission wavelength of 368 nm in a single chromatogram while a third FQ, sarafloxacin, was not observed at that wavelength. Similarly, when the detector was optimized for sarafloxacin emission at 440 nm, the other two compounds were undetected. In contrast, all three FQs were quantified at their individual maxima in a single run using the programmable fluorescence detection. The applicability of an HPLC - programmable fluorescence detector, in combination with on-line microdialysis, also was evaluated using chicken liver fortified at low ppb levels with the three FQs. After on-line microdialysis sample clean up, the resultant HPLC chromatograms were free of background interference enabling the programmable detector to optimize the quantitation of the three analytes in a single run. The limit of quantification (LOQ) determined for each FQ was 1.0 ppb and the limit of detection (LOD) was 0.2 ppb, an order lower in magnitude than was obtainable with single wavelength detection.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 26
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 267-281 
    ISSN: 0935-6304
    Schlagwort(e): Chemically bonded phases, CBPs ; liquid chromatography, HPLC ; preparation; surface characterization ; column evaluation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---In order to increase chromatographic selectivity and to extend the analytical capability of reversed phase liquid chromatography (RP HPLC) many investigators have concentrated on the preparation of silica based column packings with chemically bonded phases (CBP). These phases have also been successfully used in sample preparation techniques, mainly in solid phase extraction (SPE). Although alkyl bonded phases (e.g., C2, C8, and C18) are the most widely used packings in RP HPLC and SPE, various specific applications require CBPs with polar functional groups (e.g., -NH2, -NO2, -CN, and/or -OH). The solution of problems with separation of complicated chiral compounds was attempted by applying stationary phases with chiral selectors (e.g., cyclodextrins, Pirkle phases, crown ethers, etc.). On the other hand, packings with pseudo-membrane or liquid crystal properties have been utilized for the separation of various substances of natural origin. Porous silica is commonly used as a support in the preparation of CBPs. Its physico-chemical characteristics, such as: type and structure of siliceous matrix, porosity, type and concentration of silanol groups, as well as surface purity, strongly influence the density and structure of chemically bonded phases. Recognition of these properties is helpful in optimizing separation processes based on RP HPLC elution and/or extraction of substances with polar character.
    Zusätzliches Material: 12 Ill.
    Materialart: Digitale Medien
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  • 27
    ISSN: 0935-6304
    Schlagwort(e): capillary gas chromatography ; microplasma mass spectrometry ; radio frequency plasma ; element-selective detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Capillary gas chromatography was performed with mass spectrometric detection using a novel microplasma ion source for operation in an element-selective mode. The ion source was a 350 kHz radio frequency helium plasma, which was sustained inside the 4 cm end of a 0.32 mm i.d. fused silica capillary column, and located inside the high vacuum chamber of the quadrupole mass spectrometer. Due to the low volume of the ion source, a stable low pressure discharge was produced utilizing only the 2.25 mL min-1 of GC carrier gas (helium) for plasma support. Small amounts of oxygen (0.1-0.2% v/v) were added to the plasma gas in order to prevent carbon deposits and to enhance signal-to-noise ratios. Chlorine and bromine were selectively detected at the 5-20 pg s-1 level (S/N = 2), and both produced a response that was linear within 3 orders of magnitude.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 28
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 315-316 
    ISSN: 0935-6304
    Schlagwort(e): Tertiary amine ; ruthenium ; chemiluminescence ; photochemical oxidation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 29
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 303-307 
    ISSN: 0935-6304
    Schlagwort(e): gas chromatography ; modified silica gel ; gaseous standard mixtures ; FID calibration ; carbon monoxide and carbon dioxide ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Quartz rods coated with a thin layer of chemically modified silica gel have been used for the generation of a two-component gaseous standard mixture containing carbon monoxide and carbon dioxide. A new method based on thermal decomposition of immobilized compounds chemically bonded to the surface of silica gel has been used in the generation process. The oxalic acid moiety bonded to the glycydoxypropylsilylated surface of silica gel underwent decarbonylation and decarboxylation at 300°C, yielding carbon monoxide and carbon dioxide. On-line connection of a thermal desorber with the GC/FID enabled calibration of the detector following the process of methanization of CO and CO2. The following amounts of CO and CO2 were generated per unit length of the rod: 15.1 × 10-8 Mol cm-1 (RSD = 5.71%) for CO and 34.2 × 10-8 Mol cm-1(RSD = 5.16%) for CO2.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 30
    ISSN: 0935-6304
    Schlagwort(e): Large-volume on-column injection ; gas chromatography ; infrared spectrometry ; microcontaminants ; solid-phase extraction ; open-split interface ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A large-volume on-column GC-cryotrapping-IR system was developed for injections of up to 100 μl of organic extracts. Considerable reduction of the solvent-and-water background and enhanced analyte detectability was achieved by using an open-split interface between the GC column and the IR detector and improving the leak-tightness of the system. The system was combined with solid-phase extraction to yield on-line SPE-GC-IR. With this set-up, sample volumes of only 20 ml sufficed to detect, and identify, microcontaminants in tap and surface water at the 0.1-1 μg/L level. Detection limits were on the order of 15 ng/L for tap water when using appropriate functional-group chromatograms. Or, in other words, SPE-GC-IR is a suitable technique for the screening of environmental water samples for functional groups, i.e. classes of compounds, of interest.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 31
    ISSN: 0935-6304
    Schlagwort(e): Adsorption/thermal desorption sampling instrument ; capillary gas chromatography ; electrolytic conductivity detector ; photoionization detector ; environmental air monitoring ; hazardous air pollutants ; volatile organic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 32
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 475-476 
    ISSN: 0935-6304
    Schlagwort(e): Scent glands ; defense substances ; n-alkanes ; furanones ; 2-alkenals ; 2-alkenyl acetates ; 2-decenols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 33
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 491-497 
    ISSN: 0935-6304
    Schlagwort(e): Fast GC ; narrow-bore columns ; trace analysis ; splitless injection ; on-column injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The use of hot splitless, cold splitless, and on-column injections for trace analysis in narrow-bore capillary GC is evaluated. Despite the low flow rates for the columns used, the required splitless times for splitless injections can be surprisingly short if liners with a small inside diameter are used. On-column injection can be applied by using an appropriate normal-bore precolumn coupled to the narrow-bore analytical column using a specially designed low dead volume column connector. The effects of the experimental conditions such as sample volume, injection temperature, and initial oven temperature on peak focusing and the discrimination and degradation behavior of the analytes are discussed. The possibilities to obtain sensitive and fast separations are illustrated by various applications.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 34
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 505-508 
    ISSN: 0935-6304
    Schlagwort(e): capillary electrophoresis ; inorganic ions ; polyethyleneimine ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A capillary zone electrophoresis (CZE) method for the simultaneous assay of bromide, iodide, nitrite, nitrate, and thiocyanate using direct UV detection is reported. The method is based on the separation of anions in a capillary coated with a cationic polymer, polyethyleneimine (PEI). The minimum detection limits, reproducibility of peak areas, and migration times were determined at the optimal condition. The method was applied to the analysis of tap water and human urine. The changes in separation selectivity of the anions resulting from addition of the cationic polymer to the buffer were investigated.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 35
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 523-526 
    ISSN: 0935-6304
    Schlagwort(e): High-performance liquid chromatography ; gardenia constituent separation ; genipin gentiobioside ; geniposide ; crocin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 36
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 435-439 
    ISSN: 0935-6304
    Schlagwort(e): Micellar Electrokinetic Chromatography (MEKC) ; counter pressure moderated MEKC ; migration time window ; peak resolution and peak capacity in MEKC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The influence of a hydrostatic counter pressure on basic mobility equations in MEKC was analyzed theoretically and investigated experimentally. Taking into account the influence of counter pressure, the modified mobility equations predict a decreased migration time ratio t0/tMC, which was confirmed by results obtained in SDS-MEKC separation of a homologous series of n-alkyl phenyl ketones. As a result, the migration time window could be enlarged in a simple way without having to change the chemistry of the system. Although counter pressures reduce peak efficiency in MEKC by disturbing the plug profile, the concomitant enlargement of the migration time window compensates for this effect. Especially for later migrating compounds, peak resolution could be enhanced at moderate counter pressures. The overall peak capacities within the whole migration window increases slightly when applying counter pressures up to 10 mbar.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 37
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 445-449 
    ISSN: 0935-6304
    Schlagwort(e): chiral separation ; organic cation effect ; ethylamines ; ethanolamines ; basic drugs ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---This paper addresses the influence of small organic cations in the background electrolyte (BGE) on chiral separation by capillary zone electrophoresis (CZE). Seven basic drugs, viz. alprenolol, amphetamine, anisodamine, isoprenaline, pinacidil, synephrine, and verapamil were used as test compounds with hydroxylpropyl-β-cyclodextrin (HP-β-CD) as the chiral selector. Resolution of the chiral test compounds was studied at pH 2.5 in the presence of Tris, ethanolamine, diethanolamine, triethanolamine, diethylamine, and triethylamine, which exist in their cationic forms at this pH value. Among the six cationic additives studied, triethylamine is most effective in enhancing resolution. A tentative mechanism of the effect is proposed.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 38
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 569-573 
    ISSN: 0935-6304
    Schlagwort(e): Chinese herbal preparation ; Shao-yao-tang ; pharmaceutical analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A high-performance liquid chromatographic method for the separation of twenty one constituents of Shao-yao-tang including six flavonoids, six alkaloids, three anthraquinones, three carboxylic acids, one monoterpene, one saponin, and one aldehyde was developed. Detection at 275 nm with a linear gradient elution system consisting of tetrabutylammonium bromide (TBA) and acetic acid solution was found to be suitable for determination of nineteen marker substances in an unpretreated Shao-yao-tang extract within 75 min. This method can also be used to analyze 11-14 components in a number of Chinese herbal preparations such as San-huang-hsieh-hsin-tang, Ching-chieh-lien-chiao-tang, San-tsung-kuei-chien-tang, Chai-hu-ching-kan-tang, and Ching-yin-li-ke-tang.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 39
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 575-576 
    ISSN: 0935-6304
    Schlagwort(e): Capillary electrochromatography (CEC) ; chiral separations ; Vancomycin stationary phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 40
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 577-581 
    ISSN: 0935-6304
    Schlagwort(e): Volatiles ; Bromeliaceae ; Bromelia plumieri ; glycosidically bound volatiles ; aroma precursors ; glucoconjugates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 41
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 587-591 
    ISSN: 0935-6304
    Schlagwort(e): capillary GC ; polymethoxyflavones ; citrus oil ; GC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The cold pressed peel oils of three species of citrus fruit, viz. sweet orange, tangerine, and grapefruit, have been examined for polymethoxyflavones by GC and GC-MS. Four GC column stationary phases were compared and separation of the six predominant orange oil polymethoxyflavones was obtained isothermally at 310°C in under ten minutes, including the resolution of the polymethoxyflavones from β-sitosterol. The nature of the stationary phase and the analysis temperature exercise dramatic effects on the resolution and elution order of the components, DB-35ms providing the best overall separation. A temperature programmed separation is also presented and the polymethoxyflavone composition of all three oils, as determined by GC-MS, is described. This is the first reported GC-MS study of the PMFs of these citrus species. While tangerine oil is as rich in polymethoxyflavones as orange oil, they are less abundant and occur at lower concentrations in grapefruit oil. Hydroxy-polymethoxyflavones were identified by GC-MS in tangerine oil. One hydroxy-pentamethoxyflavone, M+ = 388, identified in tangerine was also present at low levels in both orange and grapefruit oils. These results are compared with previous studies utilizing HPLC and GC.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 42
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 605-607 
    ISSN: 0935-6304
    Schlagwort(e): Reversed-flow MEKC ; separation according to polarity ; organic modifiers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Reversed-flow MEKC, i.e. MEKC at low pHs to suppress the electroosmotic flow, was evaluated for the separation of some homologous series. At low pHs compared to MEKC, the elution order reverses and normal phase type migration is obtained. Moreover, the elution window is nearly infinite. Efficiencies are very high and reproducibilities in absolute migration times are acceptable (%RSD 〈 5). The influence of a series of alcohol modifiers was investigated.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 43
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 597-604 
    ISSN: 0935-6304
    Schlagwort(e): high temperature gas chromatography ; atomic emission detection ; microwave induced plasma ; compound independent calibration ; non-ionic surfactants ; alcohol ethoxylates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---High temperature gas chromatography (HT-GC) coupled to atomic emission detection (AED) has been applied for the determination of alkyl chain distribution, mole average degree of ethoxylation and weight percent distribution of the corresponding homologues of alcohol ethoxylates without all the actual homologues being available as pure references. Based upon its constant elemental response, the HT-GC-AED system has been evaluated for its applicability to compound independent calibration within the homologous series of the alcohols and alcohol ethoxylates. Discrimination against high molecular weight components by gas chromatography requires conversion to the acetyl or trimethylsilyl derivatives. The latter includes introduction of the hetero atom silicon and thus allows monitoring of the silicon trace. Thus selectivity will be enhanced by excluding detection of compounds which do not react with the derivatization reagent. The method has been validated with the analysis of the technical product Brij 30, consisting of a mixture of alcohol ethoxylates with a vendor-specified mole average degree of ethoxylation of four. The experimental result yields a mole average degree of 4.0 ± 0.1 in the carbon, silicon and oxygen traces.
    Zusätzliches Material: 12 Ill.
    Materialart: Digitale Medien
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  • 44
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 608-612 
    ISSN: 0935-6304
    Schlagwort(e): propolis ; profiling ; CZE ; MEKC ; flavonoids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The usefulness of capillary electrophoresis (CE) with diode array detection for the profiling of Propolis, a hive product, is investigated. Water extracts of Propolis were analyzed with both capillary zone electrophoresis (CZE) at pH 7.0 and 9.3, and micellar electrokinetic chromatography (MEKC) with sodium dodecyl sulfate at pH 9.3. Characteristic profiles were obtained and several organic acids and preservatives could be identified by means of library comparison of the recorded UV spectra combined with addition of reference compounds to the extracts. The selectivity of the CZE and MEKC system differed considerably but the information obtained with both methods was similar. The dry residues of the water extraction were extracted with ethanol-water (70 : 30, v/v) and analyzed with the MEKC system to enable the separation of the more hydrophobic constituents of the Propolis samples. Complex profiles containing various well separated peaks were obtained allowing the identification of some interesting flavonoids. On the basis of the recorded CZE and MEKC profiles, the Propolis samples could be divided into two clearly different groups which are probably from a different origin.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 45
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 625-627 
    ISSN: 0935-6304
    Schlagwort(e): End-closure ; end-seal ; static coating ; glass and fused silica capillaries ; press-fit cap ; polyethylene closure ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 46
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 633-639 
    ISSN: 0935-6304
    Schlagwort(e): capillary gas chromatography ; microplasma mass spectrometry ; radio frequency plasma ; element-selective detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Simultaneous element-selective detection of the halogens and carbon was accomplished with capillary gas chromatography coupled with microplasma mass spectrometry. The microplasma ion source was a radio frequency plasma contained inside the last 4-5 cm of the 0.32 mm i.d. fused silica capillary column. The ion source was located inside the high vacuum housing of the MS, and only the GC carrier gas (2.3 mL min-1 of helium) was used for plasma generation. Atomic ions were detected in the positive mode. Detection limits were in the low picogram area, and the selectivity to carbon ranged from 8×102 for fluorine to higher than 104 for the other halogens. By introduction of both hydrogen and oxygen as reagent gases, peak tailing was avoided by suppression of analyte reactions with the silica walls of the ion source. Special attention was given to the fluorine-selective detection due to an interfering background species at m/z 19, assumed to be H3O+ originating from the reagent gases. The background signal was minimized by careful control of the power level.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 47
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 554-560 
    ISSN: 0935-6304
    Schlagwort(e): LC stationary phases ; octadecyl and octylsilica characterization ; cyclodextrins ; partially methylated cyclodextrins ; heptakis(2,6-di-O-methyl)-β-CD ; evaporative light scattering detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---In order to establish guidelines to help the analyst in the choice of the most suitable octadecyl or octyl bonded phase for the LC analysis of a given partially methylated β-CD sample, analyses of four commercially available dimethyl-β-cyclodextrins (DM-β-CDs) have been carried out on nine octyl (C8) or octadecyl (C18) silica bonded or polymeric bonded phases which differ significantly in their hydrophilic and hydrophobic properties. Chromatograms show that the nature of the packing materials has considerable influence on the resolution of complex mixtures composed of closely related compounds such as partially methylated β-CDs. Among various kinds of C8 and C18 bonded phases, silica based and monomeric phases which present both reinforced hydrophobic and polar interactions showed the best performance. Whatever the complexity of the commercial DM-β-CD, the richest chromatographic fingerprints, which best depict the complexity of the mixture, are obtained with Nucleosil 50-5-C8 column. For the simplest mixtures, Nucleosil 50-5-C8 column with acetonitrile-water (34:66) as mobile phase is the most suitable chromatographic system and leads to the best resolution between heptakis (2,6-di-O-methyl)-β-CD and hexakis (2,6-di-O-methyl)-mono(2,3,6-tri-O-methyl)-β-CD (14 OCH3 and 15 OCH3). This chromatographic system might enable an LC-MS coupling for direct identification of the different components in the mixture as well as control of batch to batch variations.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 48
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 565-568 
    ISSN: 0935-6304
    Schlagwort(e): capillary gas chromatography ; precalculation of retention indices ; boiling points ; two- and multidimensional taxonomic groups of organic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---It was shown that reciprocally unambiguous conformity between GC retention indices (at least for the commonly used standard nonpolar polydimethylsiloxane liquid phases) and boiling points of organic compounds is typical not only within one-dimensional taxonomic groups (homologous series and/or groups of congeners), but also within two- and multidimensional taxonomic groups (with simultaneous variations of some structural fragments). In all cases, this conformity is described by three-parameter non-linear equations log RI = a log Tb + b (n1 + Σ ki ni) + c, where n1 is the serial number of homologue within corresponding series and ni is the number of other structural fragments in the molecules. The coefficients ki in this equation reflect the relative alterations of molecular polarizabilities and may be estimated as ratios of refractions ki = RD(X)/RD(CH2), where X are variable structural fragments within a group of congeners, RD(CH2) = 4.647 cm3mol-1. The approach under discussion permits precalculation of the retention indices of any organic compounds with known boiling points. The precision of proposed method of RI precalculation is comparable with the contemporary level of interlaboratory reproducibility of experimental RI determination with standard nonpolar liquid phases (5-10 i.u.).
    Zusätzliches Material: 1 Tab.
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  • 49
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 583-586 
    ISSN: 0935-6304
    Schlagwort(e): Fast gas chromatography ; narrow-bore columns ; flash-2D-GC ; dedicated fast GC instrumentation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Savings in analysis time in capillary GC have always been an important issue for chromatographers since the introduction of capillary columns by Golay in 1958. In laboratories where gas chromatographic techniques are routinely applied as an analytical technique, every reduction of analysis time, without significant loss of resolution, can be translated into a higher sample throughput and hence reduce the laboratory operating costs. In this contribution, three different approaches for obtaining fast GC separations are investigated. First, a narrow-bore column is used under conventional GC operating conditions. Secondly, the same narrow-bore column is used under typical fast GC conditions. Here, a high oven temperature programming rate is used. The third approach uses a recent new development in GC instrumentation: Flash-2D-GC. Here the column is placed inside a metal tube, which is resistively heated. With this system, a temperature programming rate of 100°/s is possible. The results obtained with each of these three approaches are compared with results obtained on a column with conventional dimensions. This comparison takes retention times as well as plate numbers and resolution into consideration.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 50
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 592-596 
    ISSN: 0935-6304
    Schlagwort(e): capillary gas chromatography ; new chiral selectors anchored to polysiloxane ; t-leucine derivatives ; immobilization ; radical-induced cross-linking ; low racemization of the phases ; high enantioselectivity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---New chiral polysiloxanes have been prepared as stationary phases for gas chromatography, with (S)-(-)-t-leucine-t-butylamide, (S)-(-)-t-leucine-(S)-(-)-1-phenylethylamide, (S)-(-)-t-leucine-(S)-(-)-1-(α-naphthyl)ethylamide, (S)-(-)-t-leucine-(R)-( + )-1-phenylethylamide, and (S)-(-)-t-leucine-(R)-( + )-1-(α-naphthyl)ethylamide as selectors. Immobilization is achieved by radical-induced cross-linking with 1,3,5,7-tetravinyl-1,3,5,7-tetramethylcyclotetrasiloxane (V4) and dicumyl peroxide (DCUP) as cross-linking reagents and cured at 170°C. Under these conditions, racemization of (S)-(-)-t-leucine is less than 4.5% (R) for 1 h curing, while for polysiloxanes with the conventional (S)-(-)-valine selectors about 20% of R-enantiomers are formed by racemization. In the presence of 5% (w/w) V4 and 6% of DCUP with regard to the phases, 70-80% immobilization is achieved; without V4, the degree of immobilization is about 50% for both the (S)-(-)-t-leucine and (S)-(-)-valine selectors. As the size of the amide moieties of the selectors increases from t-butyl to 1-(α-naphthyl)ethyl, the degree of immobilization decreases. If the curing time is prolonged to 2 h, the extent of racemization increases. The selectivity factors achieved for amino acid enantiomers and similar pharmaceuticals are generally higher than those obtained with the corresponding non-immobilized Chirasil-Val phases.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 51
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 620-622 
    ISSN: 0935-6304
    Schlagwort(e): Multidimensional gas chromatography ; comprehensive two-dimensional gas chromatography ; kerosene analysis ; cryogenic modulation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 52
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 617-619 
    ISSN: 0935-6304
    Schlagwort(e): Capillary electrochromatography ; cellulose acetate fiber ; microcolumn liquid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 53
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 613-616 
    ISSN: 0935-6304
    Schlagwort(e): Micro LC ; FID detection ; superheated water ; alcohols ; aldehydes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---In the current study, an HPLC-FID system using superheated water as the eluent is constructed and further improved. Signal stability during temperature programmed operation was improved by using separate thermostatting of the 50 μm capillary restrictor. Operating the restrictor at 75°C prevented the superheated water from sputtering in the restrictor. Conventional octadecyl-modified silica, thermostable polymeric reversed phase and carbon type HPLC columns were used. The feasibility of the system is demonstrated by the analysis of a variety of compounds such as alcohols and aldehydes. It is shown that increased temperatures decrease elution times and, in addition to this, frequently improve peak shapes and column efficiencies. The separation of lower aldehydes is performed at 175°C with a detection limit in the low μg/ml range. The possibility of temperature programming is demonstrated for the separation of a range of alcohols. Furthermore, it is shown that temperature programming can be used for sample enrichment. Large volume injection with low temperature enrichment resulted in good peak shapes and a significant improvement of the detection limit. In this way, detection limits of 0.2 μg/ml (ppm) could be obtained for the aldehydes studied. Finally, the possibilities of using mobile phase additives as, e.g., buffers were briefly examined.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 54
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 623-624 
    ISSN: 0935-6304
    Schlagwort(e): Sulfur compounds ; waste paper ; chemiluminescence detector ; food packaging ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Tab.
    Materialart: Digitale Medien
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  • 55
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 640-644 
    ISSN: 0935-6304
    Schlagwort(e): chiral separation ; uncharged and charged cyclodextrin ; borate complexation ; capillary electrophoresis ; propranolol and its metabolites ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A buffer system of borate with charged (carboxymethyl-β-CD) and uncharged (β-CD) cyclodextrins (CDs) was employed in the chiral resolution and separation of propranolol and its selected major metabolites. By appropriate choice of buffer and additive conditions, chiral resolution of all of the compounds studied was achieved in a single analysis, where near baseline resolution was found for the difficult to resolve propranolol-glycol (Pr-glycol). This has not been observed in previous studies of propranolol and its metabolites.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
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  • 56
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 645-648 
    ISSN: 0935-6304
    Schlagwort(e): gas chromatography (GC) ; nitrogen-phosphorus detection (NPD) ; sorptive extraction/thermal desorption (SE/TD) ; amines ; in-situ derivatization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The use of sorptive extraction/thermal desorption (SE/TD) for the enrichment of amines from aqueous samples was investigated. The amines were derivatized in situ in the water sample by pentafluorobenzoyl chloride and subsequently enriched onto the SE cartridge. Two SE/TD cartridges were used, a commercially available polydimethylsiloxane (PDMS) packed cartridge and a similar cartridge prepared with newly synthesized poly(butyl acrylate) (PBA). Blank profiles of PBA were not as good as those obtained from the PDMS phase. A complex chromatogram was obtained using mass spectrometric detection. Fortunately, the use of a nitrogen-phosphorus detector (NPD) resulted in clean blanks. The PBA phase showed superior performance for the enrichment of the polar amine derivatives from water samples compared to the PDMS material. Using a CGC-NPD set-up and only 1 mL samples, detection limits are in the sub-ppb range.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 57
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 661-664 
    ISSN: 0935-6304
    Schlagwort(e): SPME ; AED ; metazachlor ; pesticides ; waste water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 58
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 658-660 
    ISSN: 0935-6304
    Schlagwort(e): 1,3-Dioxolanes ; acetals ; ketals ; coffee-like flavorings ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---This paper concerns a number of commercially available coffee-like flavoring preparations, identifying certain dioxolane structures of particular interest. The research was carried out by GC/MS, and spectral characterization was performed of the compounds in question, and especially of the acetals and ketals produced from compounds with carbonyl functions and 1,2-propylene glycol. Some determinations by means of chiral gas chromatography and by Isotope Ratio Mass Spectrometry (IRMS) have been useful in improving the analytical characterization of certain dioxolanes.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 59
    ISSN: 0935-6304
    Schlagwort(e): PAHs ; on-line SPE ; disk extraction ; RPLC ; water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 60
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 11-17 
    ISSN: 0935-6304
    Schlagwort(e): Acridine-modified HPLC stationary phases ; ligand mobility ; fluorescence spectroscopy ; time-resolved fluorescence anisotropy ; solid state NMR spectroscopy ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Ligand mobility of silica-based HPLC stationary phases modified by various surface coverages of acridine-9-carboxy(N-aminoethylaminopropyl)amide ligands was investigated by fluorescence spectroscopy, time-resolved fluorescence anisotropy measurements, as well as solid-state 13C-CP/MAS- and 1H-MAS-NMR spectroscopy. Rotational correlation times, τR, of the bound acridine fluorophore obtained from fluorescence anisotropy measurements are significantly longer in the bound phase, than in solution. Also, in time-resolved experiments anisotropies do not decay to zero. These results are interpreted in terms of wobble-in-cone ligand motion. The mobility of the fluorophore in the presence of liquid phase correlates strongly with the solubility of the model compound acridine-9-carboxy-n-butylamide in the same solvent. In the good solvent acetonitrile τR = 3.2 ns is found, whereas in methanol, τR 〉 80 ns is obtained. NMR measurements of the dry phase yield large linewidths, cross polarization constants, TCH, and spin-lattice relaxation times, T1ρH, shifting around the minimum in the correlation time curve. Both fluorescence and NMR data indicate medium to low ligand mobility. No difference in the mobilities of alkyl spacer and aromatic group is observed, probably due to the rigidity of the amide group.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 61
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 18-24 
    ISSN: 0935-6304
    Schlagwort(e): Reversed-phase HPLC ; capillary electrophoresis ; MALDI-MS ; whey proteins ; multiple peaks ; bovine serum albumin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Elution of a commercial sample of bovine serum albumin (BSA) in a reversed-phase (RP) HPLC system at room temperature gives a distorted peak. If a shallow gradient is used during elution a split peak is observed. The nature of the several parts of this multiple peak is studied using sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE), size-exclusion chromatography (SEC), amino acid analysis, re-elution in RP-HPLC of collected fractions, capillary electrophoresis (CE), and matrix assisted laser desorption ionization-mass spectrometry (MALDI-MS). This study demonstrates that the split peak of BSA observed in these chromatographic conditions is due to the monomer, dimer and other aggregates existing in the commercial sample of the BSA used. Moreover, it is proved that typical RP-chromatographic conditions do not cause aggregation of BSA.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 62
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 59-62 
    ISSN: 0935-6304
    Schlagwort(e): capillary electrophoresis ; mass spectrometry ; MALDI ; CE-MALDI ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 63
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 55-58 
    ISSN: 0935-6304
    Schlagwort(e): liquid chromatography-mass spectrometry ; electrospray ionization ; haloacetic acids ; trace analysis of environmental water samples ; waste water samples ; river water samples ; seawater samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Negative ionization electrospray liquid chromatography mass spectrometry was developed for the simultaneous determination of all nine haloacetic acids containing bromine and chlorine. Haloacetic acids were separated on a crosslinked polystyrene resin column using 3% acetic acid dissolved in acetonitrile:water (20:80) as mobile phase. The precision of this method varied from ±2.2 to ±7.1% for nine haloacetic acids. In addition, quantitative results obtained with spiked water samples at three different concentrations are described. The limit of detection of the proposed method using 200 mL of water samples was between 0.003 and 0.070 μg/L. This method was successfully applied to the trace determination of haloacetic acids in waste water, river water, and seawater.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 64
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 63-64 
    ISSN: 0935-6304
    Schlagwort(e): Injection port performance ; comprehensive two-dimensional GC ; GC× ; GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 65
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 65-68 
    ISSN: 0935-6304
    Schlagwort(e): GC-MS ; rain ; roof runoff ; fatty acids ; phenols ; alkanes ; chlorinated compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 66
    ISSN: 0935-6304
    Schlagwort(e): gas chromatography, helium ionization detector (HID) ; formaldehyde ; atmospheric oxygenates ; volatile organic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Two different gas chromatographic detectors, the helium ionization detector (HID) and the more commonly used flame ionization detector (FID), were used in parallel to compare their responses to a number of organic compounds. Atmospherically important oxygenated species were analyzed, as well as hydrocarbons and chlorinated and sulfur containing organics. The HID exhibited the better response to all compounds investigated, most notably to formaldehyde and higher oxygenates. A gas chromatographic system was developed to trap and analyze atmospheric organic compounds with HID detection. This required careful choice of the adsorbent material and removal of inorganic components (namely nitrogen and oxygen) before analysis. Real air samples were then taken and analyzed qualitatively for a range of olefinic and aromatic compounds.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 67
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 81-86 
    ISSN: 0935-6304
    Schlagwort(e): Available niacin ; capillary electrophoresis ; total niacin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Available and total niacin content in lentils and faba beans have been analyzed by capillary electrophoresis (CE), and the results compared with those obtained by high performance liquid chromatography (HPLC). Acidic and enzymatic hydrolysis have been carried out for available niacin determination, and an alkaline extraction performed for total niacin. The extracts were subsequently purified using a strong anion exchanger resin. Precise conditions for purification had to be worked out for each one of the two analytical methods (HPLC and CE). The HPLC analysis for available and total niacin was carried out in an ion-pair reverse phase column with UV detection at 261 nm. For the CE separation, the following conditions were employed: a 20 mM sodium tetraborate; 15 mM sodium dodecyl sulfate and 20% isopropyl alcohol solution as separation buffer; 30 kV and 25 or 30°C. Separation was carried out in a 70 cm effective length × 75 μm i.d. fused-silica capillary using on-column UV detection at 254 nm. The results obtained by CE for lentils and faba beans were similar to those obtained by HPLC.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 68
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 94-102 
    ISSN: 0935-6304
    Schlagwort(e): supercritical fluid chromatography ; experimental design optimization ; Diesel fuel ; group-type analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---An optimization procedure is presented for group-type analysis of diesel fuel by supercritical fluid chromatography using packed silica column and a mixed mobile phase. A set of five responses, four values of resolution of a performance mixture and analysis time, was modeled using a Doehlert matrix for experimental design. Optimized experimental conditions for the five responses were obtained from a response surfaces optimization, taking into account various constraints on SF6 content in mobile phase and analysis time. The predicted and experimental resolutions were in good agreement for the different optimized conditions and one of them was selected to for application to a given diesel fuel for comparison with the results obtained by SFC using pure CO2 and by HPLC. The conditions found in this study provide an alternative method for the determination of mono-, di-, and polyaromatic compounds in middle distillates.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
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  • 69
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 107-112 
    ISSN: 0935-6304
    Schlagwort(e): Linalool; linalyl acetate ; enantioseparation by enantioselective gas chromatography ; enantiomer distributions in natural products obtained by different extraction processes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The enantiomeric distributions of linalool and linalyl acetate in various natural products are measured by enantioselective gas chromatography on alkyl-substituted cyclodextrins. Different plant cultivars were investigated by four extraction processes: steam distillation, solvent extraction, supercritical fluid extraction, and headspace analysis. Careful attention must be paid to linalool which undergoes partial racemization under certain processing conditions. In most cases, enantiomeric distribution is a powerful tool for authenticity testing.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 70
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 121-123 
    ISSN: 0935-6304
    Schlagwort(e): gas chromatography ; capillary columns ; column efficiency ; column comparison ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The correct meaning of the the term “utilization of the theoretical efficiency” vs. the “coating efficiency” is explained.
    Zusätzliches Material: 1 Tab.
    Materialart: Digitale Medien
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  • 71
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 125-127 
    ISSN: 0935-6304
    Schlagwort(e): multidimensional gas chromatography ; self-made connectors ; effluent splitting ; press fit connectors ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 72
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 133-136 
    ISSN: 0935-6304
    Schlagwort(e): GC ; analysis of vegetable oil ; petroselinic acid ; butyl esters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 73
    ISSN: 0935-6304
    Schlagwort(e): Enantioselective multidimensional capillary gas chromatography (enantio-MDGC) ; stable isotope ratio mass spectrometry (IRMS) ; multidimensional gas chromatography coupled on-line with isotope ratio mass spectrometry (MDGC-IRMS) ; calibration; isotope discrimination ; authenticity control ; authentication of genuine flavor components ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Multidimensional gas chromatography coupled on-line with isotope ratio mass spectrometry (MDGC-IRMS) is presented as a powerful method for origin-specific analysis. Scope and limitations of this sophisticated coupling technique are discussed with regard to accuracy and precision.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 74
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 161-168 
    ISSN: 0935-6304
    Schlagwort(e): Capillary electrochromatography ; optimization ; mixture design ; DUP 654 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Capillary Electrochromatography (CEC) offers a rapid, economical, and efficient means for resolving nonionic compounds in the reversed phase mode on octadecylsilane (ODS) columns. A CEC optimization on a Hypersil ODS capillary column was employed to identify a suitable mobile phase for the pressure-driven (reversed phase ODS) separation of the anti-inflammatory 2-phenylmethyl-1-naphthol (DUP 654), and its related substances. The proportions of mobile phase modifiers methanol, acetonitrile, and water as well as pH were employed as variables in a stacked mixture design. Comparable response surface profiles were obtained for the CEC separations at pH 4 and pH 8. However, subtle differences were evident in the quality of separations obtained in the liquid chromatographic (LC) mode when using a specially-prepared column packed with exactly the same stationary phase as used in the CEC experiments. A mapping of the response surface for separations on a commercially available Hypersil ODS LC column revealed obvious differences. The differences indicate that the transfer of ODS based separation methods between CEC and LC involves more than simply transferring the conditions from one mode to the other.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 75
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 175-180 
    ISSN: 0935-6304
    Schlagwort(e): Supercritical Fluid Extraction (SFE) ; supercritical fluid chromatography ; solid trapping ; solvent trapping ; polymeric phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---One way of collecting extracted analytes after a supercritical fluid extraction (SFE) is to pass the depressurized fluid through a trap composed of a solid adsorbent. The influence of the adsorbent nature on the trap efficiency has been studied. First, the retention factors of each compound of a polarity test mix (tetracosane, naphthalene, fluoranthene, acetophenone, N,N-dimethylaniline, 2-naphthol, decanoic acid) have been determined on five high specific area (greater than 800 m2/g) polymeric phases by supercritical fluid chromatography (SFC). The comparison of this values with those obtained on octadecyl silica (ODS) showed that polymeric phases have the greatest retention power. After that, the efficiency of a solid trap filled with the greatest retention power polymeric adsorbent was evaluated by using pure carbon dioxide and 2.5%, 5%, 10%, and 20% methanol-modified carbon dioxide. As expected, this trap permitted a quantitative collection of all the former compounds even when a content as high as 10% of methanol was implemented. A solid trap filled with ODS adsorbent allowed quantitative collection of all the compounds only at a methanol content lower than 2.5%.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 76
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 185-188 
    ISSN: 0935-6304
    Schlagwort(e): Dill ether ; stereoselective synthesis ; dill ether stereoisomers ; enantioselective GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 77
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 197-199 
    ISSN: 0935-6304
    Schlagwort(e): Chiral recognition of 2-pentanol enantiomers ; enantioselective interactions ; capillary gas chromatography ; permethylated-β-cyclodextrin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 78
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 287-290 
    ISSN: 0935-6304
    Schlagwort(e): DNA ; capillary electrophoresis ; sample injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Silver-coated capillaries were used for direct sample injection in multiplexed capillary electrophoresis. The absence of an additional electrode simplifies mechanical alignment, reduces contamination, and decreases the amount of sample needed. Capillaries were coated by a silver paint which is a suspension of silver particles in an organic solvent. To provide electrical contact, the upper part of the capillary and a platinum wire were wound together by a copper wire. Electrical resistance from the platinum wire to the tip of the capillary was small enough (7 ω to 50 ω) to inject large amounts of DNA samples. Electrokinetic injection from eight separate sample vials to eight capillaries was demonstrated for DNA sequencing by multiplexed capillary electrophoresis. Signal-to-noise ratio and resolution were good enough to call up to 350 base pairs.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 79
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 481-490 
    ISSN: 0935-6304
    Schlagwort(e): solid-phase extraction ; estrogens ; urine ; solvation parameter model ; system maps ; gas chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A general model is presented for the prediction of experimental conditions for the isolation of organic compounds from aqueous solution by solid-phase extraction. The solvation parameter model is used to predict the variation of retention as a function of solvent composition from characteristic solute descriptors and combined with a frontal analysis model to adjust the predicted breakthrough volumes to account for the influence of the small number of theoretical plates characteristic of sorbent cartridges. System maps are used to determine breakthrough volumes for sample processing, the composition and volume of wash solvents for matrix simplification, and the composition and volume of eluting solvents. System maps are provided for an octadecylsiloxane-bonded silica sorbent with methanol and acetonitrile as cosolvents with water. These maps are used to calculate the experimental conditions for the isolation of estrogens from urine and the model validated by experimental verification of the model predictions. The proposed approach provides a simple theoretical framework for computer-aided method development in solid-phase extraction.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 80
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 427-434 
    ISSN: 0935-6304
    Schlagwort(e): Linear solvation energy relationship ; retention ; mobile phase ; stationary phase ; additives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Linear solvation energy relationships (LSERs) were used to delineate which specific intermolecular interactions are responsible for changes in retention for a variety of well characterized analytes when acidic and basic additives were used in reversed phase HPLC. The effects of trifluoroacetic acid, triethylamine and a combination of trifluoroacetic acid and triethylamine on the LSERs were compared to those observed in the absence of additives. These effects were examined using four different mobile phase modifiers and five different stationary phases. Trifluoroacetic acid alone and in combination with triethylamine produced LSER regression coefficients nearly identical to those obtained with no additive present in the mobile phase. Triethylamine alone produced different LSER regression coefficients from the other systems unless the mobile phase contained trifluoroethanol as the mobile phase modifier, or the stationary phase consisted of a polymeric support.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 81
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 498-504 
    ISSN: 0935-6304
    Schlagwort(e): Nonaqueous solvents ; capillary electrophoresis ; charge transfer complexation ; argentation ; silver ion ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---This study represents the first application of Ag(I) charge transfer complexation in nonaqueous capillary electrophoresis. This method applies the principles of argentation chromatography to nonaqueous electrophoretic separations and is termed “nonaqueous argentation electrophoresis”. Since the separations are performed in 100% nonaqueous media, the advantages of nonaqueous solvents, such as enhanced solubility and flexibility in selectivity enhancement, compared to an aqueous or mixed hydroorganic solvent, are realized. A variety of compounds were separated. Qualitatively, the separation of eleven sulfonamides in 100% acetonitrile is shown to improve greatly upon the addition of Ag(I). These results also show that nonaqueous argentation electrophoresis provides fast, well-resolved separations of compounds, such as N-containing heterocyclics, that can selectively complex with Ag(I). Migration data and separation selectivities of these compounds by nonaqueous argentation electrophoresis were compared to previous aqueous argentation electrophoresis results. Selectivities were found to be significantly different for the two separation media. Ag(I) complexation provides an effective means of manipulating selectivity in nonaqueous capillary electrophoresis.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
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  • 82
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 519-522 
    ISSN: 0935-6304
    Schlagwort(e): Supercritical Fluid Extraction (SFE) ; Micellar Eletrokinetic Capillary Chromatography (MEKC) ; Diuron ; sugar cane ; orange ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 83
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 509-512 
    ISSN: 0935-6304
    Schlagwort(e): Cholesterol oxidation ; gas chromatography ; oxysterols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---The performance of a fused silica column coated with 50% phenyl-/50% dimethyl-polysiloxane, characterized by a high thermal stability, was evaluated for the gas chromatographic determination of cholesterol oxidation products. A silylated mixture of eighteen oxysterol standards (0.1 mg/ml of each compound) was injected into the gas chromatographic system. The temperature was programmed from 230 to 260°C at 2.5°/min and then to 290°C at 1°/min; the injector and detector temperatures were set at 325°C, and the gas linear velocity was 22.8 cm/s. The column gave a fast (15 min) and satisfactory resolution of the main cholesterol oxides. Good separation of the hydroxy from the epoxy derivatives was achieved.The suitability of the method for the determination of oxysterols in food matrices was successfully tested on a saponified lipid extract from egg yolk powder, previously enriched and purified by NH2 solid phase extraction.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 84
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 531-539 
    ISSN: 0935-6304
    Schlagwort(e): gas chromatography ; carrier gas flow ; loss modified Poiseuille flow ; hold-up times ; peak widths ; velocity profiles ; permeability of helium through fused silica ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Hold-up times and peak widths have been measured in long fused silica GC capillary columns at high temperature with helium as the carrier gas. The results lead to the conclusion that the helium permeates through the column walls. The conventional Poiseuille theory of carrier gas flow has been extended to include this phenomenon. The resulting “loss modified Poiseuille” model, which uses literature values for the permeability of fused silica to helium, has been used to simulate the observed behavior. Good agreement between simulation and experiment validates the model. Simulations have been used to explore the effect of column permeability on hold-up times, peak widths, and velocity profiles over a broad range of column geometries.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 85
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 549-553 
    ISSN: 0935-6304
    Schlagwort(e): Hydroxytyrosol ; GC-MS ; wine ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Hydroxytyrosol (HTy) is a potent natural antioxidant found in olive oil and in mill waste waters. Although wines are rich in polyphenols, hydroxytyrosol has not been identified in wines so far. We have analyzed ten wines from different grape varieties grown in several Italian regions, using a gas-chromatograph coupled to a mass selective detector (GC-MS). Solid-phase extraction of wine samples was performed on a C18 column, with ethyl acetate used as eluting agent. Eluates were derivatized with bis(trimethylsilyl)trifluoroacetamide (BSTFA) and analyzed by GC-MS using one target and two qualifying ions. The detection limit was 15 pg/μL, with 49% average recovery. Under these experimental conditions hydroxytyrosol was detected in all wines analyzed. Its average concentrations in red and white wines were 4.0 mg/L and 1.9 mg/L, respectively.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 86
    ISSN: 0935-6304
    Schlagwort(e): Ligand-exchange chromatography ; dodecyl-norephedrine ; enantiomeric separation ; amino alcohol ; coating ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Underivatized aliphatic β-amino alcohols with a primary or secondary alcohol moiety were separated into enantiomers by high performance liquid chromatography using octadecylsilanized silica coated with N-n-dodecyl-(1R,2S)-norephedrine as the stationary phase and an aqueous solution containing copper(II) and barbital as the mobile phase.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 87
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 653-657 
    ISSN: 0935-6304
    Schlagwort(e): capillary electrophoresis ; mass spectrometry ; CE-MS ; amphetamines ; Ecstasy ; biological fluids ; urine ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---Capillary electrophoresis (CE) was interfaced with a quadrupole mass spectrometer, using pneumatically-assisted electrospray ionization (ESI) in order to analyze Ecstasy and derivatives in urine. The influence of the sheath liquid composition, including the type and the percentage of the organic solvent, as well as the nature of the conductive acid modifier, were examined in order to find optimal coupling conditions. A fractional factorial design was also used to optimize the electrospray experimental parameters, such as the nebulizing gas pressure, the electrospray voltage, the drying gas flow rate, the drying gas temperature, the skimmer voltage, and the sheath liquid flow rate. The separation conditions were optimized in terms of temperature, electrolyte concentration, percentage of organic modifier, as well as capillary type. Finally, the optimal CE-ESI-MS conditions were applied to the analysis of Ecstasy and other related amphetamines in urine samples, following a liquid-liquid extraction procedure.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 88
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 671-673 
    ISSN: 0935-6304
    Schlagwort(e): gas chromatography ; monosaccharides ; pentafluorobenzylhydroxylamine ; electron capture detector ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 89
    Digitale Medien
    Digitale Medien
    New York, NY [u.a.] : Wiley-Blackwell
    Biospectroscopy 4 (1998), S. 197-208 
    ISSN: 1075-4261
    Schlagwort(e): Raman spectroscopy ; protein-ligand interactions ; streptavidin complexes ; biotin analogues ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Biologie , Physik
    Notizen: Raman spectra of anhydrous complexes of streptavidin (Strep) with biotin (Bio) and some Bio analogues [Biotin methyl ester (MEBio), desthiobiotin (DEBio), 2′-iminobiotin (IMBio), and diaminobiotin (DABio)] were recorded. The vibrational results indicate that the interaction with some of these ligands is able to modify the overall structure of the protein and this binding results in a decrease in the βsheet content and an increase in the α-helix content. To further confirm the conformational changes of the protein structure due to Bio analogue binding, the curve-fitting analysis of the amide I Raman band of neat Strep and of the complexes were performed. The intensity ratio of the components due to the β-sheet and α-helix conformations decreased in the Strep-MEBio, Strep-IMBio (pH 11), and Strep-Bio systems, whereas in all the other systems the changes were not significant. This behavior differs from that of Avi bound to the same ligands and suggests that Strep and Avi differ in their binding selectivity. A good correlation was found between the secondary structure percentages of the Avi and of the Strep complexes and ΔG°. On the basis of this linear relationship, the vibrational results allow for an acceptable evaluation of the dissociation constants of the Strep complexes, not previously reported in the literature. The present results indicate a correlation between the type of interaction and the effects of the protein-substrate bonding on the overall structure of the proteins. The amino acid residues in the binding site appear to be positioned in a such a way as to provide a precise fit of Bio. Even slight change in the substrate structure causes a weakness in the strength of the binding. The vibrational results confirm that both the imidazolidinone and the thiophan rings are important in the Strep-Bio interactions, but the former is more responsible for the high affinity of the binding. One of the Tyr residues is hydrogen bound with the ureido ring and another Tyr could be involved in the binding pocket. Trp residues do not directly bind the ligand and probably stabilize other binding site residues which in turn interact directly with Bio. © 1998 John Wiley & Sons, Inc. Biospectroscopy 4: 197-208, 1998
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 90
    Digitale Medien
    Digitale Medien
    New York, NY [u.a.] : Wiley-Blackwell
    Biospectroscopy 4 (1998), S. 209-216 
    ISSN: 1075-4261
    Schlagwort(e): high pressure ; FTIR spectroscopy ; bovine pancreatic trypsin inhibitor ; hydrogen-deuterium exchange ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Biologie , Physik
    Notizen: Fourier transform infrared (FTIR) spectroscopy combined with resolution enhancement techniques, second-derivative and difference spectroscopies, have been used to characterize pressure-induced changes in the structural rearrangements of bovine pancreatic trypsin inhibitor (BPTI) in D2O solution at 25.0°C. According to the observed changes in the amide I′ band up to 550 MPa, the secondary structure elements of BPTI, such as the α-helix, 310-helix, β-sheet, and β-turn, are scarcely rearranged except for the loop structure of residues of 9-17 and 36-43. The polypeptide backbone is not extensively unfolded up to 550 MPa. The minor pressure-induced structural rearrangements are completely reversible. A further increase in pressure above 1000 MPa associated with the precipitation of BPTI in D2O buffer solution induces the partial structural rearrangements of the α-helix, β-turn and/or 310-helix, and β-sheet. The polypeptide backbone of BPTI is not fully unfolded even above 1000 MPa. Most of the protected backbone amide protons involved in the β-sheet remain intact in the pressure range where BPTI is not precipitated, while those involved in the α-helix and β-turn and/or 310-helix are exchanged with solvent deuterons. The protected backbone amide protons located near the surface regions are more easily exchanged with solvent deuterons by application of high pressure than those involved in the core. © 1998 John Wiley & Sons, Inc. Biospectroscopy 4: 209-216, 1998
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 91
    Digitale Medien
    Digitale Medien
    New York, NY [u.a.] : Wiley-Blackwell
    Biospectroscopy 4 (1998), S. 219-227 
    ISSN: 1075-4261
    Schlagwort(e): guanosine 5′-diphosphate ; guanosine 5′-triphosphate ; magnesium ; vibrational spectroscopy ; Raman spectroscopy ; FTIR ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Biologie , Physik
    Notizen: Raman and infrared spectra were examined for guanosine 5′-diphosphate (GDP) and guanosine 5′-triphosphate (GTP) in aqueous solution. The vibrational modes were assigned on the basis of isotopic frequency shifts and relative intensities in the Raman and infrared spectra. The observed frequency shifts on 18O isotope labeling made it possible to identify the bands from each phosphate group (α, β, γ). Frequency shifts were observed as Mg2+ complexes with GDP and GTP. The results suggested that Mg2+ binds to GDP in a bidentate manner to the α, β P · · O bonds and in a tridentate manner to the α, β and γ P · · O bonds of Mg·GTP. The results indicate that structure of Mg2+ coordinated to GTP in aqueous solution differs somewhat to that found for Mg·ATP. © 1998 John Wiley & Sons, Inc. Biospectroscopy 4: 219-227, 1998
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 92
    ISSN: 1075-4261
    Schlagwort(e): near-IR ; protein folding ; denaturation ; ribonuclease A ; overtone and combination bands ; 2-dimensional correlation analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Biologie , Physik
    Notizen: We introduce near-IR spectroscopy as an ancillary tool for monitoring structural changes of proteins in aqueous solution using ribonuclease A (RNase A) as a model protein. The thermal unfolding of RNase A results in clear spectral changes in the near-IR and the mid-IR regions. In the near-IR the most pronounced changes are observed in the spectral region between 4820 and 4940 cm-1. The strong N—H combination band found at 4867 cm-1 in the spectrum of native RNase A shifts to 4878 cm-1 upon thermal unfolding. Hydrogen-deuterium exchange experiments that validate the N—H character of this mode can also be used to estimate the number of unexchanged amide protons after exposure to D2O. The transition profiles and temperatures derived from the temperature dependence of the N—H combination mode were found to be practically identical with those derived from the temperature dependence of the C=O amide I band in the mid-IR region, demonstrating that the near-IR region can be used as a conformation-sensitive monitor for the thermally induced unfolding of proteins in H2O solution. A 2-dimensional correlation analysis was applied to the mid-IR and near-IR spectra of RNase A to establish correlations between IR bands in both regions. The correlation analysis demonstrates that the thermal unfolding of RNase A is not a completely cooperative process; rather it begins with some changes in β-sheet structure, followed by the loss of α-helical structures, and then ending with the unfolding of the remaining β-sheets. © 1998 John Wiley & Sons, Inc. Biospectroscopy 4: S19-S29, 1998
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 93
    ISSN: 1075-4261
    Schlagwort(e): 13C-NMR ; 57Fe-NMR ; ν(C—O) stretching vibration ; ν(Fe—C) stretching vibration ; heme proteins ; heme models ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Biologie , Physik
    Notizen: 13C- and 57Fe-NMR spectra of several carbon monoxide hemoprotein models with varying polar and steric effects of the distal organic superstructure, constraints of the proximal side, and solvent polarity are reported. The 13C shieldings of heme models cover a 4.0 ppm range that is extended to 7.0 ppm when several hemoglobin CO and myoglobin CO species at different pHs are included. Both heme models and heme proteins obey a similar excellent linear δ(13C) versus ν(C—O) relationship that is primarily due to modulation of π backbonding from Fe dπ to the CO π* orbital by the distal pocket polar interactions. There is no direct correlation between δ(13C) and Fe—C—O geometry. The poor monotonic relation between δ(13C) and ν(Fe—C) indicates that the iron-carbon π bonding is not a primary factor influencing δ(13C) and δ(57Fe). The δ(57Fe) was found to be extremely sensitive to deformation of the porphyrin geometry, and increased shielding by more than 600 ppm with increased ruffling was observed for various heme models of known X-ray structures. © 1998 John Wiley & Sons, Inc. Biospectroscopy 4: S57-S69, 1998
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 94
    ISSN: 1075-4261
    Schlagwort(e): nucleic acid ; conformation ; Raman spectroscopy ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Biologie , Physik
    Notizen: The structure of the packaged double-stranded DNA genome of bacteriophage T7 was compared to that of unpackaged T7 DNA using digital difference Raman spectroscopy. Spectral data were obtained at 25°C from native T7 virus (100 mg/mL), empty T7 capsids (50 mg/mL), and purified T7 DNA (40 mg/mL) in buffer containing 200 mM NaCl, 10 mM MgCl2, and 10 mM Tris at pH 7.5. At these conditions, the local conformation of T7 DNA was not affected by packaging. Specifically, the local B-form secondary structure of unpackaged T7 DNA, including furanose C2′-endo pucker, anti glycosyl torsion, Watson-Crick base pairing, and base stacking, were essentially fully (〉98%) retained when the genome was condensed within the viral capsid. However, the average electrostatic environment of T7 DNA phosphates was altered dramatically by packaging as revealed by large perturbations in the Raman bands associated with localized vibrations of the DNA phosphate groups. The change in the phosphate environment was attributed to Mg2+ ions that were packaged with the genomic DNA, and the observed Raman perturbations of genomic DNA were equivalent to those generated by a 50-100-fold increase in Mg2+ concentration in aqueous phosphodiester model compounds. The T7 data were qualitatively and quantitatively similar to those observed previously for packaged DNA of bacteriophage P22 and imply that genomic DNAs of T7 and P22 are both organized in a similar fashion within their respective capsids. The results show that the condensed genome does not contain kinks or folds that would disrupt the local B conformation by more than 2%. The present findings are discussed in relation to previously proposed models for condensation and organization of double-stranded and single-stranded viral DNA. © 1998 John Wiley & Sons, Inc. Biospectroscopy 4: S47-S56, 1998
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 95
    Digitale Medien
    Digitale Medien
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 36 (1998), S. 1025-1035 
    ISSN: 0887-6266
    Schlagwort(e): polymer thin films ; thermosets ; microelectronics ; moisture ; physical aging ; Physics ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: In polymers for microelectronics applications, moisture is known to have a deleterious effect upon device reliability. In this paper, the moisture transport behaviors of a newly developed family of all-aromatic and aromatic/aliphatic copolyester thermosetting films were described. The moisture uptake as a function of temperature, relative humidity, sample thickness, and processing conditions were presented via conjugate moisture sorption tests.1 It was found that the post curing near but below Tg resulted in an increase in both total moisture uptake and diffusion coefficient due to the effect of physical aging and the generation of sample defect volume. © 1998 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 36: 1025-1035, 1998
    Zusätzliches Material: 18 Ill.
    Materialart: Digitale Medien
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  • 96
    Digitale Medien
    Digitale Medien
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 36 (1998), S. 1061-1080 
    ISSN: 0887-6266
    Schlagwort(e): polymer blends ; dilatometry ; free volume ; specific volume ; excess volume ; compressibility ; thermal expansivity ; equation of state ; scaling parameters ; crystallinity ; glass transition ; Physics ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: Melt-miscible polymer blends of poly(ethylene oxide)/atactic poly(methyl methacrylate (PEO/a-PMMA)) were prepared by melt-mixing and characterized by pressure-volume-temperature (PVT) dilatometry in the pressure and temperature range of 0 to 200 MPa and 20 to 200°C, respectively. The PVT data were analyzed in terms of two equations of state (EOS). The empirical Tait EOS was applied in the glassy, semicrystalline, and equilibrium melt state, and the Simha-Somcynsky EOS theory was applied in the equilibrium melt and glassy state. The Simha-Somcynsky EOS theory contains a free volume function. The temperature, pressure, and composition dependence of the free volume fraction h calculated from the Simha-Somcynsky EOS theory was studied. As a function of blend composition we observe that the free volume fraction, thermal expansivity, and compressibility all deviate mainly positively from linearity while the specific volume deviates mainly negatively from linearity. These findings are reconciled with composition-dependent free volume parameters, the free volume and cell volume as well as with self- and cross-interaction parameters derived from the Simha-Somcynsky EOS theory as applied to polymer mixtures. Moreover, the pressure dependence of glass and melting transitions as well as crystallization kinetics have been investigated. © 1998 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 36: 1061-1080, 1998
    Zusätzliches Material: 18 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 97
    Digitale Medien
    Digitale Medien
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 36 (1998), S. 1201-1209 
    ISSN: 0887-6266
    Schlagwort(e): polymer electrolytes ; NMR ; conductivity ; glasses ; Arrhenius and VTF dependences ; Physics ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: We have studied the temperature variation of conductivity and 1H NMR linewidth of (PEG)xNH4ClO4 (x = 20, 30, 46, 100, 200, & 1000) polymer electrolyte systems. The temperature dependence of the conductivity shows two distinct behaviors, the low temperature VTF dependence crossing over to Arrhenius dependence at higher temperatures. The departure from the VTF behavior is found to be composition dependent. NMR spectra indicate the presence of large fractions of crystalline regions that start to melt around the crossover temperature. We understand the deviation from the VTF behavior as a consequence of this crystalline to elastomer transition. © 1998 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 36: 1201-1209, 1998
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 98
    Digitale Medien
    Digitale Medien
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 36 (1998), S. 1227-1233 
    ISSN: 0887-6266
    Schlagwort(e): FTIR spectroscopy ; isotactic polystyrene ; crystallization process ; induction period ; Physics ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: The melt crystallization process of isotactic polystyrene (i-PS) was studied by means of in situ Fourier transform infrared (FTIR) spectroscopy, with a focus on the conformational changes during the induction period. The spectra obtained during the induction period suggested the occurrence of some ordered structure that is characterized by higher regularity and packing of the helical moieties than observed in the melt. This ordered structure was clearly different from the amorphous structure, and close to the crystal structure. The Avrami analysis indicated that the formation process of the ordered structure at the late stage of the induction period is similar to the growth process of the crystallites after the induction period. © 1998 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 36: 1227-1233, 1998
    Zusätzliches Material: 10 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 99
    Digitale Medien
    Digitale Medien
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 36 (1998), S. 237-251 
    ISSN: 0887-6266
    Schlagwort(e): segmented ; polyurethanes ; crosslinked ; mechanical ; dielectric properties ; Physics ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: Mechanical and dielectric properties of two series of segmented polyurethanes having soft segment concentration of 50 and 70% and a varying degree of crosslinking through the hard segment were studied. The degree of crosslinking in each series was varied by varying the butane diol/trimethylol propane ratio in the chain extender mixture. Tensile strength, elongation at break decrease, but elastic recovery increases monotonically with increasing crosslinking. The plateau modulus in the dynamic mechanical test decreases and then increases with increasing TMP content. Crosslinking causes broadening of the soft segment glass transition as seen by permittivity and loss factor measurements. It also affects high temperature behavior (above the glass transition of the hard segment); it lowers permittivity, loss factor, and ionic conductivity. © 1998 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 36: 237-251, 1998
    Zusätzliches Material: 15 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 100
    Digitale Medien
    Digitale Medien
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 36 (1998), S. 2379-2391 
    ISSN: 0887-6266
    Schlagwort(e): block copolymer ; thermoplastic elastomer ; physical gel ; polymer micelle ; Physics ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: Thermoplastic elastomer gels (TPEGs) composed of a poly[styrene-b-(ethylene-co-butylene)-b-styrene] triblock copolymer and a low-volatility, midblock-compatible mineral oil have been investigated at different oil concentrations to ascertain the effect of composition on TPEG morphology and mechanical properties. The impact of thermal processing is also examined by comparing gels thermally quenched to 0°C or slowly cooled to ambient temperature. Transmission electron micrographs reveal that gels with 70 to 90 wt % oil exhibit styrenic micelles measuring ca. 24 nm in diameter. Variation in composition or cooling rate does not have any perceivable effect on micelle size or shape, whereas the rate at which the gels are cooled influences the extent of microstructural order and the time to rupture (tR) at constant strain. Dynamic rheological testing confirms the presence of a physically crosslinked network at TPEG compositions ranging from 70 to 90 wt % oil, independent of cooling rate. Results presented here suggest that the dynamic elastic shear modulus (G′) scales as tαR where α varies from 0.41 to 0.59, depending on cooling rate. © 1998 John Wiley & Sons, Inc. J. Polym. Sci. B Polym. Phys. 36: 2379-2391, 1998
    Zusätzliches Material: 12 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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