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  • Analytical Chemistry and Spectroscopy  (2,229)
  • Deutschland
  • 2000-2004  (104)
  • 1970-1974  (2,129)
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  • 1
    Electronic Resource
    Electronic Resource
    Determination of Pollutant Phenols by Capillary High-Performance Liquid Chromatography with UV Detection (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 367-372 
    Details
    ISSN: 0935-6304
    Keywords: Capillary HPLC ; gradient elution ; temperature programming ; phenolic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---This paper describes a liquid chromatographic method using a reversed phase capillary column coupled to an UV detector for the quantitation of thirteen pollutant phenols. Chromatographic separation was carried out with gradient elution at 25.0 ± 0.1°C. The two major anisocratic elution modes (gradient elution and temperature programming) were evaluated. The detection limit range was 10-81 pg (100 nL injected). The chromatographic method combined with liquid-liquid extraction was applied to analysis of these compounds in river water. Recoveries of 75-103% were achieved for most of them.
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  • 2
    Electronic Resource
    Electronic Resource
    Use of Capillary Supercritical Fluid Chromatography in the Analysis of Zinc Dialkyldithiophosphates (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 389-392 
    Details
    ISSN: 0935-6304
    Keywords: Capillary SFC ; zinc dialkyldithiophosphates ; lubricating oils ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No abstract
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  • 3
    Electronic Resource
    Electronic Resource
    Application of Supercritical Fluid Chromatography to the Analysis of Waxes in Objects of Art (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 393-396 
    Details
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography (SFC) ; micropacked capillary columns ; waxes ; restoring ; objects of art ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No abstract
    Additional Material: 2 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Identification of Free and Glycosidically Bound Volatiles and Glycosides by Capillary GC and Capillary GC-MS in “Lulo del Chocó” (Solanum topiro) (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 379-385 
    Details
    ISSN: 0935-6304
    Keywords: Aroma ; “lulo del Chocó” ; Solanum topiro ; volatiles ; glycosidically bound volatiles ; glycoside TFA derivatives ; enantioselective gas chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The volatile constituents of lulo del Chocó (Solanum topiro) fruit pulp obtained by liquid-liquid extraction were analyzed by capillary GC and capillary GC-MS. In total, 30 components were identified with methyl salicylate, hexadecanoic acid, hexanal, guaiacol, ethyl butanoate, and ethyl acetate being the major components. Chirospecific MDGC analysis revealed the predominance of (R)-ethyl-3-hydroxybutanoate (ee 40%) and the presence of racemic mixtures both of δ-octalactone and of δ-decalactone. For γ-hexalactone, γ-octalactone, and γ-decalactone enantiomeric distributions of 22.4 : 77.6, 22.9 : 77.1, and 20.0 : 80.0, (R) : (S), respectively, were determined. Glycosidically bound aroma compounds were identified by capillary GC and capillary GC-MS after isolation of the glycosidic fraction obtained by Amberlite XAD-2 adsorption and methanol elution followed by hydrolysis with a commercial pectinase enzyme. In total 13 bound aroma compounds (aglycones) were identified. These aglycones mainly consisted of compounds exhibiting aromatic structures. Additionally, with the aid of capillary GC and capillary GC-MS (EI and NCI) of trifluoroacetylated derivatives we identified eight glucosides: the novel 3,6-epoxy-7-megastigmen-5,9-diol β-D-glucopyranoside and the hexyl, benzyl, linalyl oxide (furanic), 2-phenylethyl, vomifolyl (isomer 1), (6S,9R)-vomifolyl, and scopoletin β-D-glucopyranosides.
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  • 5
    Electronic Resource
    Electronic Resource
    System Peaks of Cyclodextrins in Capillary Electrophoresis (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 409-412 
    Details
    ISSN: 0935-6304
    Keywords: Cyclodextrin ; capillary electrophoresis ; system peak ; CHES 1 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Using a running buffer containing cyclodextrins (CDs) and 2-[N-cyclohexylamino]-ethanesulfonic acid (CHES), positive system peaks were observed in the analysis of a ganglioside mixture by CE-UV. These system peaks were related to CDs in the running buffer because these peaks were also detected when a plug of solution devoid of CDs but having the same CHES concentration and pH as the running buffer was injected. Neutral CDs were separated owing to the formation of inclusion complexes with the anionic CHES ion. One possible explanation for the positive system peaks is that the anionic CD-CHES inclusion complex is displaced by co-ions with higher UV absorptivity.
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  • 6
    Electronic Resource
    Electronic Resource
    Liquid Chromatography of Unstable Zinc Dithiocarbamates. Application to Rubber Gloves Analysis (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 565-566 
    Details
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; zinc dithiocarbamate ; vulcanization accelerator ; rubber gloves ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No abstract
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  • 7
    Electronic Resource
    Electronic Resource
    Characteristic Stationary Phase Constants for Two Popular Open-Tubular Column Stationary Phases for Gas Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 603-608 
    Details
    ISSN: 0935-6304
    Keywords: Solvation parameter model ; ystem constants for poly(dimethyldiphenylsiloxane) HP-5 and poly(ethylene glycol) HP-INNOWax stationary phases ; temperature ; molecular interaction ; retention models ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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  • 8
    Electronic Resource
    Electronic Resource
    Determination of Cinnamomi Constituents by High-performance Liquid Chromatography and Capillary Electrophoresis (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 561-564 
    Details
    ISSN: 0935-6304
    Keywords: Retention factors ; Cinnamomi ramulus ; high-performance liquid chromatography ; capillary electrophoresis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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  • 9
    Electronic Resource
    Electronic Resource
    Ion Chromatography of Inorganic Anions on Graphitic Carbon as the Stationary Phase (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 590-594 
    Details
    ISSN: 0935-6304
    Keywords: Ion chromatography ; graphitic carbon stationary phases ; anions ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Inorganic anions could be separated on porous graphitic carbon stationary phases in ion chromatography. Ion exchange between eluent anions and sample anions on the stationary phase was confirmed by the retention behavior and the possibility of indirect photometric detection. The elution order of anions was different from that observed for commercially available anion exchangers. Chloride, nitrate, and sulfate contained in tap water could be determined in 7 min.
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  • 10
    Electronic Resource
    Electronic Resource
    Solid-Phase Microextraction of Pyrethroid Pesticides from Water at Low and Sub-ppt Levels at Different Temperatures (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 485-488 
    Details
    ISSN: 0935-6304
    Keywords: Pyrethroids ; solid-phase microextraction ; water analysis ; temperature ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Synthetic pyrethroids are increasingly being used for insect control on field crops because of their advantageous environmental properties such as short field life, broad spectrum of insecticide activity, and relatively low mammalian toxicity. In the present work, experimental conditions were optimized for trace analysis of pyrethroids in water by using solid-phase microextraction followed by capillary gas chromatography. Effects of temperature, SPME-fiber diameter, and matrix were studied. SPME used off-line with a gas chromatograph electron-capture detection (GC-ECD) showed a linear response over a wide concentration range. Our results showed a strong temperature effect on pyrethroid extraction yield. The detection limit after 5 min of SPME-fiber exposure to the samples changed from 1 ppb (at 30°C) to 0.1 ppt (at 90°C), which is a 10000 increase in pyrethroid detection. The standard deviations of the analyte peak area ratios were typically in the range of 1-7% at 30°C and of 3 to 15% at 90°C. Best conditions for pyrethroids analysis were achieved using high temperature solution and a 100 μm polydimethylsiloxane fiber. No matrix (river water) influence was observed on detection of the investigated pyrethroids.
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  • 11
    Electronic Resource
    Electronic Resource
    Microfabricated Monolith Columns for Liquid Chromatography. Sculpting Supports for Liquid Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 19-26 
    Details
    ISSN: 0935-6304
    Keywords: Microfabrication ; monolith ; electrochromatography ; peptides ; reactive ion etching ; reversed phase ; nanocolumns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Monolith columns are generally fabricated by polymerization of monomers within a column. This paper reviews an alternative strategy in which the bed is microfabricated in an inorganic material by ablation. Channels of 1.5 μm width and 10 μm depth were sculpted in quartz by deep reaction ion etching. Using this approach chromatographic beds were constructed in which cubic support structures were created and arranged in rows to mimic particles in a conventional column. Beds ranging from hundreds of thousands to millions of “particles” with volumes of 15 nL to 15 μL were produced. Columns that had been derivatized with an octadecyl silane stationary phase were used to separate both low molecular weight analytes and peptides in the CEC mode. Plate height in the CEC mode was 1.2 μm at maximum efficiency.
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  • 12
    Electronic Resource
    Electronic Resource
    Dynamic Capacity Studies of CIM (Convective Interaction Media)® Monolithic Columns (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 39-43 
    Details
    ISSN: 0935-6304
    Keywords: Monoliths ; CIM® monolithic column ; dynamic binding capacity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The characterization of CIM® DEAE monolithic columns in terms of dynamic binding capacity is presented in this paper. Breakthrough experiments were performed for capacity determination. Bovine serum albumin (BSA) was used as a model protein. It is shown that CIM® monolithic columns have good batch-to-batch reproducibility as well as long-term stability. The experiments performed under different linear velocities demonstrated that the dynamic capacity is unaffected at least up to a linear velocity of 2450 cm/h. Furthermore, the breakthrough curve slope is constant, indicating that the capacity would remain constant at even higher linear velocities. The adsorption isotherm of BSA dissolved in 20 mM Tris-HCl buffer shows a constant capacity of around 30 mg/mL of support down to a concentration of 20 μg/mL. The capacity is substantially influenced by the ionic strength; however, 20% of the maximal capacity is still preserved at 0.3 M NaCl.
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  • 13
    Electronic Resource
    Electronic Resource
    Affinity Chromatography of Human Blood Coagulation Factor VIII on Monoliths with Peptides from a Combinatorial Library (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 47-58 
    Details
    ISSN: 0935-6304
    Keywords: Monolith ; factor VIII ; affinity chromatography ; combinatorial peptide library ; peptide synthesis ; recombinant proteins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: FVIII is a very complex molecule of great therapeutic significance. It is purified by a sequence of chromatographic steps including immunoaffinity chromatography. A peptide affinity chromatography method has been developed using peptides derived from a combinatorial library. Spot technology using cellulose sheets has been applied for this purpose. The dual positional scanning strategy was used for identification of the amino acids in random positions. Approximately 5000 possible candidates found in the first screening round were reduced to a panel of 36. Six candidates have been selected empirically. Five peptides seem to be directed against the light chain of FVIII, one peptide seems to be directed against the heavy chain. The peptides have been immobilized on conventional beaded material and CIM polymethacrylate monoliths. Much better performance with respect to capacity and selectivity has been observed with the monolithic material. Exposure of the ligand and its ensuing accessibility are responsible for these properties.
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  • 14
    Electronic Resource
    Electronic Resource
    Capillary Electrochromatography with Monolithic Poly(styrene-co-divinylbenzene-co-methacrylic acid) as the Stationary Phase (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 67-72 
    Details
    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; monolithic column ; electroosmotic flow ; retention mechanism ; aromatic compound ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A new kind of monolithic capillary electrochromatography column with poly(styrene-co-divinylbenzene-co-methacrylic acid) as the stationary phase has been developed. The stationary phase was found to be porous by scanning electron microscopy and the composition of the continuous bed was proved by IR spectroscopy to be the ternary polymer of styrene, divinylbenzene, and methacrylic acid. The effects of operating parameters, such as voltage, electrolyte, and organic modifier concentration in the mobile phase on electroosmotic flow were studied systematically. The retention mechanism of neutral solutes on such a column proved to be similar to that of reversed-phase high performance liquid chromatography. In addition, fast analyses of phenols, chlorobenzenes, anilines, isomeric compounds of phenylenediamine and alkylbenzenes within 4.5 min were achieved.
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  • 15
    Electronic Resource
    Electronic Resource
    Continuous-Bed Columns Containing Sol-Gel Bonded Packing Materials for Capillary Electrochromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 73-80 
    Details
    ISSN: 0935-6304
    Keywords: Continuous-bed ; sol-gel ; octadecylsilica ; mixed-mode stationary phase ; large-pore ; column technology ; capillary electrochromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Sol-gel bonded packing materials in continuous-bed columns have been prepared for capillary electrochromatography (CEC). Three packing materials were investigated: small-pore Spherisorb ODS1 (3 μm, 80 Å) with octadecyl as stationary phase, small-pore mixed-mode Spherisorb ODS/SCX (3 μm, 80 Å) with octadecyl and propyl sulfonic acid as stationary phases, and large-pore Nucleosil ODS (7 μm, 1 400 Å) with octadecyl as stationary phase. The characteristics of these columns were compared in terms of electroosmotic flow, efficiency, inertness, and retention factors. In contrast to columns containing sol-gel bonded ODS, columns containing sol-gel bonded mixed-mode ODS/SCX generated nearly pH independent electroosmotic flow (EOF) over pH 2-9. Columns containing sol-gel bonded large-pore ODS produced nearly three times lower reduced plate height than those containing small-pore ODS. Efficiencies of 220,000 plates per meter and 175,000 plates per meter were obtained from columns containing sol-gel bonded 7 μm, 1 400 Å ODS and columns containing sol-gel bonded 3 μm, 80 Å ODS, respectively, which are among the highest reported efficiencies for continuous-bed columns. In CEC, over one million plates per meter and pH independent EOF are expected from continuous-bed columns containing sol-gel bonded 1.5 μm particles with large pores and mixed-mode stationary phases.
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  • 16
    Electronic Resource
    Electronic Resource
    Particle Loaded Monolithic Sol-Gel Columns for Capillary Electrochromatography: A New Dimension for High Performance Liquid Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 81-88 
    Details
    ISSN: 0935-6304
    Keywords: Monolithic chromatography columns ; capillary electrochromatography (CEC) ; micro high performance liquid chromatography ; sol-gel based columns for chromatography ; fritless capillary chromatography columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Particle-loaded (3 μm, octadecylsilica) monolithic sol-gel columns have been prepared and selected characteristics measured. Several electrical properties may be calculated from simple current measurements in the column as a whole. Resistivity in the packed segment is approximately three times that in open segments, resulting in a 60% increase in field strength in the packed regions compared to the capillary with no packing. The surprisingly high specific permeability of these sol-gel columns is characteristic of 8-μm particles, which allows their operation in the microLC mode at pressures as low as 69 kPa where their efficiency is about 50,000 plates per meter and in the CEC mode where efficiency is about 106,000 plates per meter at 5 kV. There is a relatively rapid loss of efficiency with increasing linear velocity beyond 0.2 mm/s in microLC mode, which may be due to additional diffusion processes in the inter-particulate voids. A rapid loss of efficiency above 0.5 mm/s is also observed in the CEC mode, for the same reasons. Chromatographic retention behavior in either separation mode is characteristic of conventional octadecylsilica particles, indicating that analytes have significant access to the surface within the pores of the immobilized bonded phase.
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  • 17
    Electronic Resource
    Electronic Resource
    Preparation of Fritless Packed Silica Columns for Capillary Electrochromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 89-92 
    Details
    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; packed columns ; fritless columns ; stationary phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Fritless packed silica gel columns were prepared using sol-gel technology. A part of a 75 μm i.d. fused silica capillary was filled with a mixture of tetramethoxysilane and poly(ethylene glycol). After gelling at 40°C and heating at 300°C, the resultant silica gel was derivatized with dimethyloctadecylchlorosilane. A scanning electron micrograph of a cross-section of the capillary column showed that the gel took the form of a spherical particle aggregate and adhered to the column inner wall. The column performance was evaluated for electrochromatography using acetonitrile-50 mM HEPES buffer (pH 6.6) (60/40 or 40/60, v/v) as the mobile phase. An electroosmotic flow of 1.0 mm/s was generated with (60/40, v/v) acetonitrile/HEPES buffer at a field strength of 546 V/cm. Using a sol-gel-derived packed column at an electroosmotic flow of 0.5 mm/s, efficiencies of up to 1.1×105 plates/m were obtained for retained solutes.
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  • 18
    Electronic Resource
    Electronic Resource
    A New Monolithic-Type HPLC Column For Fast Separations (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 93-99 
    Details
    ISSN: 0935-6304
    Keywords: HPLC ; monolithic column ; silica rod column ; fast separations ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The application of a new silica-based, monolithic-type HPLC-column for fast separations is presented. The column is prepared according to a new sol-gel process, which is based on the hydrolysis and polycondensation of alkoxysilanes in the presence of water soluble polymers. The method leads to “rods” made of a single piece of porous silica with a defined pore structure, i. e. macro- and mesopores. The main feature of silica rod columns is a higher total porosity, about 15% higher than of conventional particulate HPLC columns. The resulting column pressure drop is therefore much lower, allowing operation at higher flow rates including flow gradients. Consequently, HPLC analysis can be performed much faster, as it is demonstrated by various applications.
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  • 19
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    Monolithic Stationary Phases for Capillary Electrochromatography Based on Synthetic Polymers: Designs and Applications (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 3-18 
    Details
    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; monolithic columns ; synthetic polymers ; stationary phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Monolithic materials have quickly become a well-established stationary phase format in the field of capillary electrochromatography (CEC). Both the simplicity of their in situ preparation method and the large variety of readily available chemistries make the monolithic separation media an attractive alternative to capillary columns packed with particulate materials. This review summarizes the contributions of numerous groups working in this rapidly growing area, with a focus on monolithic capillary columns prepared from synthetic polymers. Various approaches employed for the preparation of the monoliths are detailed, and where available, the material properties of the resulting monolithic capillary columns are shown. Their chromatographic performance is demonstrated by numerous separations of different analyte mixtures in variety of modes. Although detailed studies of the effect of polymer properties on the analytical performance of monolithic capillaries remain scarce at this early stage of their development, this review also discusses some important relationships such as the effect of pore size on the separation performance in more detail.
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  • 20
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    Preparative Monolithic Silica Sorbents (PrepRODs™) and Their Use in Preparative Liquid Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 100-105 
    Details
    ISSN: 0935-6304
    Keywords: Preparative chromatography ; silica monoliths ; PrepROD™ ; productivity ; SMB-chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The use of monolithic silica sorbents for the isolation of substances by preparative liquid chromatography is demonstrated. Preparative liquid chromatography is recognized as a valuable technique for the isolation and purification of substances in the pharmaceutical and fine chemicals industry. The system technology has meanwhile reached a high standard, and the greatest future improvements are expected to arise from new and improved adsorbents. Monolithic silica sorbents offer some unique features for preparative liquid chromatography. They exhibit high efficiencies even at high flow rates due to their fast convective mass transfer and can therefore be used at very high mobile phase velocities, leading to high productivity and hence to maximum process economy. The benefits of this new type of adsorbent are illustrated for an example in batch-chromatographic mode and an example using the continuous simulated moving bed (SMB) technology.
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  • 21
    Electronic Resource
    Electronic Resource
    Tailoring Mesopores in Monolithic Macroporous Silica for HPLC (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 106-110 
    Details
    ISSN: 0935-6304
    Keywords: Silica ; monolithic column ; aging ; mesopores ; pore size distribution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Mesopore formation in silica gels having continuous macropores has been investigated. The macroporous wet silica gel prepared by the sol-gel process including phase separation was aged in a basic solvent making use of hydrolysis of urea in a closed condition. The mesopore structure was finally obtained by subsequent evaporation drying of solvent and heat-treatment at 600°C for 2 h. The dissolution-reprecipitation kinetics at the interfaces between wet gel skeletons and an external solvent affected the size and volume of pores formed within the skeletons. Below 120°C, mesopores suitable for various chromatographic applications have been formed typically within 24 h. On the other hand, at 200°C, the pore size attained the macropore dimensions (〉50 nm), and the whole macroporous morphology was significantly modified.
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  • 22
    Electronic Resource
    Electronic Resource
    Monolithic Silica Columns for HPLC, Micro-HPLC, and CEC (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 111-116 
    Details
    ISSN: 0935-6304
    Keywords: Monolithic column ; silica monolith ; HPLC ; capillary liquid chromatography ; capillary electrochromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Two types of monolithic silica columns derivatized to form an ODS phase, one prepared in a fused silica capillary (SR-FS) and the other prepared in a mold and clad with an engineering plastic (poly-ether-ether-ketone) (SR-PEEK), were evaluated. The column efficiency and pressure drop were compared with those of a column packed with 5-μm ODS-silica particles and of an ODS-silica monolith prepared in a mold and wrapped with PTFE tubing (SR-PTFE). SR-FS gave a lower pressure drop than a column packed with 5-μm particles by a factor of 20, and a plate height of 20 μm at a linear velocity below 1 mm/s. SR-PEEK showed higher flow-resistance than the other monolithic silica columns, but they still showed a minimum plate height of 8-10 μm and a lower pressure drop than popular commercial columns packed with 5-μm particles. The evaluation of SR-FS columns in a CEC mode showed much higher efficiency than in a pressure-driven mode.
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  • 23
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    Note on the Net Retention Volume in Chromatography with a Real Gas as a Carrier (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 119-126 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography ; retention volume ; real gas carrier ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The problem of the calculation and interpretation of the net retention volume with a real gas as carrier is revisited. The properties of the carrier are described by a first order virial equation of state. The net retention volume of a solute is related to the mean flow rate of the carrier, therefore determination of the mean flow rate of a real gas carrier is reviewed. It is shown that the mean flow rate cannot be calculated from the mean column pressure. With a real gas carrier the local capacity factor depends on the local pressure of the real gas. The basic relationship between the net retention volume and the function describing this pressure dependence is also reviewed. Precise formulae as well as practical approximations are presented for the calculation of the mean flow rate, of the mean column pressure, and of a representative pressure related to the mean capacity factor.
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    Detection of Polyols by HPLC Coupled with an On-Line Photochemical Oxidation Reactor and Chemiluminescence Detection (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 127-130 
    Details
    ISSN: 0935-6304
    Keywords: Chemiluminescence ; diol compound ; oxalate ; post-column reaction ; ruthenium complex ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---In this paper we propose a new post-column detection method for polyols containing 1,2-diol, 1,3-diol, and saccharides. The polyols are oxidized in a photochemical reactor to yield oxalate with subsequent chemiluminescence detection using [Ru(III)(bpy)3]3+. A mixing solution of eluate and oxidizing reagent is delivered to a reaction coil, which is then irradiated with ultraviolet light to promote the oxidation reaction. The detection limits for 1,2-ethanediol (ethylene glycol) and 1,3-propanediol were 38 pmol and 23 pmol, respectively.
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    Coupled LC-GC-NPD for Determination of Carbazole-Type PANH and Its Application to Personal Exposure Measurement (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 131-137 
    Details
    ISSN: 0935-6304
    Keywords: On-line coupled LC-GC ; nitrogen selective detection ; NPD ; carbazoles ; PANH ; personal exposure measurement ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A coupled LC-GC method for the analysis of carbazole-type PANH has been developed and evaluated. Group separation and isolation of carbazoles from interfering acridines in a complex sample matrix was accomplished by using a back-flush technique and an in situ end-capped dimethylaminopropyl silica column in the HPLC part of the system. On-line injection of the carbazole fraction into the GC column was performed with a loop-type interface utilizing concurrent solvent evaporation technique. An LOD of 1-3 pg of individual carbazole compounds was achieved by nitrogen selective detection using an NPD. The method is shown to be robust and is demonstrated by application to personal exposure measurement in an aluminum reduction plant.
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    Fast Separation of Nucleosides by Capillary Electrochromatography on Non-Endcapped Phenyl-Bonded Silica Phase Using Short-End Injection Method (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 138-142 
    Details
    ISSN: 0935-6304
    Keywords: Capillary electrochromatography ; nucleosides ; short-end injection ; phenyl-bonded silica ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The influence of several experimental parameters (pH, ionic strength, organic modifier content of hydro-organic buffer) upon EOF, migration time, and retention factor has been studied in CEC with a phenyl-bonded silica column on a model mixture of five nucleosides. This paper illustrates the current interest in CEC as a method of resolving complex mixtures of neutral and ionic solutes and demonstrates the potential of the short-end injection method as a means of reducing analysis time.
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    Separation of Anthraquinones by Capillary Electrophoresis and High-Performance Liquid Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 143-148 
    Details
    ISSN: 0935-6304
    Keywords: Analysis of anthraquinones ; capillary electrophoresis ; high-performance liquid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The separation and determination of twelve anthraquinones, viz. anthraquinone 1, chrysphanol 2, aloe-emodin 3, alizarin 4, anthraquinone-2-carboxylic acid 5, purpurin 6, sennoside B 7, sennoside A 8, emodin 9, quinalizarin 10, rhein 11, and anthraflavic acid 12, were achieved by capillary electrophoresis (CE) and high-performance liquid chromatography (HPLC). Detection at 260 nm with a buffer solution containing 30 mM sodium borate (adjusted to pH = 10.56 with 0.05N NaOH) and acetonitrile (9 : 1) in CE or with a linear gradient elution containing 20 mM KH2PO4 with 0.05% phosphoric acid (pH = 2.91) and methanol in HPLC was found to be the most suitable approach for this separation. Contents of six components (2, 3, 7, 8, 9, 11) in crude Rhei Rhizoma extract could easily be determined within 39 min by CE or 63 min by HPLC. The effects of buffers on this separation and the validation of the two methods were studied.
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    Capillary Gas Chromatography of Trichlorophenols Using Ammonia as Carrier Gas (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 156-157 
    Details
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; trichlorophenols ; ammonia ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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    Large Volume Injection in Fast Gas Chromatography with On-Column Injector (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 149-155 
    Details
    ISSN: 0935-6304
    Keywords: Capillary GC ; fast GC ; on-column injection ; narrow-bore column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---In this work a fast gas chromatography set-up with on-column injection was optimized and evaluated with a model mixture of C8-C28 n-alkanes. Usual injection volumes when using narrow-bore (e. g., 0.1 mm i.d.) analytical columns are ca. 0.1 μL. The presented configuration allows introduction of 10-30-fold larger sample volumes without any distortion of peak shapes. In the set-up a normal-bore retention gap (1 m×0.32 mm i. d.) was coupled to a narrow-bore (4.8 m×0.1 mm i. d.×0.4 μm film thickness) analytical column using a low dead volume column connector. The effects of the experimental conditions such as inlet pressure, sample volume, initial injection temperature, and oven temperature on a peak focusing are discussed. H-u curves for helium and hydrogen are used to compare their suitability for high speed gas chromatography and to show the dependence of separation efficiency on the carrier gas velocity at high inlet pressures. In the fast gas chromatography system a baseline separation of C10-C28 n-alkanes was achieved in less than 3 minutes.
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    Proper Tuning of Comprehensive Two-Dimensional Gas Chromatography (GC×GC) to Optimize the Separation of Complex Oil Fractions (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 182-188 
    Details
    ISSN: 0935-6304
    Keywords: Comprehensive two-dimensional gas chromatography ; GC×GC ; thermal modulation ; oil analysis ; petroleum analysis ; analysis of middle-distillate oil fractions ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Comprehensive two-dimensional gas chromatography (GC×GC) is an utterly suitable separation technique for the analysis of complex samples, such as oil fractions. Once the two columns and the operating conditions are properly tuned, the technique is able to provide a detailed characterization of such materials. Some considerations applying to the tuning of a GC×GC system for a specific separation are presented and discussed. The authors present a number of different column sets and conditions which allow the separation of a non-aromatic hydrocarbon solvent, a kerosene, the light end of a crude oil, and an olefinic fraction, respectively. The highly structured GC×GC chromatograms, together with chemical knowledge about the samples, provide a much more comprehensive characterization of the samples than hitherto possible.
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    Comprehensive Two-Dimensional Gas Chromatography with a Rotating Thermal Desorption Modulator and Independently Temperature-Programmable Columns (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 189-196 
    Details
    ISSN: 0935-6304
    Keywords: Comprehensive two-dimensional gas chromatography ; thermal desorption modulator ; temperature programming ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---In comprehensive two-dimensional gas chromatography, two individual separations are coupled by means of a rotating thermal desorption modulator interface. The injection pulse introduced via the interface onto the second column should be as short as possible. Parameters affecting the modulator operation are studied. In the set-up used in this study, the temperature of the second column can be programmed independently from that of the first column. Optimization of the second-dimension separation to minimize peak broadening and maximize resolution is discussed and an elegant approach to determine second-dimension retention times using a non-constant modulation frequency is demonstrated. The high separation power of the comprehensive system is demonstrated by the analysis of technical and biota samples containing chlorinated biphenyls and toxaphene.
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    Determination of Oxygenates in Gasoline by GC×GC (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 197-201 
    Details
    ISSN: 0935-6304
    Keywords: Multidimensional gas chromatography ; comprehensive two-dimensional gas chromatography ; GC×GC ; oxygenates ; MTBE ; reformulated gasoline ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Comprehensive two-dimensional gas chromatography (GC×GC) has been applied to the quantitation of oxygenates in reformulated gasoline. Target oxygenates were C1-C4 alcohols, tert-pentanol, methyl tert-butyl ether (MTBE), diisopropyl ether (DIPE), ethyl tert-butyl ether (ETBE), and tert-amyl methyl ether (TAME). These were separated from the gasoline matrix using a volatility-based selectivity in the first chromatographic dimension, followed by a mixed-phase polarity/shape selectivity in the second dimension. The high resolving power of this stationary phase combination completely separated all oxygenates except DIPE, ETBE, and TAME, which exhibited coelution with other nonpolar gasoline components. Oxygenates quantitation was achieved with the use of an internal standard, an FID detector, and calibration curves. Quantitation results are in good agreement with ASTM and EPA standard methods. When coupled with our previous method for BTEX and aromatics, a single GC×GC method can now quantitate MTBE, alcohols, BTEX, and aromatics in a one-hour analysis.
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    Biodegradation of Pharmaceutical Residues Investigated by SPE-GC/ITD-MS and On-Line Derivatization (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 474-478 
    Details
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Solid-phase extraction, on-line derivatization, and measurement by ion trap mass spectrometry (ITD-MS) were used to investigate the biological degradation of pharmaceutical residues (clofibric acid, ibuprofen, diclofenac). The results of the single steps of sample pretreatment and analytical determination are reported. MS/MS measurements were performed on an ITD-MS by selecting collision induced dissociation of the molecular ions (M+) as parent ions to defined daughter ions. A pilot sewage plant and biofilm reactors operating under oxic and anoxic conditions were run as model systems with synthetic sewage water containing 10 to 50 mg/L dissolved organic carbon (DOC) and pharmaceuticals in concentrations of 10 μg/L. Clofibric acid displayed its persistent character in all cases. The pilot sewage plant and the oxic biofilm reactor showed comparable results for diclofenac and ibuprofen, which both were partly degraded. These results can explain the occurrence of these substances in sewage effluents and in the aquatic environment. A high degree of degradation was found especially for ibuprofen in the oxic biofilm reactor, which was attributed to adaptation of the biofilm to the residue. Two metabolites of ibuprofen could be identified on the basis of their mass spectra and comparison with literature data, viz. hydroxyibuprofen and carboxyibuprofen.
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    Characterization of Polydimethylsiloxanes Using an Off-Line Combination of Supercritical Fluid Chromatography with Matrix-Assisted Laser Desorption Ionization Mass Spectrometry (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 502-506 
    Details
    ISSN: 0935-6304
    Keywords: Silicone oil ; supercritical fluid chromatography (SFC) ; micropacked columns ; MALDI-TOF ; GC/MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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    Separation and Detection of Metal Ions in Ecological Samples by Capillary Zone Electrophoresis with Indirect UV Detection (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 511-514 
    Details
    ISSN: 0935-6304
    Keywords: CZE ; indirect UV detection ; metal ions ; ecological samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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    Solventless Sample Preparation Techniques in Environmental Analysis (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 297-303 
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    ISSN: 0935-6304
    Keywords: Sample preparation ; gas extraction techniques ; membrane-type techniques ; water analysis ; soil analysis ; gas chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---This review focuses on the role of so-called solventless methods of sample preparation in contemporary environmental analysis. The basic classification of this group of methods as well as the principal features and advantages of the techniques in current use are discussed.
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    Comparison of Thermal Sweeper and Cryogenic Modulator Technology for Comprehensive Gas Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 253-258 
    Details
    ISSN: 0935-6304
    Keywords: Comprehensive gas chromatography ; cryogenic modulation ; semi-volatile aromatics ; thermal sweeper ; peak widths ; peak asymmetries ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The two current technologies for achieving comprehensive gas chromatography (GC×GC) - the thermal sweeper and the cryogenic modulator - are compared in an interlaboratory study using a multicomponent semi-volatile aromatic compound sample. The same column set (phases, film thickness, dimensions of columns) and conditions of oven temperature program were used. Carrier gas flow settings however were different for the data reported here. The thermal sweeper has a longer overall length due to the extra ca. 30 cm length of narrow bore tubing used for the modulator/accumulator section. Data reveal that the two methods behave in an analogous manner in respect of delivering GC×GC results, with key peak parameters of peak widths and symmetry measures showing good correlation. Retention time dissimilarity on the first dimension columns in the two systems arises from different flow rates used, however the second column retention is similar, and this is due to the resulting different elution temperatures that peaks elute on the first dimension in each system. Overall, the two approaches to GC×GC appear to produce equivalent results within the scope of the application studied. Each system does have its experimental limitations; the thermal sweeper has what may be called a ‘thick film effect’, where at high temperature it can be difficult to sufficiently trap the migrating bands in the accumulator column, and the pulsing of solutes in the cryogenic system may suffer from a ‘thick wall effect’ if a column with too thick a wall dimension is used at low oven temperature.
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    Is Multidimensional High Performance Liquid Chromatography (HPLC) an Alternative in Protein Analysis to 2D Gel Electrophoresis? (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 259-265 
    Details
    ISSN: 0935-6304
    Keywords: Proteomics ; protein analysis ; multidimensional HPLC ; ion-exchange chromatography ; reversed phase chromatography ; comprehensive HPLC ; two-dimensional HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The interactive modes of High Performance Liquid Chromatography (HPLC) of proteins provide a platform for the construction of a multidimensional HPLC system coupled to mass spectrometry. We present a system composed of both anion and cation exchanger columns, in the first dimension, and n-octadecyl bonded 1.5 μm nonporous silica columns in the second dimension. Both columns are operated under gradient conditions. A system suitability test with standard proteins showed that the total analysis can be performed within about 20 minutes. The fractions taken from the ion exchanger column are directly analyzed within one minute on the reversed phase column at a high flow rate. Two reversed phase columns are applied and operated alternatively: while the first column performs the separation within one minute, the analytes leaving the first dimension are enriched in an on-column focusing mode on top of the second column. The sample clean-up and enrichment is performed on a novel type of restricted access cation exchanger column with internal sulfonic acid groups and external diol groups. The columns exhibit a molecular weight exclusion limit for globular proteins of about 15 kDa. Our next studies will be directed towards the analysis of proteins and peptides from extracts of fibroblasts.
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    Fiber Conditioners for Solid Phase Microextraction: Design, Testing, and Application (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 343-347 
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    ISSN: 0935-6304
    Keywords: SPME ; desorption ; fiber conditioning ; field sampling ; sample preparation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No abstract
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    Silver Ion High-Performance Liquid Chromatographic Separation of Conjugated Linoleic Acid Isomers, and other Fatty Acids, after Conversion to p-Methoxyphenacyl Derivatives (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 348-352 
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    ISSN: 0935-6304
    Keywords: Silver ion high-performance liquid chromatography (Ag-HPLC) ; conjugated linoleic acid (CLA) ; p-methoxyphenacyl derivatives ; single-column Ag-HPLC ; fatty acid analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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    Seed Oil Fatty Acids of Mongolian Compositae: The trans-Fatty Acids of Heteropappus hispidus, Asterothamnus centrali-asiaticus and Artemisia palustris (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 360-366 
    Details
    ISSN: 0935-6304
    Keywords: Artemisia palustris ; Asterothamnus centrali-asiaticus ; capillary gas liquid chromatography ; Compositae (Asteraceae) ; Heteropappus hispidus ; seed oil ; silver ion thin layer chromatography ; trans-fatty acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Seed oils from the Compositae plant family are known to contain a variety of unusual fatty acids. Subsequent to the recent discovery of γ-linolenic acid in Saussurea and Youngia, further Mongolian Compositae species were investigated for their seed oil fatty acid composition. A number of δ3trans-fatty acids (16 : 1δ3t, 18 : 1δ3t and 18 : 3δ3t, 9c, 12c) were found in the seed oils of Heteropappus hispidus and Asterothamnus centrali-asiaticus. The latter fatty acid, but not the trans-monoenes, was also found in one species of Artemisia. These unusual fatty acid isomers were characterized by capillary gas-liquid chromatographic (GLC) separations in combination with other chromatographic techniques (analytical thin layer chromatography, TLC and preparative argentation TLC), and infrared spectrocsopy (IR). Their identity was further confirmed by co-chromatography with other seed oils known to contain these trans-fatty acids. The fact that within the Compositae plant family there are apparently two or three distinct groups of genera containing δ3trans-fatty acids is discussed.
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    2H/1H Ratio Analysis of Flavor Compounds by On-Line Gas Chromatography Pyrolysis Isotope Ratio Mass Spectrometry (HRGC-P-IRMS): Benzaldehyde (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 357-359 
    Details
    ISSN: 0935-6304
    Keywords: 2H/1H ratio analysis ; HRGC-P-IRMS ; stable isotopes ; benzaldehyde ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Isotope ratio monitoring gas chromatography-mass spectrometry of the 2H/1H ratio by pyrolysis isotope ratio mass spectrometry (P-IRMS) was used to analyze benzaldehyde originating from various sources. Based on the δ2HSMOW value of an authentic reference sample determined with an elemental analyzer (EA), the range of reproducibility and linearity was checked. Correct (EA related) and reproducible data were obtained for sample amounts 〉0.6 μg benzaldehyde (on column). In another series of experiments, the influence of sample preparation, i. e. simultaneous distillation-extraction (SDE) was found to be negligible. The following ranges of δ2HSMOW values were determined for benzaldehyde using five types of samples, i. e. (i) synthetic (δ2HSMOW -78 to -85‰, ex benzal chloride; +420 to +668‰, ex toluene) and ‘natural’ (including ‘ex-cassia’) references (δ2HSMOW -83 to -144‰); (ii) bitter almond oils (δ2HSMOW -113 to -148‰); (iii) fruits (δ2HSMOW -111 to -146‰); (iv) kernels (δ2HSMOW -115 to -188‰); and (v) leaves (δ2HSMOW -165 to -189‰).
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    Effects of Injected Volume and Applied Voltage on Column Efficiency in Capillary Electrochromatography with Open Tubular Columns of 10 μm i. d. (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 373-378 
    Details
    ISSN: 0935-6304
    Keywords: Open tubular columns ; capillary electrochromatography ; column efficiency ; injected volume ; applied voltage ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The effect of some instrumental parameters on column efficiency in open tubular capillary electrochromatography (OTCEC) has been evaluated. First, it was investigated whether band broadening due to the sample injection process is within a tolerable range when an open tubular column (OTC) of about 10 μm i. d. is used. As a result of the small injection profile factor (K2 = 1.3), injected volumes must be sufficiently small (less than 10 pL) to avoid a significant efficiency loss (〉5%) when hydrodynamic injection by siphoning is employed. Secondly, the kinetic performance of OTCs in a CEC system was estimated from the variation of the reduced plate height (h) with the reduced linear velocity (ν) which was controlled by the voltage applied. Reasonable agreement was obtained between the theoretical h versus ν curve and the experimental values for a group of polycyclic aromatic hydrocarbons used as test compounds. Values of 0.25 for minimum h at an optimum ν of 16 are estimated, which permit separations with around 400,000 plates per meter to be obtained in less than 5 min. Finally, the possibility of estimating the diffusion coefficients of the solutes in the mobile phase from the plot of the height of a theoretical plate versus electroosmotic flow velocity is shown.
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    Separation of Enantiomers of Drugs by Capillary Electrophoresis with Permethyl-gamma-Cyclodextrin as Chiral Solvating Agent (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 413-429 
    Details
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; enantiomer separation ; chiral drugs ; TM-γ-cyclodextrin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---High-throughput screening is a promising new approach in analytical chemistry. Within the framework of an extended screening program (The German-Chinese Drug Screening Program), the enantioseparation of 86 drugs was investigated by capillary zone electrophoresis in the presence of the chiral solvating agent (CSA) octakis-(2,3,6-tri-O-methyl)-γ-cyclodextrin (TM-γ-CD). By this means, 15 drugs could be separated into enantiomeric pairs. Approximate measures for the degree of interaction (migration retardation factor, Rm) and for the degree of enantiomer recognition (migration separation factors, αm) revealed intriguing patterns that were compared with those found for native γ-cyclodextrin (γ-CD). Although there is a distinct influence of the analyte structure on the electrophoretic data, interpretation remains difficult. Most remarkably, permethylation of γ-CD leads neither to a higher affinity nor to better chiral recognition, in contrast to the findings with α-CD.
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    Retention Prediction System of O-Aryl,O-(1-methylthioethylidene-amino)phosphates on RP-HPLC (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 445-448 
    Details
    ISSN: 0935-6304
    Keywords: O-Aryl,O-(1-methylthioethylideneamino)phosphates ; retention prediction ; quantitative structure-retention relationship (QSRR) ; reversed-phase HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Using factor analysis and stepwise linear regression methods, two parameters - CMR and ECCR - were selected from eight solute-related structure parameters as the most retention-influencing parameters. The relationships between the retention data (k ´) and the two structure parameters were established for 13 O-aryl,O-(1-methylthioethylideneamino)phosphate compounds under a wide range of experimental conditions. The retention data (k ´) of another seven compounds with similar structures were predicted using these QSRR equations. Good agreement was obtained between the experimental k ´ values and predicted ones.
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    Temperature-Programmed Packed Capillary Liquid Chromatography Coupled to Fourier-Transform Infrared Spectroscopy (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 525-530 
    Details
    ISSN: 0935-6304
    Keywords: Packed capillary liquid chromatography ; temperature programming ; Fourier-transform infrared spectroscopy ; polymer additives ; pneumatic nebulization ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Temperature-programmed packed capillary liquid chromatography has been coupled off-line to Fourier-transform infrared spectroscopy, utilizing a commercially available interface with a pneumatic nebulizer rebuilt to handle low flow rates at elevated temperatures. The modified interface showed excellent performance with regard to non-aqueous reversed phase separations of polymer additives, resulting in constructed Gram-Schmidt chromatograms comparable to chromatograms obtained using UV detection. The spray of the in-house constructed nebulizer was not influenced by temperature changes of the column effluent, and hence temperature-programmed gradient separations could be used successfully. The relative standard deviation of peak height was 4.4% (n = 5) and the mass limit of detection was determined to be about 40 ng, using a polymer antioxidant as model compound. The present instrumental coupling has been used for characterization of the antioxidant Irgafos P-EPQ.
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    Separation of Enantiomers by On-Line Capillary Isotachophoresis-Capillary Zone Electrophoresis (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 531-538 
    Details
    ISSN: 0935-6304
    Keywords: Capillary isotachophoresis ; capillary electrophoresis ; column-coupling electrophoresis ; enantiomers ; chiral ; amino acids ; tryptophan ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The ability of capillary zone electrophoresis (CZE) coupled on-line with capillary isotachophoresis (ITP) sample pretreatment in the column-coupling capillary electrophoresis equipment to separate trace enantiomers present in samples of complex ionic matrices and enantiomers present in their mixtures at significantly differing concentrations has been studied. Enantiomers of 2,4-dinitrophenyl labeled norleucine (DNP-Nleu) and tryptophan enantiomers were employed as model analytes in this work while urine and mixtures of tryptophan enantiomers of differing concentrations served as model samples. Experiments performed with urine samples spiked with the DNP-Nleu racemate at sub-μmol/L concentrations demonstrated excellent sample pretreatment capabilities of ITP (concentration of the analytes, in-column and post-column sample clean up) when coupled on-line with chiral CZE separations. In the CZE separations of enantiomers present in the samples at trace concentrations the sample pretreatment could be performed in both achiral and chiral ITP electrolyte systems. The use of a chiral electrolyte system was found to be essential in the ITP pretreatment of the samples containing the enantiomers at very differing concentrations. For example, a 2×10-7 mol/L concentration of L-tryptophan could be detected in the CZE separation stage of the ITP-CZE combination in samples containing about a 104 excess of D-tryptophan only when the ITP pretreatment was carried out in the electrolyte system providing the resolution of enantiomers (α-cyclodextrin served for this purpose in the present work). A post-column ITP sample clean up was found effective in enhancing the destacking rate of the trace enantiomer in the CZE stage when the migration configuration of the enantiomers was less favorable (the trace constituent migrating behind the major enantiomer).
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    Characterization and Comparison of Tea Tree and Lavender Oils by Using Comprehensive Gas Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 554-560 
    Details
    ISSN: 0935-6304
    Keywords: Comprehensive gas chromatography ; multidimensional gas chromatography ; essential oils ; coupled column analysis ; high resolution analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The essential oils from French lavender (Lavandula angustifolia) and tea tree (Melaleuca alternifolia) were separated by the two-dimensional GC technique of comprehensive gas chromatography. A coupled column combination of non-polar (5% phenyl equivalent) and polyethylene glycol phase columns was used to provide the desired resolution performance. By using a range of known standards, some of the peaks in lavender oil can be assigned. Some of these also occur in tea tree oil; however, from our knowledge of the major constituents in this oil and their relative retention behaviour, most of the major peaks may be tentatively assigned within the 2-dimensional separation space. There appear to be elution patterns within the 2-D space which should be useful in correlating retention with chemical and structural properties of the components, although this will require further evaluation. A range of coeluting peaks, which may not be so readily separated by using a single column capillary GC analysis, are resolved in the experiment described.
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    Gas Chromatographic Enantiomer Separation of Atropisomeric PCBs Using Modified Cyclodextrins as Chiral Phases (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 619-627 
    Details
    ISSN: 0935-6304
    Keywords: Enantiomer separation ; mixed chiral selectors ; modified cyclodextrins ; gas chromatography ; PCB ; o,p´-DDD ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Columns containing different types of cyclodextrin derivatives have been evaluated for chiral gas chromatographic separation of atropisomeric PCBs, o,p´-DDT and o,p´-DDD. Separation was attempted on columns containing mixed chiral selectors, and the performance of two closely related selectors was also examined. The cyclodextrins were: permethylated-β-CD (PM-β-CD), heptakis(2,3-di-O-methyl-6-O-tert-butyldimethylsilyl)-β-CD (2,3-M-6-TBDMS-β-CD), heptakis(2,3-di-O-methyl-6-O-tert-hexyldimethylsilyl)-β-CD (2,3-M-6-THDMS-β-CD), and heptakis(2,3-di-O-ethyl-6-O-tert-hexyldimethylsilyl)-β-cyclodextrin (2,3-E-6-THDMS-β-CD). The cyclodextrins were dissolved in OV-1701 or in a dimethylsiloxane/silarylene copolymer containing 5% phenyl in the backbone. The application of mixed chiral selectors led to improved separations, however; at most eleven PCB congeners were separated on a single column. Chiral resolution of o,p´-DDD was achieved. The use of a dimethylsiloxane/silarylene copolymer as a matrix for the cyclodextrins is a promising approach. With such a matrix, blocking of the CD cavities by silicone substituent groups can be avoided, and a reasonable CD solubility can be provided. The selectivity of heptakis(2,3-di-O-ethyl-6-O-tert-hexyldimethylsilyl)-β-CD and heptakis(2,3-di-O-methyl-6-O-tert-hexyldimethylsilyl)-β-CD was quite different, the former selector could separate four congeners, while the latter separated ten congeners.
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    Determination of Free D-Amino Acids in Mammalia by Chiral Gas Chromatography-Mass Spectrometry (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 576-582 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography-mass spectrometry ; amino acid enantiomers ; D-amino acids ; physiological fluids ; mammals ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Quantities of D-amino acids were determined in body fluids (urine, blood plasma and blood serum, milk) of mammals (hamster, horse, bovine, sheep, pig, and dog). Amino acids were isolated using a cation exchanger and converted into their N(O)-pentafluoropropionyl (or trifluoroacetyl) amino acid 2-propyl esters. Enantiomers were separated and quantified on a Chirasil-L-Val capillary column with mass spectrometric detection using selected ion monitoring. D-Enantiomers of most protein L-amino acids were detected. Largest absolute and relative amounts in most cases were determined for D-Ser and D-Ala in urine. Stereoisomers of 2,6-diaminopimelic acid were also measured in bovine, ovine, and porcine urine. Since D-amino acids were detected in all representative classes of the major orders of Mammalia, namely Artiodactyla, Perissodactyla, Rodentia, and Carnivora, and taking reports in the literature into account, it is postulated that D-amino acids occur in all mammals.
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    Optimization of a GC-MS/MS Method for the Analysis of PCDDs and PCDFs in Human and Fish Tissue (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 595-599 
    Details
    ISSN: 0935-6304
    Keywords: GC-MS/MS ; PCDDs ; PCDFs ; human tissue ; fish tissue ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---This paper outlines the possibilities of selectivity and sensitivity enhancement in measuring PCDD/F congeners using an ion trap GC-MS/MS. The pressure of the collision gas and the collision energy were optimized. The modified GC-MS/MS method was applied to the determination of PCDDs and PCDFs in human and fish tissues. Limits of quantification were about 1 pg/g of fat for all seventeen 2378 PCDD/Fs tested (starting amount of fat, 2 g).
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    Use of Coupled HPLC/1H NMR and HPLC/ESI-MS for the Detection and Identification of (2E,4Z)-Decadienoic Acid from a New Agromyces Species (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 609-612 
    Details
    ISSN: 0935-6304
    Keywords: On-line coupling HPLC/NMR ; HPLC/ESI-MS ; (2E,4Z)-decadienoic acid ; Agromyces spec ; isolation ; structure elucidation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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    A Few Milestones on the Journey of Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 497-501 
    Details
    ISSN: 0935-6304
    Keywords: Historical remarks ; modern separation methods ; gas chromatography ; selective sorbents ; selectors ; discovery process ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The research conducted and the discoveries during the development of chromatography are briefly surveyed, with emphasis being placed on gas chromatography. Some actors are presented who played major roles en route from Tswett's original discovery to modern separation methods. The article is based mainly on personal memories and encounters. A few examples of the participation of our country in the development of chromatography are mentioned as well as international contacts. Some remarks are made on the use of selective sorbents or selectors in modern analytical separations. The paper closes with a few comments on the “philosophy” of the discovery process.
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    Group-Type Identification of Oil Samples Using Comprehensive Two- Dimensional Gas Chromatography Coupled to a Time-of-Flight Mass Spectrometer (GC×GC-TOF) (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 507-510 
    Details
    ISSN: 0935-6304
    Keywords: Comprehensive two-dimensional GC ; time-of-flight ; oil analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---In this work a comprehensive two-dimensional system (GC×GC) was coupled to a time-of-flight mass spectrometer (TOF/MS) for the analysis of oil samples. Group-types like the alkanes and saturated cyclic compounds (naphthenes), which are present in oil, are shown separately by selecting their unique masses. On selecting appropriate ion fragments, this method also permits the determination of sulfur- and oxygen-containing species in oil. Former results obtained by FID detection could be confirmed. After proper selection of unique ions in GC×GC-TOF both selectivity and sensitivity increase.
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    Open Tubular Supercritical Fluid Chromatography (ot-SFC) Applied to the Separation of Coal-Derived Products Obtained by Supercritical Fluid Extraction (SFE) (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 515-518 
    Details
    ISSN: 0935-6304
    Keywords: Capillary supercritical fluid chromatography (c-SFC) ; coal analysis ; SFE ; instrumentation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---This work describes the construction and evaluation of a simple and versatile capillary supercritical fluid chromatographic (SFC) system and its application to the analysis of liquid fuels obtained by SFE. The modular supercritical fluid chromatography (SFC) system uses a syringe pump, a fused silica capillary column (100 μm i.d., coated with a 0.2-μm thick film of 5% phenylpolymethylsiloxane), a FID detector, and a high pressure injection valve with a 60-nL internal loop. Coal-derived samples were obtained by supercritical fluid extraction (SFE) of a Brazilian high-inertinite coal from Amando Simões mine, located in Paraná state (Brazil) using toluene as solvent and operating in the static mode. SFE was followed by preparative liquid chromatography fractionation into eight discrete fractions (PLC-8 method). Two of those fractions (F-2 and F-8) were used to evaluate the proposed set-up. The system described proved to be simple, easy-to-use, and versatile when used in the analysis of a range of samples from low molecular weight-low volatility (F-2) to higher molecular weight-high polarity asphaltols (F-8).
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    An Introduction to Monolithic Disks as Stationary Phases for High Performance Biochromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 27-38 
    Details
    ISSN: 0935-6304
    Keywords: Monolith ; continuous bed column ; convective interaction media ; membrane chromatography ; membrane adsorber ; HPMDC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Monolithic stationary phases have revolutionized protein chromatography because they combine speed, capacity, and resolution in a unique manner. Since such stationary phases contain no particles but only flow-through pores, the usual mass transfer restrictions to the chromatography of large molecules are not observed and extremely fast separations become possible. Recently the area of application of monolith chromatography has been extended to the separation and analysis of small molecules and plasmid DNA. This review summarizes the state of art in high performance monolith and especially high performance monolithic disk chromatography (HPMDC). The current understanding of the theory of protein HPMDC is summarized, while an introduction to the evolving field of small molecule HPMDC is attempted. The basic differences between the monolithic disks and columns packed with conventional stationary phases (including perfusion and micropellicular particles) but also monolithic columns (porous rods) are outlined. Finally, the potential of HPMDC to analytical and preparative biochromatography is demonstrated by a discussion of recent applications of chromatographic disks for protein isolation and bioprocess analysis.
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    Miniaturized Molecularly Imprinted Continuous Polymer Rods (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 44-46 
    Details
    ISSN: 0935-6304
    Keywords: In situ molecular imprinting ; continuous polymer rod ; miniaturized column ; chiral recognition ; diastereoselectivity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Molecularly imprinted continuous polymer rods are prepared inside PEEK tubes of 1 mm i. d. by an in situ preparation technique; and chiral separations on such media have been demonstrated. The miniaturized column filled with (-)-cinchonidine-imprinted or (+)-cinchonine-imprinted polymer rods based on a copolymer of 2-(trifluoromethyl)acrylic acid and ethylene glycol dimethacrylate permitted diastereoseparation of (-)-cinchonidine and (+)-cinchonine; the template molecule is retained to a greater extent than the corresponding antipode. Increasing the amount of cyclohexanol in the polymerization mixture decreased the backpressure of the resultant rod and the addition of latex beads suspended in water to the prepolymerization mixture affected the selectivity and affinity of the imprinted polymer rods. The column length is adjusted easily by cutting, thus allowing easy control of retention behavior and analysis time.
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    Enantiomeric Separations of Acidic and Neutral Compounds by Capillary Electrochromatography with β-Cyclodextrin-Bonded Positively Charged Polyacrylamide Gels (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 59-66 
    Details
    ISSN: 0935-6304
    Keywords: Enantiomeric separation ; capillary electrochromatography ; positively charged polyacrylamide gel ; allyl carbamoylated β-cyclodextrin derivatives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The novel enantiomeric separation of acidic and neutral compounds by capillary electrochromatography with β-cyclodextrin-bonded positively charged polyacrylamide gels was examined. The columns used are capillaries filled with a positively charged polyacrylamide gel, a so-called monolithic stationary phase, to which allyl carbamoylated β-CD derivatives covalently bind. The capillary wall was activated first by bifunctional reagent to make the resulting gel bind covalently inside the fused-silica tubing. Enantiomeric separations of sixteen acidic and two neutral compounds were achieved using the above-mentioned columns and 200 mmol dm-3 Tris-300 mmol dm-3 boric acid buffer (pH 8.1) as a mobile phase. High efficiencies of up to 150 000 plates m-1 were obtained for dansyl-DL-amino acids. The within-run and between-run reproducibilities of retention time and separation factor were examined for three dansyl-DL-amino acids and warfarin. The relative standard deviations of the within-run and between-run reproducibilities of retention time were less than 1.2 and 1.3% over the six injections, respectively. Those of the separation factor were less than 0.3 and 0.2%, respectively. The gel-filled capillaries were stable for at least four months with intermittent use.
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    Comparison of Different Di-tert-butyldimethyl-Silylated Cyclodextrins as Chiral Stationary Phases in Capillary Gas Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 569-575 
    Details
    ISSN: 0935-6304
    Keywords: Enantioselective gas chromatography ; cyclodextrins ; heptakis(2,6-di-O-tert-butyldimethylsilyl)-β-cyclodextrin ; heptakis(2,6-di-O-tert-butyldimethylsilyl-3-O-methyl)-β-cyclodextrin ; heptakis(3,6-di-O-tert-butyldimethylsilyl-2-O-methyl)-β-cyclodextrin ; octakis(2,6-di-O-tert-butyldimethylsilyl-3-O-methyl)-γ-cyclodextrin ; thermodynamic parameters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Separation factors and thermodynamic data for the separation of various chiral analytes on different di-O-tert-butyldimethyl-silylated cyclodextrin derivatives are collected and described. Modifying the substitution pattern of the tert-butyldimethylsilyl group in position 2 and 3 or changing from β- to γ-cyclodextrin significantly affects the separation properties of the cyclodextrin derivatives.
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    Synthesis and Silica-Based Immobilization of Monofunctionalized Heptakis(2,6-di-O-methyl-3-O-pentyl)-β-cyclodextrin for Enantioselective Capillary-HPLC (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 583-589 
    Details
    ISSN: 0935-6304
    Keywords: Monofunctionalized cyclodextrins ; enantioselective capillary-HPLC ; immobilized chiral stationary phases ; separation of chiral drugs ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Heptakis(2,6-di-O-methyl-3-O-pentyl)-β-cyclodextrin was monofunctionalized by the regioselective introduction of exactly one ω-epoxyoctyl group at the primary site of the cyclodextrin. The site-specifically substituted cyclodextrin was immobilized to commercially available aminopropyl silica by nucleophilic opening of the epoxy function of the spacer substituent resulting in a lipophilic chiral stationary phase with broad applicability for enantiomer separations in capillary-HPLC under reversed-phase conditions.
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    Determination of Lucidin in Rubia tinctorum Aglycones by an HPLC Method with Isocratic Elution (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 600-602 
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    ISSN: 0935-6304
    Keywords: HPLC separation ; lucidin ; Rubia tinctorum ; anthraquinones ; isocratic elution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---An HPLC method has been developed for the separation of anthraquinones with particular attention to the determination of lucidin in commercially available sources of Rubia tinctorum aglycones. Variations of chromatographic conditions have been studied in order to provide suitable resolution of anthraquinones under isocratic conditions on an end-capped RP C18-column.
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    The Determination of Benzoic Acid in Lemon Flavored Beverages by Stir Bar Sorptive Extraction-CGC-MS (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 644-646 
    Details
    ISSN: 0935-6304
    Keywords: Stir Bar Sorptive Extraction (SBSE) ; thermal desorption (TD) ; capillary GC-MS ; benzoic acid ; beverages ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Stir Bar Sorptive Extraction (SBSE), a recently introduced solventless extraction technique, was applied for the enrichment of benzoic acid in lemon flavored beverages. The stir bar is covered with 50 mg polydimethylsiloxane (PDMS) and the extraction mechanism is similar to that of solid phase micro extraction (SPME) but the enrichment factor is ca. 100 times higher. SBSE is followed by thermal desorption (TD)-capillary gas chromatography (CGC)-mass spectroscopy (MS). Calibration graphs for benzoic acid were linear from 1 to 1000 ppm for water and diluted soft drinks and the repeatability (n = 6) was less than 5% RSD.
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    Separation of Ceramides by Sub-Ambient Temperature-Assisted Large Volume Injection in Temperature-Programmed Packed Capillary Liquid Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 653-655 
    Details
    ISSN: 0935-6304
    Keywords: Packed capillary LC ; large volume injection ; temperature programming ; ceramides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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    A Simple Way to Speed up Separations by GC-MS Using Short 0.53 mm Columns and Vacuum Outlet Conditions (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 677-680 
    Details
    ISSN: 0935-6304
    Keywords: Capillary ; fast separations ; mass spectrometry ; vacuum ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---There is a constant drive to speed up GC separations. Shorter analysis times provide more analyses per day, which reduces cost. One approach is to reduce column length and column diameter and columns of 0.15 mm i.d. have indeed grown in popularity. However, the majority of applications are still done with 0.25 mm and 0.32 mm columns.
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    Optimization of Focused Microwave-Assisted Extraction of DDT and Derivatives from Soil Samples (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 681-687 
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    ISSN: 0935-6304
    Keywords: Focused microwave assisted extraction ; close microwave-assisted extraction ; DDT ; soil samples ; experimental design ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Optimization of focused microwave (FMW)-assisted extraction of 4,4′-DDE, 4,4′-DDD, and 4,4′-DDT from soil samples was carried out using central composite designs. All the extracts were analyzed with GC/MS and some of them also with GC/AED using columns of different polarities for each of the techniques. The extraction of the analytes was carried out in two ways: with acetic acid as microwave radiation absorbent solvent and n-decane to concentrate the analytes and with reagent water and iso-octane as solvents. In the first case, the influence of the extraction temperature, the extraction time, and the addition of sodium chloride were studied and the optimum conditions for the extraction of 1 g of soil with 5 mL of acetic acid and 2 mL of n-decane were 1.30 mol L-1 sodium chloride at 98°C for 9.3 min. In the second case, the temperature was kept constant (94°C) and the influence of the concentration of sodium chloride and the extraction time were studied. The optimum conditions were 5 mL of a 2.0 mol L-1 sodium chloride together with 2 mL of iso-octane for 15 min. The recoveries obtained by water-FMW extraction were significantly lower than those obtained by the acetic acid-FMW procedure. These last recoveries were in good agreement with those obtained by closed microwave assisted-extraction with acetone-n-hexane as solvent.
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    RP-HPLC Method for the Separation of Some Phenol Derivatives Using Gradient Elution and UV Detection (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 699-701 
    Details
    ISSN: 0935-6304
    Keywords: Phenol derivatives ; RP-HPLC separation ; short RP column ; gradient elution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---No abstract
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    Two-Dimensional Gas Chromatography. Concepts, Instrumentation, and Applications - Part 2: Comprehensive Two-Dimensional Gas Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 167-181 
    Details
    ISSN: 0935-6304
    Keywords: Comprehensive two-dimensional GC ; GC×GC ; orthogonal chromatography ; GC/MS ; group type separations ; PCBs ; petroleum ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The writer of this review published in 1978 a three-part article on two-dimensional gas chromatography in the first three issues of this journal [1]. The review was written at a time when capillary column GC was still in its infancy. Commercial columns were (essentially) unavailable and sample introduction into capillary columns was done exclusively in the split mode. Two-dimensional separations were explored in only a few laboratories. The limitations of capillary column technology made this exercise rather difficult. The introduction of fused silica capillary columns in the early eighties drastically changed the landscape in which gas chromatography was practiced. It took the chromatographic community just a few years to convert from packed columns to capillary columns. Instrumentation and accessories specifically designed for capillary column use came onto the market. This writer had great hopes that the revolution in capillary column GC would be mirrored in the development of instrumentation for Two-Dimensional Gas Chromatography. This never materialized. On the contrary, tentative steps taken by a few manufacturers and suppliers of chromatographic equipment fizzled out. It was perhaps the introduction of relatively inexpensive and user friendly GC/MS instrumentation, in combination with nearly indestructible fused silica capillary columns that took away the incentive to develop commercially viable Two-Dimensional Gas Chromatography. Much of the thinking went like this: why insist on good chromatography if mass spectrometry can do the job without the need of complete separation. Some progress in the further development of conventional Two-Dimensional Gas Chromatography has certainly been made over the last 20 years but there has not been a great deal of excitement. Applications have also been relatively sparse and they are limited to just a few areas. Science does not remain static and chromatography is no exception. Progress in gas chromatography is driven by new technology and ideas. Substantial improvements in two-dimensional GC were not forthcoming until Phillips and his research group introduced and implemented an entirely new form of Two-Dimensional Gas Chromatography, called comprehensive GC×GC. This breakthrough occurred only in 1991 [2]. It does take some time before scientists change attitudes and habits. There is always a time lag between the introduction of new technology and its general acceptance. The public's attitude toward comprehensive Two-Dimensional Gas Chromatography is probably no exception. The number of scientists who are actively pursuing this new branch of gas chromatography is still very small. It is often a single individual who carries the torch. J.B. Phillips' name is synonymous with comprehensive Two-Dimensional Gas Chromatography. He is not only its inventor and proponent but his fertile mind has initiated research in other related areas. Sadly, he passed aware shortly before this review was written. This contribution is dedicated to his memory.
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    Jet-Cooled Thermal Modulator for Comprehensive Multidimensional Gas Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 202-204 
    Details
    ISSN: 0935-6304
    Keywords: GC×GC ; comprehensive two-dimensional GC ; thermal modulation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A jet of cool gas is used to locally cool a section of modulator tube in the presence of the stirred oven bath of a GC×GC instrument. Local cooling decouples the temperature of the modulator tube from that of the first dimension column, which was 100 meters long. Overall resolution of the GC×GC experiment was improved as a result. Another consequence of the jet-cooled thermal modulation structure is the elimination of moving parts in the GC oven. By pulsing cold and hot jets of gas onto a modulator tube with solenoid valves, two stage thermal modulation can be obtained without the complexity of moving parts in the vicinity of the capillary columns.
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    GC3: Comprehensive Three-Dimensional Gas Chromatography (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 205-207 
    Details
    ISSN: 0935-6304
    Keywords: GC×GC ; thermal modulation ; comprehensive three-dimensional GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Comprehensive three-dimensional gas chromatography (GC3) is demonstrated using modified GC×GC apparatus. A new thermal modulation scheme employing a single moving heater to operate two thermal modulators is introduced. Considerations of the bandwidth/resolution tradeoff of GC3 show that high-speed tertiary columns would make GC3 practical, with modest loss of underlying GC×GC peak capacity.
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    Application of Comprehensive Two-Dimensional Gas Chromatography (GC×GC) to the Qualitative Analysis of Essential Oils (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 208-214 
    Details
    ISSN: 0935-6304
    Keywords: Spearmint ; peppermint ; GC×GC ; essential oils ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---This paper investigates the separation of moderately complex samples by comprehensive two-dimensional gas chromatography (GC×GC). The analysis of peppermint (Mentha piperita) and spearmint (Mentha spicata) essential oil components, including acetates, alcohols, furans, ketones, sesquiterpenes, and terpenes, was achieved by one-dimensional gas chromatography with quadrupole mass spectrometry detection (GC/MSD) and GC×GC with flame ionization detection. Peppermint essential oil was found to contain 89 identifiable peaks by GC×GC compared to 30 peaks in the GC/MSD chromatogram. Likewise, 68 peaks were found in the GC×GC chromatogram of spearmint (compared to 28 in GC/MSD). Plots of the first dimension versus second dimension retention times provided a fingerprint of the two essential oils, which revealed 52 similar compounds between the two essential oils as opposed to 18 matches by 1D GC.
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    Pressure-Tunable Dual-Column Ensembles for High-Speed GC and GC/MS (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 225-234 
    Details
    ISSN: 0935-6304
    Keywords: Tunable column ensembles ; high speed GC ; comprehensive two-dimensional GC ; time of flight ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---A series-coupled ensemble of two capillary GC columns of different selectivity with an adjustable pressure at the column junction point is used to obtain tunable selectivity for high-speed GC and GC/TOFMS. An electronic pressure controller with a 0.1-psi step size is used to obtain numerous computer-selected unique selectivities. System configurations for conventional, atmospheric-pressure outlet operation with flame ionization detection and for vacuum-outlet operation with photoionization detection are described for GC-only experiments. Polydimethylsiloxane is used as the non-polar column and polyethylene glycol (atmospheric outlet) or triflouropropylpolysiloxane (vacuum outlet) is used as the polar column. For GC/TOFMS experiments, 5% phenyl polydimethylsiloxane was used as the non-polar column, and polyethylene glycol was used as the polar column. The time-of-flight mass spectrometer can acquire up to 500 complete mass spectra per second. Since spectral continuity is achieved across the entire chromatographic peak profile, severely overlapping peaks can be spectrally deconvoluted for high-speed characterization of completely unknown mixtures. For mixture components with significantly different fragmentation patterns, spectral deconvolution can be achieved for chromatographic peak separations of as little as 6.0 ms. This can result is very large peak capacity for time compressed (not completely resolved) chromatograms. The use of columns with tunable selectivity allows for precise peak-position control, which can result in more efficient utilization of available peak capacity and thus further time compression of chromatograms. The limits of tunability and deconvolution are tested for near co-elutions of different classes of hydrocarbon compounds as well as for more multi-functional mixtures.
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    Identification of 2-hydroxy fatty acids in complex mixtures of fatty acid methyl esters by mass chromatographyAbbreviations: Hydroxy fatty acids are identified by h preceding chain length. (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 10-14 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Repetitive mass spectrometric scanning of gas-liquid chromatographic effuents at short (6 to 15 s) intervals, with a digital computer for data acquisition, reduction and display, allows plots (mass chromatograms) to be made of the intensities of specific ion fragments. Plotting of m/e values characteristic for certain classes of compounds and/or individual components reveals the location of constituents in the gas chromatogram. This technique was applied to the identification of trimethylsilyl derivatives of unsubstituted and 2-hydroxy fatty acid methyl esters in mixtures obtained from acid catalyzed methanolysis of cat brain galactocerebrosides. The plot of total ionization intensity vs scan number generated the gas-liquid chromatogram. Mass chromatograms of m/e 73 and [M - 59]+ gave the locations in the gas-liquid chromatogram of the hydroxy fatty acid derivatives, and mass chromatograms of m/e 74 and [M]+ located the unsubstituted fatty acid derivatives. Integrated ion intensities were used to determine the composition of the mixture of fatty acids.
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    URL: http://dx.doi.org/10.1002/bms.1200010105
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    The structural elucidation of polyene macrolide antibiotics by mass spectrometry. Nystatin, amphotericin B and pimaricin (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 20-28 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Complete mass spectra of the pertimethylsilylated derivatives of three high molecular weight polyene macrolide antibiotics are reported for the first time. The fragmentation pathways which are proposed have been corroborated by the stable isotope derivatives d9-TMS and d3-acetyl. Accurate mass measurements and metastable transitions confirm the proposed fragmentation mechanisms in the low mass range. Nystatin - the macrolide of highest molecular weight in this study - expels several TMSOH molecules and a TMS radical. Amphotericin B underwent extensive rearrangements preliminary to eliminating a series of TMSOH molecules. An apparent equilibrium between the keto and ketal forms of amphotericin B facilitated the rearrangements. Pimaricin fragmented in a manner parallel to that of the other two macrolides. The sugar portion of the molecules dominated the fragmentation in the low mass region in the spectra of all compounds. The transfer of a TMS group from the sugar amine to the glycosidic oxygen was observed when the amino sugar was eliminated from the intact molecule. The resulting sugar ion then expelled ammonia.
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    Sex-linked specificity of the hepatic metabolism of steroids in rats. Mass fragmentography as a method for the assay of hydrogenated metabolites of corticosterone in the liver (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 29-39 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for the separation, identification and quantitation of endogenous hydrogenated metabolities of corticosterone in rat liver Corticosterone, 5α- and 5β-dihydrocorticosterone, 3α,11β,21-trihydroxy-5α-pregnane-3,20-dione, 3β,11β,21-trihydroxy-5α-pregnane-3,20-dione, 3α,11β,21-trihydroxy-5β-pregnane-3,20-dione, 3β,11β,21-trihydroxy-5α-pregnane-3,20-dione, 5α-pregnane-3α,11β,20α,21-tetrol, 5α-pregnane-3α,11β,20β,21-tetrol and 5α-pregnane-3β,11β,20β,21-tetrol are specifically quantitated in one analysis by mass fragmentography all as their O-methyloxime pertrimethylsilyl derivatives. A pronounced difference in the amounts of these nine metabolites between male and female adult rats was found, while in newborn rats only the two tetrahydro-compounds bearing a 5α-hydrogen were detected in both sexes. On the other hand 3α,11β,1 5α,21-tetrahydroxy-5α-pregnan-20-one was detected only in the adult female as its second prominent metabolite of corticosterone. Corticosterone metabolites being biochemical markers of the sex-linked differentiation of the hepatocytes, their mass fragmentographic assay is proposed as a tool for the quantitative analysis of this type of gene expression.
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    Determination of the structure of partially methylated sugars as O-trimethylsilyl ethers by gas chromatography-mass spectrometry (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 62-65 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The separation and structural determination of ten partially methylated methyl glucosides by gas chromatography and gas chromatography-mass spectrometry are described. These glucosides were four possible structures for methyl tri-O-methylglucosides and six for methyl di-O-methylglucosides. The positions of free hydroxyl groups in four isomers of methyl tri-O-methylglucosides could be fairly distinguished from each other by their mass spectra. Mass spectra of methyl di-O-methylglucosides were similar to each other, though their spectra were different from those of fully methylated or methyl tri-O-methylglucosides. After introduction of a trimethylsilyl group to the free hydroxyl group, mass spectra of methyl di-O-methylglucosides showed a characteristic pattern for the position of the trimethylsilylated hydroxyl group, and O-trimethylsilyl ethers of methyl tri-O-methylglucosides also showed distinguishable mass spectra. The structures of fragment ions of partially methylated methyl glucosides were confirmed by high resolution mass spectrometry.
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    Liquid chromatography-mass spectrometry. II - continuous monitoring (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 80-82 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Monitoring of solutes eluted from a liquid chromatograph is possible by continuous introduction of the effluent solution into the ion source of a chemical ionization mass spectrometer. Detection sensitivities in the nanogram range are possible for a wide variety of solutes and solvents. Auxiliary techniques which have proved valuable for g.c.-m.s. also appear to be applicable to l.c.m.s.
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    Study on drug metabolites by mass spectrometry. IVFor Part III, see Ref. 1. - metabolites of 2-(diethylamino) ethyltetrahydro-α-(1-naphthylmethyl)-2-furanpropionate oxalate in rats (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 66-72 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The determination of drug metabolites is very important in the biochemical field. However, the procedure for doing this has been very complicated in many cases. The major reason is because of the need for fairly large amounts of the samples. We have been studying procedures for the determination and identification by use of mass spectrometry, which usually gives a lot of information rapidly from very small amounts of the samples (below μg). In this paper, the metabolites excreted in urine and bile following oral administration of 2-(diethyamino)ethyl tetrahydro-α-(1-naphthylmethyl)-2-furanpropionate oxalate (1) in rats, were investigated by means of mass spectrometry and other techniques. The drug was not excreted unchanged in urine. Of the eight metabolites suspected to be present in urine and bile, the structures of three metabolites were elucidated to be tetrahydro-α-(1-naphthylmethyl)-2-furanpropionic acid (3) and α-(1-naphthylmethyl)-2-perhydro-5-oxofuranpropionic acid (4) in urine, and diethylaminoethanol (2) in bile. These metabolites might also be present as their structural isomers or conjugates.
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    Masthead (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974) 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200010201
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    Interpretation of mass spectra, 2nd Edition, by F. W. McLafferty. W. A. Benjamin Inc., Reading, Massachusetts, 1973. $15.00 (cloth) $7.50 (paper) (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. xiv 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    URL: http://dx.doi.org/10.1002/bms.1200010118
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    Qualitative and quantitative mass spectrometry of some noncatecholic biogenic amines and related compounds as their dansyl derivatives (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 83-95 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The use of the integrated ion current technique for the analysis of biogenic amines and phenols as their 1-dimethylaminonaphthalene-5-sulphonyl (dansyl) derivatives is described, particularly as regards to the linearity and sensitivity of detection. The mono derivatized amines gave a linear response over the range 10-9 to 10-14 mol, with a few being detected in quantities as small as 5 × 10-15 mol. The bisdansyl derivatives have a lower sensitivity and the response is linear over a more restricted range, terminating at 10-13 mol. Deuterated analogues of some of the amines were prepared and the feasibility of their use as internal standards was investigated. In this way, the problems associated with quantitative biochemical analyses caused by losses during extractions, chromatographic separations and thermal decomposition in the mass spectrometer lon source are overcome. The differentiation of isomers of biogenic amines as their dansyl derivatives has been accomplished by fractional sublimation and by examination of differences in their fragmentation patterns.
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    Amino acid mixture analysis by mass spectrometry in the form of their dimethylaminomethylene methyl esters (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 115-119 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The amino acids, arginine, citrulline, cysteine, cystine, histidine, hydroxyproline, methionine, ornithine, proline, serine, threonine, tryptophan and tyrosine, have been analysed in the form of their N-(N′, N′-dimethylaminomethylene) methyl esters. formed in a single step by reaction of the free amino acid or its hydrochloride with N,N-dimethylformamide dimethylacetal in acetonitrile/methanol (2:1). A reaction time of 15 minutes at 100 °C ensures complete derivatization, the derivatives being volatile at source temperatures below 150 °C, and giving electron impact spectra characterized by abundant (or moderately abundant) peaks at or near the mass of the molecular ion.The analysis of amino acid mixtures by mass fragmentography on characteristic high mass peaks of their N-(N′,N′-dimethylaminoethylene) methyl ester derivatives, introduced on a direct insertion probe and volatilized during temperature programming of the source, is qescribed. The method is applied to the analysis of a mixture containing arginine, citrulline, cystine, histidine and tryptophan, traditionally difficult to analyse by other methods.
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    Observations on the mechanism of hydroxylation of cyclophosphamide by rat liver microsomes: The metabolism of cyclophosphamide-4-d2 (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 130-136 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The metabolism of cyclophosphamide-4-d2 (2-[bis(2-chloroethyl)amino]-tetrahydro-4,4-dideuterio-2H-1,3,2-oxazaphosphorine 2-oxide), was studied. The first detectable metabolite was a hydroxy derivative which was trapped with ethanol. Mass spectrometry of the resulting two ethoxy derivatives and of the deuterated acrolein 2,4-dinitrophenylhydrazones formed therefrom via reaction with acidic 2,4-dinitrophenylhydrazine, afforded evidence that the ethoxy substituents were at C-4, which was therefore the position of the original hydroxy substituent. The mass spectrum of the deuterated acrolein 2,4-dinitrophenylhydrazone obtained from the total reactive metabolites was used to estimate the ratio of 4- to 6-hydroxylation. The rate of metabolism and the antitumour activity of cyclophosphamide and its 4-d2 analogue were compared.
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    Mass spectral studies of airborne particulates and possible pollution sourcesWork supported in part by EPA under Agreement No. EPA-IAG-0217(D) entitled ‘Correlation of Hazardous Compound Composition of Coal, Ash, Fly-Ash, and Other Emissions from Combustion’. (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 137-141 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The organic material in airborne particulate matter is being studied by high resolution mass spectrometry to determine if hydrocarbons typical of major sources of pollution can be detected. Carbon number distributions and hydrogen-to-carbon ratios of components found in airborne particulate samples and the corresponding data for compounds detected in fuel combustion products show great similarity. Samples collected near large power stations and major airports were compared with typical urban particulate samples. Particulates collected from jet engine exhaust and a condensate from the stack effluent from a coal-fired combustion system were studied. Mass spectral data were obtained for an auto exhaust tar, a coal tar pitch and several fuels. The mass spectra of two total particulate samples, compared to the spectrum of an ether extract of the organic matter, indicate that direct vaporization can be used and extraction is not essential for qualitative mass spectral studies.
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    Analysis of intact phospholipids by field desorption mass spectrometry (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 154-155 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The first application of field desorption mass spectrometry to the analysis of intact diacyl glycerophosphorylcholines (lecithins) has led to the detection of prominent molecular ions. This technique enables positive identification of the components of a mixture of phosphatidylcholines, which will provide valuable information on the phospholipid composition of biological fluids.
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    Mass spectrometry of pesticides and pollutants, by S. Safe and O. Hutzinger. CRC Press Inc., Cleveland, Ohio, 1973. pp. 220, $32.00 (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 157-157 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200010215
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    News and events (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. xi 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200010216
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    Detection and quantitative analysis of amphetamine (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 159-162 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The high resolution mass spectrometric integrated ion current procedure has been used to identify and quantitate amphetamine, isolated as its dansyl derivative, as it is found after addition to urine and in tissues of the rat following intraperitoneal injection. A linear relationship between amphetamine and ion current response has been established at least in the range 5 × 10-12 to 5 × 10-7 g, and as little as 8 × 10-13 mol of amphetamine in urine may be detected.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200010302
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    Thin-layer chromatography-mass spectrometry for the identification of sapogenins from Digitalis species (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 166-168 
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    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is described for the identification of the sapogenins of several Digitalis species. The steroids are separated by repeated development thin-layer chromatography and identified by means of high resolution mass spectrometry. The spectra of tigogenin, gitogenin, digalogenin and digitogenin are recorded. These spectra are of particular use in establishing the position of extra hydroxy moieties in the steroid nuclei. Several species of Digitalis were screened for their sapogenin content. D. purpurea, D. mertonensis and D. lutea were found to contain tigogenin and digitogenin in small amounts, the principal steroid being gitogenin, whilst D. ambigua and D. lanata contained all four steroids.
    Additional Material: 2 Tab.
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    URL: http://dx.doi.org/10.1002/bms.1200010304
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    Intramolecular isotopic order in biologically produced acetic acid (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 172-174 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Acetic acid isolated from cider vinegar and inorganically synthesized glacial acetic acid have markedly different intramolecular isotopic distributions of the stable carbon isotopes. Carbon-12 is concentrated in the methyl group relative to the carboxyl group in the biologically produced acid. The reverse distribution is observed in the particular sample of glacial acetic acid examined here.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/bms.1200010306
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  • 90
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    Identification of some organic smog components based on rain water analysis (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 192-194 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An analysis has been made of a sample of rain water collected in Washington, D.C. following a sustained photo-oxidant smog alert which was accompanied by haze and low visibility. The analysis was effected by purging the organic content from the water with helium gas and identifying the constituents by means of gas chromatography - mass spectrometry. The predominant compound was found to be 3-methylfuran, a possible intermediate or end product of the atmospheric decomposition of terpenoid hydrocarbons. The analysis suggests that the smog resulted from the air oxidation of hydrocarbons evolved from Appalachian forestation rather than from manassociated activities.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200010309
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    Source of the carboxamide nitrogen atom in 2-carboxamido-5-isopropoxycarbonylaminobenzimidazole, a metabolite of cambendazole (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 190-191 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Combined gas chromatography-mass spectrometry and isotope labeling techniques have been employed to demonstrate that the carboxamide nitrogen atom in 2-carboxamido-5-isopropoxycarbonylaminobenzimidazole, a metabolite of 2-thiazolyl-5-isopropoxycarbonylaminobenzimidazole (cambendazole), is derived wholly from the parent drug. [15N] Thiazole-labeled cambendazole was administered to a rat and the metabolite isolated from urine. Trideutero-2-carboxamido-5-isopropoxycarbonylaminobenzimidazole was employed as a carrier to isolate the metabolite in sufficient purity for isotope ratio measurements using multiple ion detection. The metabolite was converted to its tetramethyl derivative by on-column reaction with trimethylanilium hydroxide to permit satisfactory gas chromatography.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200010308
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    Workshop reports (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 206-207 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200010312
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    News and events (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. xiii 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200010314
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    Masthead (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974) 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200010401
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    Evaluation of bilirubin derivatives for mass spectral analysis (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 219-222 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Twelve derivatives of bilirubin were evaluated from the point of view of providing intense molecular ion peaks on electron impact and unambiguous molecular weights. The tetrakis-(trimethylsilyl) derivative of bilirubin was judged to be the most suitable because its molecular ion carries 22% of the total ion current and is the base peak in the spectrum. Molecular ions were found to carry 10% of the total ion current in the spectrum of the trimethylsilylated methyl ester of the phenylazo derivative of bilirubin. Fragmentation patterns of these two compounds were studied using deuterium labeling.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200010404
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    The use of Edman degradation in peptide mixture analysis by mass spectrometryA preliminary report including some of the data presented in this paper has been given at the 6th International Mass Spectrometry Conference, Edinburgh, Scotland, September 1973. (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 231-236 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mass spectrometric analysis of peptide mixtures may lead to ambiguous results when it is possible to change from one peptide chain to another during the interpretation of the spectra. This kind of ambiguity can be eliminated by submission of part of the sample to one cycle of Edman degradation, followed by comparison of the results obtained for this preparation with those obtained for the nondegraded sample. Combination of this procedure with the use of deuterated derivatives has allowed an unambiguous interpretation for two mixtures of synthetic peptides.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200010406
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    Field desorption mass spectrometry of ten medicinal carbamates (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 256-262 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The field desorption mass spectra of ten medicinal carbamates - meprobamate, mebutamate, carisoprodol, emylcamate, bethanechol chloride, styramate, hydroxyphenamate, mephenesin carbamate, methocarbamol and chlorphenesin carbamate - were run and compared with their published electron impact spectra. Of the ten compounds run only emylcamate did not give a field desorption mass spectrum. All others gave abundant molecular ions, with the exception of bethanechol chloride which has a quarternary ammonium group and gave a field desorption spectrum characteristic of compounds possessing such a functional group. No general characteristic fragmentation was attributed to the carbamate function in the field desorption mode. However, the ease of obtaining abundant molecular ions or quasimolecular ions makes the field desorption method a valuable complementary technique to electron impact studies of carbamates.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200010409
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    The determination of sequence information in homologously related proteins by mass spectrometry (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 269-273 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An azurin, a small respiratory copper protein from the bacterium Pseudomonas fluorescens biotype G, has been studied by mass spectrometry to determine sequence information. The study of homologously related proteins by mass spectiometry is particularly attractive, since the correct nature of major parts of the deduced sequences can be confirmed by comparison with the sequences of the protein from related organisms. An oxidized tryptohan residue has been identified amongst the products from a cyanogen bromide digest of this wild type azurin. In the same digest, a product is also found to arise from cleavage of the peptide chain at the C-terminal side of the same tryptophan residue. These results are rationalized.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200010411
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    The mass spectral fragmentation of partially ethylated alditol acetates, a derivative used in determining the glycosly linkage composition of polysaccharidesSupported in part by AEC Contract No. AT(11-1)-1426.Abbreviations: PEGS = poly-(ethylene glycol succinate); PEGA = poly-(ethylene glycol adipate). (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 263-268 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mass spectral data for the primary fragmentation of partially ethylated alditol acetates have been tabulated in order to allow easy reference for the identification of these polysaccharide derivatives. Sodium borodeuteride is used in all the aldose to alditol reductions, since the presence of a single deuterium label on C-1 greatly increases the information available in the mass spectrum and allows some identifications to be made which would not otherwise be possible. The primary fragmentations of these derivatives are analogous to those of the partially methylated alditol acetates, with each fragment shifted to a higher m/e value by fourteen mass units for each ether linkage contained in the fragment. The secondary fragmentation is also very similar, being characterized by the loss of acetic acid or ketene, or, less frequently, by the loss of ethanol or acetaldehyde. Coupled with the chromatographic retention time data for the partially ethylated alditol acetates tabulated elsewhere, the unambiguous mass spectral identification makes this derivative an excellent choice as a complementary derivative to the partially methylated alditol acetates for polysaccharide analysis. The utility of the partially ethylated alditol as a routine analytical derivative is further enhanced by the almost identical procedures required for synthesis of the ethyl and methyl derivatives. Through the combined use of these derivatives, most of the possible linkage isomers of the seven common aldoses of plant cell wall polysaccharides can be resolved, identified and quantitated.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200010410
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    Characterization of cytosine nucleosides by mass spectrometry (1974)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 1 (1974), S. 281-285 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mass spectra of most nucleosides of cytosine exhibit molecular ions of low abundance, rearranged ions base + 2H in greater abundance than the companion species base + H, and a characteristic and abundant ion which corresponds to base + C2HO from the sugar. Deuterium, oxygen-18 and substituent labeling showed the presence of C-1′, 2′, H-2′ and O-4′ in the latter ion, which led to a proposed mechanism of formation involving opening of the sugar ring and recyclization between O2 and C-2′ with expulsion of water. Primary driving force for the reaction is due to resonance stabilization promoted by unshared electrons from N4, which results in diminished abundance in the case of imino isomers and derivatives which contain electron-withdrawing groups at N4, and enhanced abundance resulting from methylation at N4. Data for 24 nucleosides are presented and discussed in terms of the determination of nucleoside structure.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/bms.1200010413
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