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  • 1
    ISSN: 1572-8935
    Schlagwort(e): Poly(amide-imide)s ; Polycondensation ; Phosphorylation ; Aromatic diamines ; 1,3-bis(4-aminophenoxy)benzene ; 1, 3-bis(4-trimellitimidophenoxy)benzene
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie , Maschinenbau , Physik
    Notizen: Abstract A diamine, 1,3-bis(4-aminophenoxy) benzene (II), was synthesized in two steps; fist from the condensation of resorcinol with p-chloronitrobenzene in the presence of potassium carbonate, producing I ,3-bis(4-nitrophenoxy) benzene (I), followed by hydrazine hydrate/Pd-C reduction. A two imide rings-preformed dicarboxylic acid, 1,3-bis(4-trimellitimidophenoxy)benzene (III), was prepared from the condensation of diamine II and trimellitic anhydride in 1:2 molar ratio. A series of structurally new polyamide-imides (Va-p) were directly synthesized from the diacid III and various aromatic diamines (IVa-p). The resultant polyamide-imides had inherent viscosities between 0.56–1.39 dl/g. All polymers, except some derived from diamines with p-phenoxy structure, showed excellent solubility. Some polymer resulted in tough or flexible transparent films. Dynamic TG data indicated that all polymers possess excellent thermal stability with no significant weight loss up to the temperature of approximately 450 °C in nitrogen, and their 10% weight loss temperature was recorded in the range of 489–577 °C. Measurements of wide-angle X-ray diffraction revealed that some polymers derived from p-phenoxy group-containing diamines showed crystalline patterns.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 2
    Digitale Medien
    Digitale Medien
    Springer
    Journal of comparative physiology 174 (1994), S. 267-280 
    ISSN: 1432-1351
    Schlagwort(e): Electric fish ; Pacemaker ; GABA ; Glutamate ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The medullary pacemaker nucleus of Hypopomus triggers each electric organ discharge (EOD) by a single command pulse. It consists of electrotonically coupled ‘pacemaker’ cells, which generate the rhythm, and ‘relay’ cells, which follow the pacemaker cells and excite the spinal motoneurons of the electric organ. The pacemaker cells receive two inputs from the complex of the diencephalic prepacemaker nucleus (PPn), a GABA-ergic inhibition and a glutamatergic excitation. Relay cells, on the other hand, receive two glutamatergic inputs, one from a subnucleus of the PPn, the PPn-C, and a second from the sublemniscal prepacemaker nucleus (SPPn). We have labelled afferents to the pacemaker nucleus by injecting HRP to specific sites of the prepacemaker complex. By using immunogold-labelled antibodies and en-grid staining techniques, we demonstrated GABA and glutamate immunoreactivity in labelled synaptic profiles of ultra-thin sections of the pacemaker nucleus. The two types of synapses were interspersed on the surfaces of pacemaker cells, with GABA-immunoreactive synapses apparently representing the GABA-mediated input of the ‘PPn-I’, an inhibitory subdivision of the PPn, and glutamate-immunoreactive synapses representing the input of the ‘PPn-G’, an excitatory subdivision of the PPn. Only glutamate-immunoreactive synapses were found on relay cells.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 3
    Digitale Medien
    Digitale Medien
    Springer
    Mycopathologia 128 (1994), S. 181-192 
    ISSN: 1573-0832
    Schlagwort(e): Aflatoxin B1 ; Embryo ; Mature ; Ultrastructure ; Zea mays L.
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract Mature maize (Zea mays L.) embryos were exposed to aflatoxin B1 (AFB1) concentrations ranging from 0.1 to 25 µg/ml for 9 days. With increasing toxin concentration above 2 µg/ml, primary root elongation of germinated embryos was progressively inhibited, to reach a maximum value of 81% at 25 µ/ml toxin. An ultrastructural investigation of the subcellular alterations induced following toxin exposure provided evidence of deteriorative changes in several compartments of the plant cell. Alteration in membrane integrity (e.g., the tonoplast, plasmalemma and inner mitochondrial membrane) was a frequent feature of many cells. Apparent fusion of vacuoles, incorporation of cytoplasmic components into vacuoles and intravacuolar membrane whorls might be interpreted as deteriorative alterations. The results are discussed in the light of ultrastructural findings for other plant systems exposed to similar AFB1 concentrations, as well as findings for animal systems.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 4
    Digitale Medien
    Digitale Medien
    Springer
    Calcified tissue international 55 (1994), S. 180-189 
    ISSN: 1432-0827
    Schlagwort(e): Collagen ; Crystal habit ; Ultrastructure ; Turkey leg tendon
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin , Physik
    Notizen: Abstract Transmission electron micrographs of fully mineralized turkey leg tendon in cross-section show the ultrastructure to be more complex than has been previously described. The mineral is divided into two regions. Needlelike-appearing crystallites fill the extrafibrillar volume whereas only platelike crystallites are found within the fibrils. When the speciment is tilted through a large angle, some of the needlelike-appearing crystallites are replaced by platelets, suggesting that the needlelike crystallites are platelets viewed on edge. If so, these platelets have their broad face roughly parallel to the fibril surface and thereby the fibril axis, where the intrafibrillar platelets are steeply inclined to the fibril axis. The projection of the intrafibrillar platelets is perpendicular to the fibril axis. The extrafibrillar volume is at least 60% of the total, the fibrils occupying 40%. More of the mineral appears to be extrafibrillar than within the fibrils. Micrographs of the mineralized tendon in thickness show both needlelike-appearing and platelet crystallites. Stereoscopic views show that the needlelike-appearing crystallites do not have a preferred orientation. From the two-dimensional Fourier transform of a selected area of the cross-sectional image, the platelike crystallites have an average dimension of 58 nm. The needlelike-appearing crystallites have an average thickness of 7 nm. The maximum length is at least 90 nm. Atomic force microscopy (AFM) of unstained, unmineralized turkey leg tendon shows collagen fibrils very much like shadow replicas of collagen in electron micrographs. AFM images of the mineralized tendon show only an occasional fibril. Mineral crystallites are not visible. Because the collagen is within the fibrils, the extrafibrillar mineral must be embedded in noncollagenous organic matter. When the tissue is demineralized, the collagen fibrils are exposed. The structure as revealed by the two modalities is a composite material in which each component is itself a composite. Determination of the properties of the mineralized tendon from the properties of its elements is more difficult than considering the tendon to be just mineral-filled collagen.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 5
    ISSN: 1432-0827
    Schlagwort(e): In vitro ; Bioactive glass ceramic ; Mineralization ; Bone bonding mechanisms ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin , Physik
    Notizen: Abstract Rat bone cells were cultured in the presence of bioactive glass-ceramic containing crystalline apatite and wollaston te. Scanning electron microscopy observations of the surface of the seeded ceramic disks revealed that cells attached, spread, and proliferated on the material surface. Soaking in cell-free culture medium showed that no change occurred in the surface structure. However, when cultured with bone cells and observed under a transmission electron microscope, an electron-dense layer was noted initially at the surface of the material, before bone formation occurred. In addition, energy-dispersive X-ray microanalysis demonstrated the presence of calcium and phosphorus in this layer. Progressively, during the following days of culture, active osteoblasts synthetized and laid down an osteoid matrix composed of numerous collagen fibrils arranged either parallel or perpendicularly to the first-formed electron-dense layer. Mineralization initiated on the ceramic surface dispersed then along the collagenous fibrils, leading to a mineralized matrix which surrounded the ceramic particles. These results demonstrate the capacity of apatite-wollastonite glass ceramic to initiate biomineralization in osteoblast cultures and to achieve a direct bond between the surface apatite layer of the bioactive glass-ceramic and the mineralized bone matrix.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 6
    Digitale Medien
    Digitale Medien
    Springer
    Calcified tissue international 55 (1994), S. 398-400 
    ISSN: 1432-0827
    Schlagwort(e): Enamel ; Proteins ; Phosphorylation ; Amelogenins ; Tooth
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin , Physik
    Notizen: Abstract The amelogenins of the extracellular matrix of developing dental enamel, comprise a family of tissue-specific proteins which are postulated to play a central role in the biomineralization of dental enamel [1]. The primary structures of amelogenins derived from cow, pig, human, mouse and rat have now been elucidated by the interpretation of cDNA sequences or by direct amino acid sequence determinations [2–6] demonstrating a high degree of sequence homology between species [1]. However, the nature of post-translational modification of these proteins is less clear. In particular, early reports of amelogenin phosphorylation [7–8] have proved to be difficult to confirm by direct chemical analyses [1]. Using mass spectrographic analysis, we recently [9], reported that the lower molecular weight (5–7 kDa) bovine and porcine amelogenin polypeptides (TRAP and LRAP) contained a single phospho-serine residue at position 16Ser and, since these polypeptides are derived by proteolytic processing from the higher molecular weight “parent” amelogenins (18–25 kDa), we concluded that these precursor molecules must also be phosphorylated, as has previously been suggested [10]. In contrast to these observations, an extensive amino acid sequencing study of porcine amelogenins has recently reported no evidence for such phosphorylation [11]. We now report that a new analysis of the major porcine(“20K”) amelogenin provides positive evidence for porcine amelogenin phosphorylation.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 7
    Digitale Medien
    Digitale Medien
    Springer
    Archives of microbiology 162 (1994), S. 267-271 
    ISSN: 1432-072X
    Schlagwort(e): Key words     Extremely thermophilic eubacterium ; Calderobacterium hydrogenophilium ; Ultrastructure ; Electron microscopy
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract       Calderobacterium hydrogenophilum is an extreme thermophilic, obligately chemoautotrophic, hydrogen-oxidizing bacterium. The cells were shown to be non-motile straight rods of average size 0.4 × 2.5 μm. After negative-staining of the whole cells, no flagella were observed. The multilayered cell wall was of type 1 and possessed a crystalline proteinaceous surface layer exhibiting p4 symmetry. The square unit cells had a lattice constant of approximately 11 nm. Cell division occurred by a constriction mechanism. C. hydrogenophilum differred from a similar hydrogen-oxidizing eubacterium, Hydrogenobacter thermophilus, by the absence of intracytoplasmic membrane structures in chemically fixed cells. However, an electron-dense intracytoplasmic hemispherical structure adhering to the inner membrane was frequently observed.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 8
    Digitale Medien
    Digitale Medien
    Springer
    Archives of microbiology 162 (1994), S. 267-271 
    ISSN: 1432-072X
    Schlagwort(e): Extremely thermophilic eubacterium ; Calderobacterium hydrogenophilium ; Ultrastructure ; Electron microscopy
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract Calderobacterium hydrogenophilum is an extreme thermophilic, obligately chemoautotrophic, hydrogen-oxidizing bacterium. The cells were shown to be nonmotile straight rods of average size 0.4x2.5 μm. After negative-staining of the whole cells, no flagella were observed. The multilayered cell wall was of type 1 and possessed a crystalline proteinaceous surface layer exhibiting p4 symmetry. The square unit cells had a lattice constant of approximately 11 nm. Cell division occurred by a constriction mechanism. C. hydrogenophilum differred from a similar hydrogen-oxidizing eubacterium, Hydrogenobacter thermophilus, by the absence of intracytoplasmic membrane structures in chemically fixed cells. However, an electron-dense intracytoplasmic hemispherical structure adhering to the inner membrane was frequently observed.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 9
    Digitale Medien
    Digitale Medien
    Springer
    The journal of membrane biology 139 (1994), S. 31-40 
    ISSN: 1432-1424
    Schlagwort(e): Connexin45 ; Gap junction ; Intercellular communication ; Phosphorylation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Chemie und Pharmazie
    Notizen: Abstract Connexin45 is a gap junction protein which forms channels with unique characteristics. RNA blots demonstrated that connexin45 is expressed in a number of cell lines including WB, SK Hepl, BHK, A7r5, CLEM, and BWEM cells. Connexin45 was further studied in BWEM cells using specific affinity-purified antibodies directed against a synthetic peptide representing amino acids 285–298 of its sequence. Immunofluorescence experiments demonstrated that the BWEM cells expressed both connexin43 and connexin45 and that these connexins colocalized. Connexin45 polypeptide, immunoprecipitated from BWEM cells metabolically labeled with [35S]-methionine, consisted of a predominant 48 kD polypeptide. Connexin45 and connexin43 contained radioactive phosphate when immunoprecipitated from BWEM cells metabolically labeled with [32P]-orthophosphoric acid. This phosphate label was removed from connexin45 by alkaline phosphatase digestion. Treatment of BWEM cells with the tumor promoting agent 12-O-tetradecanoylphorbol-13-acetate (TPA) inhibited intercellular passage of microinjected Lucifer yellow. While TPA treatment induced phosphorylation of connexin43 in these cells, it reduced the expression of connexin45. Furthermore, the connexin45 expressed after TPA treatment was not phosphorylated. These results suggest that treatments which alter protein phosphorylation may regulate connexin43 and connexin45 in BWEM cells by different mechanisms.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 10
    Digitale Medien
    Digitale Medien
    Springer
    Cell & tissue research 277 (1994), S. 87-95 
    ISSN: 1432-0878
    Schlagwort(e): Key words: Blood-brain barrier ; Anionic sites ; Larvae ; Septate junctions ; CNS ; Glia ; Ultrastructure ; Drosophila melanogaster (Insecta)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract. The blood-brain barrier ensures brain function in vertebrates and in some invertebrates by maintaining ionic integrity of the extraneuronal bathing fluid. Recent studies have demonstrated that anionic sites on the luminal surface of vascular endothelial cells collaborate with tight junctions to effect this barrier in vertebrates. We characterize these two analogous barrier factors for the first time on Drosophila larva by an electron-dense tracer and cationic gold labeling. Ionic lanthanum entered into but not through the extracellular channels between perineurial cells. Tracer is ultimately excluded from neurons in the ventral ganglion mainly by an extensive series of (pleated sheet) septate junctions between perineurial cells. Continuous junctions, a variant of the septate junction, were not as efficient as the pleated sheet variety in blocking tracer. An anionic domain now is demonstrated in Drosophila central nervous system through the use of cationic colloidal gold in LR White embedment. Anionic domains are specifically stationed in the neural lamella and not noted in the other cell levels of the blood-brain interface. It is proposed that in the central nervous system of the Drosophila larva the array of septate junctions between perineurial cells is the physical barrier, while the anionic domains in neural lamella are a “charge-selective barrier” for cations. All of these results are discussed relative to analogous characteristics of the vertebrate blood-brain barrier.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 11
    ISSN: 1432-0878
    Schlagwort(e): Key words: C-PON ; Neuropeptide Y ; Neostriatum ; Immunocytochemistry ; Ultrastructure ; Erinaceus europaeus (Insectivora)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract. The present study provides light- and electron-microscopic immunocytochemical data on the presence of neurons that are immunoreactive to the C-terminal flanking peptide of neuropeptide Y, C-PON, in the neostriatum of the hedgehog (Erinaceus europaeus). Positive neurons have mostly fusiform or round perikarya from which two to four poorly branched processes arise. Immunostained fibers and puncta are also evenly distributed throughout the neostriatum. Ultrastructurally, each neuron exhibits a deeply invaginated nucleus surrounded by abundant cytoplasm with a well-developed rough endoplasmic reticulum and Golgi apparatus. Positive neurons receive symmetric and asymmetric synapses from unlabeled terminals. The results of this study can be correlated with previous findings, as the C-PON-positive neurons of the hedgehog resemble medium-sized neostriatal neurons that are known to be local circuit neurons exhibiting C-PON in the rat. Thus, a high degree of C-PON neuronal system phylogenetic conservation and function can be postulated for the neostriatum of mammals.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 12
    Digitale Medien
    Digitale Medien
    Springer
    Cell & tissue research 277 (1994), S. 87-95 
    ISSN: 1432-0878
    Schlagwort(e): Blood-brain barrier ; Anionic sites ; Larvae ; Septate junctions ; CNS ; Glia ; Ultrastructure ; Drosophila melanogaster (Insecta)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The blood-brain barrier ensures brain function in vertebrates and in some invertebrates by maintaining ionic integrity of the extraneuronal bathing fluid. Recent studies have demonstrated that anionic sites on the luminal surface of vascular endothelial cells collaborate with tight junctions to effect this barrier in vertebrates. We characterize these two analogous barrier factors for the first time on Drosophila larva by an electron-dense tracer and cationic gold labeling. Ionic lanthanum entered into but not through the extracellular channels between perineurial cells. Tracer is ultimately excluded from neurons in the ventral ganglion mainly by an extensive series of (pleated sheet) septate junctions between perineurial cells. Continuous junctions, a variant of the septate junction, were not as efficient as the pleated sheet variety in blocking tracer. An anionic domain now is demonstrated in Drosophila central nervous system through the use of cationic colloidal gold in LR White embedment. Anionic domains are specifically stationed in the neural lamella and not noted in the other cell levels of the blood-brain interface. It is proposed that in the central nervous system of the Drosophila larva the array of septate junctions between perineurial cells is the physical barrier, while the anionic domains in neural lamella are a “charge-selective barrier” for cations. All of these results are discussed relative to analogous characteristics of the vertebrate blood-brain barrier.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 13
    ISSN: 1432-0878
    Schlagwort(e): Odontoclasts ; Resorption ; Predentine ; Ultrastructure ; Histochemistry ; TR-ACPase (tartrateresistant acid phosphatase) ; Deciduous teeth ; Shedding ; Human
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract Resorption by odontoclasts of a superficial nonmineralized layer of predentine that occurs in prior to the shedding of human deciduous teeth was studied by light and electron microscopy. As resorption of the tooth roots neared completion, multinucleate cells appeared on the predentine surface of the coronal dentine between the degenerated odontoblasts, excavated characteristic resorption lacunae in the nonmineralized predentine. These multinucleate cells had the same ultrastructural characteristics as odontoclasts and histochemical demonstration of tartrate-resistant acid phosphatase activity in the multinucleate cells revealed intense staining in numerous small granules identified as lysosomes. Occasionally, the multinucleate cells simultaneously resorbed both nonmineralized and calcospherite-mineralized matrix in the predentine. The study demonstrates that multinucleate odontoclasts can resorb nonmineralized predentine matrix in vivo, probably in the same way as they resorb demineralized organic matrix in the resorption zone underlying their ruffled border.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 14
    ISSN: 1432-0878
    Schlagwort(e): C-PON ; Neuropeptide Y ; Neostriatum ; Immunocytochemistry ; Ultrastructure ; Erinaceus europaeus (Insectivora)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The present study provides light- and electronmicroscopic immunocytochemical data on the presence of neurons that are immunoreactive to the C-terminal flanking peptide of neuropeptide Y, C-PON, in the neostriatum of the hedgehog (Erinaceus europaeus). Positive neurons have mostly fusiform or round perikarya from which two to four poorly branched processes arise. Immunostained fibers and puncta are also evenly distributed throughout the neostriatum. Ultrastructurally, each neuron exhibits a deeply invaginated nucleus surrounded by abundant cytoplasm with a well-developed rought endoplasmic reticulum and Golgi apparatus. Positive neurons receive symmetric and asymmetric synapses from unlabeled terminals. The results of this study can be correlated with previous findings, as the C-PON-positive neurons of the hedgehog resemble medium-sized neostriatal neurons that are known to be local circuit neurons exhibiting C-PON in the rat. Thus, a high degree of C-PON neuronal system phylogenetic conservation and function can be postulated for the neostriatum of mammals.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 15
    ISSN: 1432-0878
    Schlagwort(e): Sarcolemma ; Surface tubules ; Smooth muscle ; Endothelial cells ; Fibroblasts ; Ultrastructure ; Lamprey, Lampetra japonica (Cyclostomata)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract Numerous tubular structures were observed in the surface region of smooth muscle cells making up the vascular walls in the lamprey, Lampetra japonica; they were designated as surface tubules. The limiting membrane of the surface tubules was connected to the plasma membrane, allowing communication of the lumen of the tubule with the extracellular space. Tannic acid reacted with osmium, serving as an extracellular marker, penetrated into the tubules but not into the intracellular organelles, such as the endoplasmic reticulum and the Golgi complex. The surface tubules were grouped in longitudinal parallel rows, separated from each other by tubule-free areas where dense plaques were present. Each tubule was fairly cylindrical (approximately 60 nm in diameter) and often ramified into two or three branches with a blind end. Occasionally, these tubules were encircled by the sarcoplasmic reticulum which was located immediately beneath the plasma membrane. Similar tubules were also observed in the surface region of vascular endothelial cells and fibroblasts in the adventitial connective tissue. The possibility that the surface tubules in the present observations are analogous to the smooth muscle caveolae or the striated muscle T-tubule is discussed.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 16
    ISSN: 1432-0878
    Schlagwort(e): Glucagon-like peptide 1 ; Endocrine tumors ; Immunohistochemistry ; Ultrastructure ; Multiple endocrine neoplasia type 1 ; Co-localization ; Man
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The preproglucagon gene encodes, in addition to glucagon, two smaller peptides with structural similarity: glucagon-like peptides 1 and 2. Glucagon-like peptide 1 (GLP-1) 7–36 amide is the most powerful incretin candidate. In the present study, GLP-1 immunoreactivity was investigated in tissue specimens of various types of gastroenteropancreatic tumors, and the serum-levels of GLP-1 were assayed. Immunohistochemical staining of 88 tumors revealed GLP-1 immunoreactivity in 17 neoplasias (19.3 %), viz., in 7 out of 33 non-functioning tumors, 4 out of 20 gastrinomas, 4 out of 13 insulinomas, 1 out of 3 vasoactive-intestinal-polypeptide (VIP)omas and 1 adrenocorticotropic-hormone (ACTH)-producing tumor. In these tumors, GLP-1-immunoreactive cells were distributed either diffusely, arranged in clusters, or as single cells. All GLP-1-positive tumors were immunoreactive for glucagon or glicentin, 10 tumors were immunoreactive for pancreatic polypeptide, and 8 tumors for insulin. Ultrastructural analysis of 8 GLP-1-positive tumors, with the immunogold technique, demonstrated GLP-1 immunoreactivity mainly in cells resembling the A-cells of the pancreas or the L-cells of the gut. Of the 17 GLP-1-immunoreactive tumors, 15 were primarily located in the pancreas. Additionally, 2 non-functioning tumors of the rectum were GLP-1 immunoreactive. Five tumors were GLP-1 immunoreactive from 9 patients with multiple endocrine neoplasia I syndrome. Patients with GLP-1-immunoreactive tumors were characterized by a significantly lower rate of distant metastases (P〈0.01) and a higher rate of curative resections (P〈0.05). In 2 out of 22 patients, elevated serum-levels of GLP-1 were found: one patient with a vasoactive-intestinal-polypeptide (VIP)oma and 1 patient with a non-functioning tumor. This indicates that GLP-1 might be secreted at least by a few gastroenteropancreatic endocrine tumors.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 17
    ISSN: 1432-0878
    Schlagwort(e): Abdominal nerve neurohaemal area ; FMRFamide ; Immunogold-labelling ; Serotonin ; Ultrastructure ; Rhodnius prolixus (Insecta)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The ultrastructure of neurohaemal areas on abdominal nerves of the blood-sucking bug Rhodnius prolixus was investigated. Four types of axon terminals were found, distinguished by the morphology of their neurosecretory granules. By use of post-embedding immunogold labelling, granules in Type I axon terminals were shown to contain serotonin-like immunoreactive material, and granules in Type II axon terminals were shown to contain FMRFamide-like immunoreactive material. There was no colocalization of these materials. It is suggested that Type III terminals contain peptidergic diuretic hormone, which has previously been reported to be present in electron-dense neurosecretory granules in this neurohaemal area. The identity of material in Type IV terminals is unknown.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 18
    ISSN: 1432-0878
    Schlagwort(e): Key words: Abdominal nerve neurohaemal area ; FMRFamide ; Immunogold-labelling ; Serotonin ; Ultrastructure ; Rhodnius prolixus (Insecta)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract. The ultrastructure of neurohaemal areas on abdominal nerves of the blood-sucking bug Rhodnius prolixus was investigated. Four types of axon terminals were found, distinguished by the morphology of their neurosecretory granules. By use of post-embedding immunogold labelling, granules in Type I axon terminals were shown to contain serotonin-like immunoreactive material, and granules in Type II axon terminals were shown to contain FMRFamide-like immunoreactive material. There was no colocalization of these materials. It is suggested that Type III terminals contain peptidergic diuretic hormone, which has previously been reported to be present in electron-dense neurosecretory granules in this neurohaemal area. The identity of material in Type IV terminals is unknown.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 19
    Digitale Medien
    Digitale Medien
    Springer
    Cell & tissue research 275 (1994), S. 339-344 
    ISSN: 1432-0878
    Schlagwort(e): Secretory granules ; Golgi apparatus ; Haloperidol ; Ultrastructure ; Pituitary gland, pars intermedia ; Rat (Sprague Dawley)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The formation of secretory granules in chronically hypersecretory melanotrophs in the rat pituitary was studied. Hypersecretion was induced by treatment with the dopamine antagonist haloperidol (1.5 mg/kg daily for 7 days), which releases the normal neural dopaminergic inhibition of secretion from the melanotroph. Morphometric analysis showed a 100% increase in the volume fraction of granular endoplasmic reticulum after haloperidol treatment, while the volume fractions of electron-dense granules, electron-lucent granules and the Golgi apparatus were unaltered. The mean diameter of the mature secretory granules was increased by 10%, indicating a 30% increase in mean granule volume. A similar increase in diameter was observed in condensing granules within the Golgi area. With earlier results on the effect of chronic inhibition the study shows that a main adaptive response of the melanotroph to altered secretory conditions is a change in the volume of the secretory granules, regulated by a mechanism that operates at an early stage of granule formation.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 20
    Digitale Medien
    Digitale Medien
    Springer
    Cell & tissue research 275 (1994), S. 481-492 
    ISSN: 1432-0878
    Schlagwort(e): Skin ; Ultrastructure ; Endogenous peroxidase ; Water acidification ; Cyprinus carpio (Teleostei)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The skin of carp was examined after exposure to acidified water. Degenerative cells were common in the upper epidermal layers. During the first days most of these cells exhibited signs of necrosis. Later on the incidence of necrosis decreased and that of apoptosis increased. In the acid-exposed fish, the upper filament cells and pavement cells produced secretory vesicles of high electron density, some of which showed peroxidase activity. This enzyme activity was also present in the glycocalyx covering these cells, and in the cytoplasm of apoptotic cells. Mitotic figures and newly differentiating mucous cells were common in the outer epidermal layers. Mucous cells became elongated and produced mucosomes of high electron density. Mucosomes with peroxidase activity were also found. Club cells increased in number. Chloride cells and solitary chemo-sensory cells, not seen in the controls, appeared in the upper epithelial layer. The skin was invaded by many leucocytes and by pigment-containing cytoplasmic extensions of melanocytes. Some leucocytes apparently penetrated into the club cells. These structural observations reflect the complexity of the physiological response of the skin to acid water.
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  • 21
    ISSN: 1432-0878
    Schlagwort(e): Comb cell ; Growth cone ; Motility ; Substrate ; Basement membrane ; Ultrastructure ; Hirudo medicinalis (Annelida)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The oblique muscle organizer (Comb- or C-cell) in the embryonic medicinal leech, Hirudo medicinalis, provides an amenable situation to examine growth cone navigation in vivo. Each of the segmentally iterated C-cells extends an array of growth cones through the body wall along oblique trajectories. C-cell growth cones undergo an early, relatively slow period of extension followed by later, protracted and rapid directed outgrowth. During such transitions in extension, guidance might be mediated by a number of factors, including intrinsic constraints on polarity, spatially and temporally regulated cell and matrix interactions, physical constraints imposed by the environment, or guidance along particular cells in advance of the growth cones. Growth cones and their environment were examined by transmission electron microscopy to define those factors that might play a significant role in migration and guidance in this system. The ultrastructural examination has made the possibility very unlikely that simple, physical constraints play a prominent role in guiding C-cell growth cones. No anatomically defined paths or obliquely aligned channels were found in advance of these growth cones, and there were no identifiable physical boundaries, which might constrain young growth cones to a particular location in the body wall before rapid extension. There were diverse associations with many matrices and basement membranes located above, below, and within the layer in which growth cones appear to extend at the light level. Additionally, a preliminary examination of myocyte assembly upon processes proximal to the growth cones further implicates a role for matrix-associated interactions in muscle histogenesis as well as process outgrowth during embryonic development.
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  • 22
    ISSN: 1432-0878
    Schlagwort(e): Endocrine pancreas ; Ontogeny ; Ultrastructure ; Dicentrarchus labrax (Teleostei)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The primordial cord and the primitive, single and primordial islets present in the 3 earliest stages of the developing endocrine pancreas of sea bass were studied ultrastructurally. The primordial cord consisted of type I and II cells and was included in the gut. Besides these cell types, X cells were seen in the primitive islet. The single islet was made up of type I, II, III and IV cells. A correlation between these endocrine cell-types and cells previously identified immunocytochemically, was established. Type I, II, III and IV cells, correlated respectively with SST-25-, insulin-, SST-14- and glucagon-immunoreactive cells, and could be related to the D1, B, D2 and A cells, respectively, of older larvae and adult sea bass. Each cell type shows characteristic secretory granules from its first appearance. A progressive development of the organelles and an increase in the number and size of the secretory granules, whose ultrastructure also varied, was observed in the endocrine cells of the primordial cord and the succeeding islets. In 25-day-old larvae at the beginning of the fourth developmental stage, the primordial islet, the first ventral islet found, was close to a pancreatic duct and blood vessel, and consisted of type I and II cells whose ultrastructure was similar to that of the type I and II cells in the primordial cord. These data suggest a ductular origin for the pancreatic endocrine cells in the ventral pancreas. It is suggested that although endocrine cells undergo mitosis, their increase in number during the earliest development stages is principally due to the differentiation of surrounding cells.
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  • 23
    ISSN: 1432-0878
    Schlagwort(e): Endocrine pancreas ; Ontogeny ; Ultrastructure ; Dicentrarchus labrax (Teleostei)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The big and secondary islets of sea bass larvae were characterized ultrastructurally from, 25 to 60 days after hatching. From the 25th day, big islets consisted of inner type II and III, external type I and peripheral type IV cells. From the 55th day, type V cells appeared in limited peripheral areas. Secondary islets, first found in 32-day-old larvae, were made up of inner type II and III, external type I, and peripheral either type IV and V cells (type I islets), or only type V cells (type II islets). Type I cells contained secretory granules with a fine granular, low-medium electron-dense material, whereas the secretory granules of type II cells were smaller and had a high electron-dense core with diffused limits; needle and rod-like crystalloid contents were occasionally found. Type III secretory granules posessed a homogeneous, high or medium electron-dense material with or without a clear halo. Type IV cells had secretory granules with a polygonal dense core embedded in a granular matrix and granules containing a high or medium electron-dense material. Type V cells had secretory granules with a fine granular, high or medium electron-dense content. These cell-types correlated with cells previously identified immuno-cytochemically, as regards to their distribution in the islets, and related to those characterized ultrastructurally in adult specimens. Thus, types I, II, III, IV and V correspond to D1, B, D2, A and PP cells, respectively. From the 32nd day onwards, endocrine cells of all the different types were found grouped, type V cells also being observed in isolation close to pancreatic ducts and/or blood vessels. Small groups consisting of type I and II cells were found in 40-day-old larvae. A mitotic centroacinar ductular cell containing some secretory granules similar to those of type I cells, was seen adjacent to a type I cell. As the larvae grew older, the endoplasmic reticulum developed, the number of free ribosomes decreased, and the number and size of the secretory granules increased. Dark type I, II, III, IV and V cells were found in the islets and cell clusters from the 55th day onwards.
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  • 24
    ISSN: 1432-0878
    Schlagwort(e): Platelets ; Storage ; Ultrastructure ; Freeze fracture ; Transmission electron microscopy ; Human
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract We report the ultrastructural changes occurring in human platelets during eight days of storage. Extension of pseudopodia is frequently observed, but a concentration of organelles in the centre of the platelets is found only in a minor fraction (∼5%). Striking changes can be observed in both the granules and the open canalicular system. In fresh platelets, the latter often has the form of stacked membranes that have no lumen, but these membranes separate and spread with increasing storage time. However, the openings of this system on the outer surface of the platelet remain unchanged. Some of these features differ from the morphological description of platelets activated by thrombin or ADP, and suggest that the storage lesion is the result of a prolonged weak activation that leads to an incomplete release reaction within the first five days.
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  • 25
    ISSN: 1432-0878
    Schlagwort(e): Yolk sac ; Tubular endosomes ; Smooth endoplasmic reticulum ; Ultrastructure ; Endocytosis ; Rat (Wistar)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The three-dimensional architecture of the tubular endocytic apparatus and the endoplasmic reticulum in the rat yolk-sac endoderm was investigated after loading with horseradish peroxidase-conjugated concanavalin A by intrauterine administration. After 30 min, small vesicles (50–150 nm in diameter), small tubules (80–100 nm in diameter) and large vacuoles (0.2–1.0 μm in diameter) in the apical cytoplasm were labeled with the tracer, but lysosomes (1.0–3.5 μm in diameter) in the supranuclear cytoplasm were not labeled until 60 min after loading. Stereo-viewing of the labeled small tubules in thick sections revealed that they were not isolated structures but formed three-dimensional anastomosing networks, which were also confirmed by scanning electron microscopy after maceration with diluted osmium tetroxide. Their earlier labeling with the endocytic tracer, localization in the apical cytoplasm and three-dimensional network formation indicated that the labeled small tubules represented tubular endosomes (tubular endocytic apparatus). These well-developed membranous networks provided by the tubular endosomes are suggested to facilitate the receptor-mediated endocytosis and transcytosis of the maternal immunoglobulin in the rat yolk-sac endoderm. Scanning electron microscopy further revealed lace-like networks of the smooth endoplasmic reticulum near the lateral plasma membrane. Their possible involvement in transport of small molecules or electrolytes is discussed.
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  • 26
    Digitale Medien
    Digitale Medien
    Springer
    Protoplasma 179 (1994), S. 142-150 
    ISSN: 1615-6102
    Schlagwort(e): Dinoflagellate ; Eyespot ; Gymnodinium natalense ; Ontogeny ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Summary Ultrastructure and ontogeny of a new type of eyespot in dinoflagellates is described. A marine tidal poolGymnodinium natalense is found to possess a highly organized eyespot whose structure is unique among dinoflagellates. The eyespot is rectangular in ventral view, C-shaped in apical view, and is located posterior to the sulcus. The eyespot is independent of the chloroplast and consists of several (typically six) layers of hemi-cylindrical walls which are concentrically arranged with narrow spacing between them. Each hemicylindrical wall is enclosed by a single unit membrane and is composed of many regularly arranged rectangular crystalline bricks. These crystalline bricks are produced in small vesicles which are formed in the invaginations of the chloroplast. The vesicles containing newly formed crystalline bricks are then transported to the sulcal area to assemble the eyespot. The crystalline bricks are arranged in a neat row within the vesicle termed “eyespot forming vesicle” (EFV), which is located near the sulcus. The hemi-cylindrical wall is constructed within the EFV. Based on the structure of the eyespot, viz. consisting of concentric multi-layered walls, the eyespot is thought to act as a quarter-wave stack antenna.
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  • 27
    Digitale Medien
    Digitale Medien
    Springer
    Protoplasma 178 (1994), S. 34-47 
    ISSN: 1615-6102
    Schlagwort(e): Appressorium ; Cochliobolus sativus ; Electron microscopy ; Thigmotropism ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Summary GerminatingCochliobolus sativus spores were induced to form appressoria on a variety of artificial surfaces, including replicas of the barley leaf surface. Evidence was obtained for the involvement of chemical and topographic signals during induction of appressorium formation inC. sativus. Germ tube thigmotropism was also observed in vitro. Ultrastructure relevant to appressorium formation was observed, including the germ tube apex, apical swelling of the germ tube apex prior to appressorium formation, the appressorium with associated septation and the penetration peg. Cytochemical probes applied to germlings at the electron microscope level failed to detect α-D-mannan, α-D-glucan, β-D-galactan, D-glcNAc or D-galNAc polymers in the extracellular mucilage associated with the fungal germlings. The ultrastructure of hyphal apices from germlings grown under different nutritional conditions differed with respect to Spitzenkörper morphology, apex shape and in the quantity of associated extracellular mucilage. Experimental findings are discussed relative to current understanding of appressorium induction in more extensively studied systems.
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  • 28
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Column-switching ; Determination of triamterene ; Fluorescence detection
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A liquid chromatographic method incorporating column-switching and fluorimetric detection for the determination of triamterene in untreated urine, is described. The urine samples (5 μL) were directly introduced onto an Hypersil ODS-C18, 30 μm (20 mm×2.1 mm I.D.) pre-column. Polar urinary compounds were removed by flushing the pre-column with water for 1 min, and the analyte was then switched onto an HP-LiChrospher RP C18,5 μm (125 mm×4mm ID) analytical column using an acetonitrile/phosphate buffer gradient elution. Fluorescence detection was performed at 230 nm excitation and 430 nm emission wavelengths. The recovery of drug was 102±2% in the 0.10–20.0 μg/mL concentration range, the limit of detection being 5 ng/mL. A validation of the usefulness of this procedure was accomplished by analysing urine extracts obtained from real samples.
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  • 29
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Characterization of reversed phases ; Column hydrophobicity ; Column hydrophylicity
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The validity of a method for characterizing stationary phases for reversed-phase, liquid chromatography, based on the use of homologous series, has been evaluated. The method is based on a retention model which describes the dependence of the logarithm of the capacity factor on mobile phase composition and the carbon number of specific homologous series. A first-order as well as a second-order version of this model was investigated. The second-order model proved to be a significant improvement on the first-order model, even for smaller mobile-phase ranges. Nevertheless both models showed a significant lack of fit, reflecting the incompleteness of these models. Therefore, it is very questionable whether this method is suitable to describe HPLC-column characteristics like hydrophobicity and hydrophylicity.
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  • 30
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Copoly(styrene/acrylonitrile) ; Gradient elution ; Precipitation chromatography of polymers ; Solubility of polymers
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Copolymers from styrene and acrylonitrile could be separated according to composition by gradient elution through methanol after injection inton-heptane and sudden addition of 50, 60, or 70 vol% tetrahydrofuran. The peak sequence was the same as with a common binary gradientn-heptane/tetrahydrofuran, i.e., retention increased with acrylonitrile content of the samples. With copolymers containing 37, 31, or 26% acrylonitrile, the elution characteristics in the ternary systems could be logically extrapolated towards the points measured in the corresponding binary gradient system.
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  • 31
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Chiral recognition ; Aminoalkylphosphonic acid derivatives ; β-cyclodextrin bonded phases
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An acetylated β-cyclodextrin column was used to analyse the enantiomeric resolution of a number of aminophosphonic acids. Effects of the structure of these compounds on the extent of separation was examined. Molecular modelling studies were also carried out in an attempt to relate any interaction between the amino and phosphonic acid groups to chiral recognition by the stationary phase.
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  • 32
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Chiral separation ; Association constants ; Frontal analysis ; Cyclodextrin bonded-phases
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The interaction between cyclodextrin and the drug (1R,2S,3S,4S)-(5Z)-7-(3-((phenylsulfonyl)amino)bicyclo[2.2.1]hept-2-yl)hept-5-enoic acid ((+)-S-145), was studied using α-, β-, and γ-cyclodextrin bonded-phase columns. Retention behavior of (+)-S-145 on these columns revealed that the strength of inclusion was β→γ→α-cyclodextrin. Interaction between β-cyclodextrin and (+)-S-145 was found to increase as the proportion of carboxylic ion in the (+)-S-145 molecule increased. Comparison of binding capacities of these bondedsilica gels obtained by frontal analysis and surface coverage indicated that availability of the immobilized β- and γ-cyclodextrin was 20–25%. The synthesized β-cyclodextrin bonded-phase column was superior to that of commercial columns in terms of chiral separation of (±)-S-145. A typical usage of the β-cyclodextrin column is discussed for separation of (±)-S-145 in plasma samples.
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  • 33
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Primary and secondary aliphatic alcohols ; Aqueous derivatization ; Phthalic acid monoesters
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Determination of primary and secondary aliphatic alcohols in aqueous and nonaqueous solutions by high-performance liquid chromatography (HPLC) is described. The alcohol is derivatized with phthalic anhydride to yield the corresponding monophthalate. Separation of the derivative is achieved on an ODS-10 reverse phase (RP) column by elution with an appropriate isocratic mobile phase of acetonitrile and aqueous phosphoric acid (0.1%). Detection is accomplished by UV absorption at 230 nm or 280 nm giving linear calibration plots, for alcohols in aqueous solution from 0.05% to 0.50% (w/v) and in pyridine solution from 0.0025% to 0.0250% (w/v).
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  • 34
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Hybrid mobile phases containing alcohols ; Solute-micelle association constants ; Polynuclear aromatic hydrocarbons
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The interaction between some polynuclear aromatic hydrocarbons of environmental concern, and sodium dodecylsulphate and hexadecyltrimethylammonium bromide in the presence of methanol, 2-propanol and n-butanol has been evaluated by high-performance liquid chromatography using micellar mobile phases. Solute-micelle association constants have been determined for the compounds investigated. The results show that the addition of the alcohol to the mobile phase decreases the association constant values, methanol 〈2-propanol 〈n-butanol, relative to those in the absence of any additive.
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  • 35
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 38 (1994), S. 571-578 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Wine ; Biogenic amines ; Solid-phase extraction ; Derivatization
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A method suitable for the determination of 19 biogenic amines in wine has been developed. The method involves derivatization of amines by treatment with dansyl chloride and solid-phase extraction of the derivatives. Prior to the derivatization procedure, clean-up of the wine sample with polyvinylpyrrolidone is carried out. Reversed-phase gradient elution HPLC with UV detection at 250 nm was used to determine these compounds. Some consideration was given to the effect of temperature on the separation process. Linearity of derivatization was obtained for amounts of all the biogenic amines ranging from 500 μg·L−1 to 20 mg·L−1. Limits of detection (signal-to-noise ratio=3) of the amines were similar for all the dansylderivatives (between 50 and 150 μg·L−1). Addition of standard amines was used for the determination of amine recoveries. These were better than 85% for ethanolamine, tryptamine, phenetylamine, putrescine, cadaverine and histamine. The overall process was succesfully applied to identify and quantify biogenic amines in white and red wines.
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  • 36
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 38 (1994), S. 629-632 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Chiral/enantiomeric iseparation ; Cellulose-based chiral phases ; Tifluadom analogues ; 2-acylaminomethyl-1,4-benzodiazepines
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The resolution of nine recamic mixtures of tifluadom analogues has been evaluated using the chiral stationary phases Chiralcel OD and Chiralcel OJ. The separation was performed on an analytical scale to optimize the conditions for chiral resolution, approaching baseline separation, of the two enantiomers. Eight racemates were baseline separated on Chiralcel OJ using a mobile phase of hexane/2-propanol.
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  • 37
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Phenolic compounds ; Ion-pair solid-phase extraction ; Comparison of sorbents
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A comparative study of the solid phase extraction of phenolic compounds in water was carried out. Three different sorbents, C18, CH and PLRP-S, were tested for the preconcentration process in order to determine phenolic compounds in water at μg l−1 levels by reversed-phase LC separation and diode-array detection. The addition of an ion-pair reagent in the extraction process was also studied in order to increase the breakthrough volume of some compounds. Using the optimized conditions the limit of detection was less than 0.5 μg l−1, the maximum admissible concentration (MAC) in drinking water. The method was applied to determine phenolic compounds in Ebro river water however no phenols were found within the detection limits of the method.
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  • 38
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Extraction-determination ; Basic drugs ; Blood
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A new method for the extraction of basic drugs from whole blood based on the use of a buffered protein precipitating reagent at pH9, to form NiWO4 in biological fluids and a ternary organic extracting phase of density below 1 is proposed. The extract is analysed by high performance liquid chromatography using a Hypersil C8 column and detection at 230 nm; the mobile phases used consist of binary mixtures of acetonitrile and aqueous solutions containing 20 mmol/l ofn-propylamine at pH 5 andn-hexylamine at pH 4, as blockers of the free silanol groups. The proposed method was applied to the determination of 16 basic drugs including narcotics, analgesics, cocaine-related compounds and adulterants, as well as 8 benzodiazepines, in whole blood.
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  • 39
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 62-66 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Column switching ; Imidazolinone herbicides in soil ; Imazethapyr ; Imazapyr
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A column-switching method using two separation columns combined with UV detection at 260 or 236 nm has been used to determine the imidazolinone herbicides imazethapyr and imazapyr in soils. The residues were extracted from the soil with 0.1 M aqueous sodium carbonate solution and, after adjusting the pH to 2.0, the solution was partitioned with dichloromethane. Limits of determination for imazethapyr and imazapyr were 3 μg/kg. Recoveries were from 55 to 75% for both imidazolinone herbicides in the range 3–100 μg/kg in soil.
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  • 40
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 246-248 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Mercury ; Diphenylethynylmercury
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A new procedure for derivatisation of inorganic mercury(II) to diphenylethynylmercury with simultaneous extraction into dichloromethane is proposed. The organomercury derivative is effectively analysed by HPLC using UV detection. The calibration curve is linear over three orders of magnitude (0.02–50 mg L−1 Hg); the detection limit is 0.1 ng Hg. A preliminary study of the effect of potential interfering agents, in particular Cu(II), Zn(II), Cd(II), Pb(II), and cysteine, and applications of the present methodology to real environmental samples are presented.
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  • 41
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Ion exclusion ; Alipathic acids ; Silage effluents
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Short chain aliphatic acids are important components of the dissolved organic matter in silage effluents. Although ion exclusion chromatography offers some advantages for the analysis of these compounds, no attempt has yet been made to prove the suitability of this method for silage effluent analysis. In order to gain experience in this field, the separation characteristics of a Dionex ion exclusion column (IonPac-ICE As5) have been evaluated, the separation conditions have been improved, and several sample clean-up methods have been checked. Ten effluents generated during silaging of five different crops were collected from Bavarian farms and analyzed. Lactic and acetic acids were the predominant aliphatic acids. Pyruvic, formic, propionic, and succinic acid were detected in all samples, whereas glyceric and iso-citric acid were found in a few samples only. If some restrictions of substance specificity and separation efficiency can be accepted, the analytical method presented will be a reliable tool for the analysis of carboxylic acids in silage effluents.
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  • 42
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 38 (1994), S. 756-760 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Polymer encapsulated packings ; Poly(ethylstyrene-divinylbenzene) ; Preparation and evaluation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A series of polymer-encapsulated packing materials for reversed phase high-performance liquid chromatography was prepared by radical polymerization of ethylstyrene and divinylbenzene with vinyl-modified silica in solution. Some characteristics such as polymer structure, swelling propensity, residual silanols, column efficiency and retention properties were evaluated. Such material is easy to pack and yields high column efficiencies. Its superior performance for the separation of mixtures of aromatic hydrocarbons, amino- and hydroxyl group containing compounds are demonstrated by several examples.
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  • 43
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; β-Cyclodextrin in mobile phase ; Estrogens ; Pregnant and non-pregnant women
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A procedure is described for simultaneous determination of estriol, estrone and 17β-estradiol in human urine. After acid hydrolysis of the sulphate conjugates, the estrogens were extracted into diethyl ether. The ether extracts were concentrated and applied directly to an HPLC column. Using a 25 cm C-18 column and acetonitrile-water modified by the addition of β-cyclodextrin as mobile phase, the separation of estriol, estradiol and estrone was achieved within 20 minutes. The extraction of estrogens from the biological matrix is excellent. Estrogens were detected using a UV-detector (280 nm) or a spectrofluorimetric detector (λexc=280nm, λem=312 nm). The latter detection system has been used for the determination of estrogens in the urine of non-pregnant women. The procedure is simple and can be used in clinical practice.
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  • 44
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 38 (1994), S. 158-162 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Reversed-phase chromatography ; Retention mechanism ; Retention convergence ; Small molecules
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary It is shown theoretically that when the concentration of organic solvent in the mobile phase increases, or solute size decreases, log k′ values of small solutes in reversed-phase liquid chromatography (RPLC) will tend to have a minimum value called the convergence point. A theoretical model for evaluating the convergent coordinates of small solutes is presented by using a stoichiometric displacement model for retention (SMDR). The physical meaning of the coordinates of each kind of convergence are also elucidated. The convergence points have either two-dimensional coordinates with a common ordinate (the logarithm of the phase ratio of the column, log φ) or threedimensional corrdinates with two common axes: — log φ and the logarithm of the molar concentration of the pure displacing agent in mobile phase, log aD. The other axis relates to the nature of the solutes, such as carbon number of a homolog, van der Waal's surface area, hydrophobic fragment constant etc. for the latter and those and/or concentration axis for the former. The model was tested with published data and found to give a good fit.
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  • 45
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 38 (1994), S. 283-290 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Chemically bonded phase (CBP) ; Silica-gel with aminopropylsilyl ligands ; Physico-chemical characterization ; CP/MAS NMR investigation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Aminopropyl chemically bonded phases for high performance liquid chromatography (HPLC) have been prepared using mono- and trifunctional methoxyor ethoxysilanes. Three types of silica gel with different surface characteristics were used as support for the chemically bonded phases (CBPs). Surface characteristics of the packings before and after chemical modification were determined by porosity parameters, elemental analysis and CP/MAS NMR spectroscopy.29Si and13C CP/MAS NMR investigations gave informations about different interactions between aminosilyl ligands and/or these ligands and/or water molecules condensed in the pores of the silica gel surface. With decreasing pore diameter of the silica gel the proportion of protonated aminopropyl ligand increases.
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  • 46
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 38 (1994), S. 313-316 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Open-tubular capillary columns ; ‘Z’-shaped UV cells ; Solvent make-up
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary ‘Z’-shaped UV cells for packed capillary columns cannot be used in open-tubular capillary column liquid chromatography (OT-LC) because of their relatively large volume. With post-column solvent make-up, a commercial ‘Z’-shaped cell (volume 100 nl) was used in our OT-LC system, resulting in 9-fold sensitivity increase against on-column UV detection and with little efficiency loss. A small volume (5 nl) ‘Z’-shaped cell allows the direct coupling of the cell to high efficiency columns. For dilute samples, 9-19-fold sensitivity enhancement could be obtained. However, column efficiency decreases with increasing signal level as a result of peak deformation.
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  • 47
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Cyclosporin ; Reversible conversion ; Activation energy
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Reversed-phase liquid chromatography of cyclosporin A, a peptide immunosuppressant, at various temperatures produced remarkably different chromatograms. At 60°C one sharp peak was obtained, at 23°C this became a single broad peak and between 15° and 0°C this became one high sharp peak followed by a tailing or low plateau. Remarkably different chromatograms were produced also by varying the mobile phase flow-rate. The effects of both temperature and flow-rate on the chromatogram could be accounted for by interconversion between two forms of the cyclosporin molecule. Kinetic analysis showed that one form was converted by first-order kinetics with a half-life of 2.0 min at 20°C and that the apparent activation energy for the conversion was about 18 kcal/mol. The other two immunosuppressants, cyclosporin C and D, were also shown to undergo interconversion. This kinetic analysis of the interconversion should be helpful in clarifying the relationship between molecular structure and activity of the immunosuppressants.
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  • 48
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 38 (1994), S. 395-399 
    ISSN: 1612-1112
    Schlagwort(e): Supercritical fluid extraction ; Column liquid chromatography ; Carbendazime analysis ; Vegetable samples
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An SFE-HPLC method for the determination of carbendazime in lettuce leaves is described. The method involves a prior lyophilization of the sample and subsequent extraction with supercritical carbon dioxide containing methanol. The extraction conditions are as follows: amount of lyophilized sample, 1 g; CO2 density, 0.75 g/ml; temperature, 50 °C; flow-rate, 1.8 ml/min; dynamic extraction time, 25 min. Carbendazime is determined with an octadecylsilane column, an acetonitrile/water 30∶70 mobile phase and fluorescence detection at 285/317 nm. Carbendazime recoveries from spiked samples were all close to 100%. A comparison with the results from a conventional method for the determination of carbendazime reveals the new method to be more rapid, simple and reproducible for samples with low concentrations of analyte.
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  • 49
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 38 (1994), S. 421-430 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Pumps ; Flow control
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The measurement of flow constancy and pulsation amplitudes of HPLC pump based on the photoconversion of malachite green leucocyanide is described. The irradiation time and hence the degree of conversion of the leucocyanide is correlated to flow fluctuations of piston driven HPLC pumps. It is possible to measure the amplitude of pulsations and determine the constancy of the flow rate. Most of the pumps show a flow stability better than ±1% measured as relative standard deviation of the flow rate under HPLC conditions (pressure drop 100 bar at 1 ml/min flow rate). The most expensive pump of those tested showed less than ±0.5% flow instability, however, this result was achieved by installation of a large-volume pulsation damper. The method described also allows flow rate measurements under FIA conditions where there is little or no pressure drop at the pump outlet.
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  • 50
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 29-34 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Calcium modified silica ; Calcium adsorption isotherms
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The modification of silica surfaces by calcium ions has been studied by high-performance liquid chromatography. After treatment at pH 7.0 and 9.0 with calcium hydroxide, the modified silicas were characterised by physical and chemical analysis. From measurements by atomic absorption, the amount of calcium adsorbed was 650 ppm on silica modified at pH 7.0, and 4800 ppm on silica modified at pH 9.0. The amount of calcium on the modified silica was 0.574 groups nm−2 at pH 9.0 (original silica: mean pore diameter 176 Å, specific surface 279 m2 g−1, pore volume 1.23 ml g−1, mean particle size 9.8 μm). On the other hand, the amount of calcium in the original silica was 58 ppm. The separation factor, α for N-methylaniline and N,N-dimethylaniline was 5.2 on silica modified at pH 9.0, but could not be measured on silica modified at pH 7.0 and the original silica, using iso-propyl alcohol—n-hexane (0.5∶99.5) eluent.
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  • 51
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Sample preconcentration ; Solid-phase extraction ; Solvent focussing ; Injection techniques
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A new dual injector solvent focussing and elution technique developed for high-performance liquid chromatography (HPLC) greatly improves chromatographic efficiency for the on-line analysis of C18 solid-phase extraction (SPE) cartridges. Solutions containing three benzene homologs were used to characterize the dual injector analysis technique and to compare the chromatographic efficiency of this method with conventional SPE analysis methods. Sampling was performed off-line using a glass precolumn cartridge (3 mm i.d. × 30 mm) packed with 15–35 μm C18 silica. On-line cartridge analysis was achieved with two injection valves in either serial or parallel configuration. The injection loop of the first valve contains the eluting solvent, and the cartridge holder is connected in place of the injection loop of the second valve. When an injection is made, both valves are turned to the inject position, and the solvent plug is forced through the cartridge, focussing the analyte at the solvent front as it elutes the cartridge. Solvent focussing at the head of the column, resulting from preconditioning of the column with a small plug of water during injection, further minimizes the variance of the injection plug and improves the chromatographic efficiency. The technique has potential applications to environmental and biological fluid analysis where analyte preconcentration and resolution from the sample matrix components may be difficult with current SPE methods.
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  • 52
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 85-90 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Solid phase extraction ; Carbopack B ; Free sphingosine in human plasma
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A rapid, sensitive and selective high-performance liquid chromatographic method has been developed for the determination of sphingosine in human serum. After precipitation with methanol, the samples were extracted using Carbopack B disposable columns; the sphingosine was eluted with 0.05 M hydrochloric acid in methanol-dichloromethane (20∶80, v/v) and the extract evaporated to dryness at 40°C. The sample residue was then reconstituted with methanol and reacted with o-phthaldialdehyde reagent to produce a fluorescent compound. Separation was performed using an LC-18 column with 0.05 M phosphate buffer (pH 7)-methanol-acetonitrile (15∶80∶5, v/v) as mobile phase. Fluorescence detection was performed with excitation and emission wavelengths of 340 and 455 nm, respectively. The serum extract was re-analyzed with a cyano LC column to minimize the possibility of false positive results. The possible interference of compounds having a structure similar to that of sphingosine was evaluated. The mean recovery of sphingosine was 〉94.5%. The limit of detection of the assay was 1 ng mL−1. The between-run and within-run coefficients of variation for replicate analyses were 〈4.0% and 〈3.4%, respectively. The levels of free sphingosine in the serum of 40 normal subjects (20 male and 20 female) was investigated; the average level was 81.6±41.1 ng mL−1 (mean ±S.D.) for males and 85.5±33.7 ng mL−1 for females.
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  • 53
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Atmospheric pressure chemical ionization-mass spectrometry ; Dried yeast ; Thiamine ; Ion-pair extraction
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary High-performance liquid chromatography (HPLC) and high-performance liquid chromatography/atmospheric pressure chemical ionization-mass spectrometry (HPLC/APCI-MS) have been applied to the analysis of thiamine in dried yeast. Thiamine was extracted from dried yeast with isobutanol containing sodium 1-octanesulfonate as an ion-pairing agent and determined by HPLC on a reversed phase ODS column with UV detection at 254 nm. Response was linear in the range 25–300 μg/g of thiamine in dried yeast with a coefficient of variation in the reproducibility of 8.0%. Thiamine was recovered in good yield (109.2%, n=5). Identification of the thiamine peak was obtained by the mass spectrum using the HPLC/APCI-MS system. The utility of the selected ion monitoring technique using the HPLC/APCI-MS was also investigated. The results obtained by this method are in good agreement with those obtained by the thiochrome method [1].
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  • 54
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 107-109 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Drug assay ; Chlorpropamide ; Tolbutamide ; Human plasma
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Samples were extracted with dichloromethane and the organic layer evaporated to dryness. The residue was dissolved in methanol, and 10 μl aliquot injected onto the column. Tolbutamide was used as the internal standard for chlorpropamide. The UV detector response was linear over the range 0–200 μg ml−1 with a correlation coefficient of 0.999; detection limit: 0.002 μg ml−1. Within-day and between-day assay variation was generally ≤7%. No interference from endogenous constituents was observed. The utility of the method was demonstrated by determining chlorpropamide in samples from six healthy volunteers following a single oral dose of 250 mg. The procedure is simple and requires small volumes of plasma.
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  • 55
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Chemically bonded phases ; Non-silica based supports ; Hydrosilation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A process for bonding a monolayer of silane to the surface of alumina, zirconia, thoria and titania by reaction with the hydrolysis product of triethoxysilane is described. The hydride containing material is then further reacted with a terminal olefin in the presence of a platinum catalyst to produce a chemically modified oxide surface which could be used as a chromatographic stationary phase. The success of this reaction is monitored by diffuse reflectance infrared Fourier transform and cross-polarization magic-angle spinning nuclear magnetic resonance spectroscopy as well as by differential scanning calorimetry. On all four oxides both the hydride intermediate and the alkyl bonded product are successfully formed via the silanization/hydrosilation reaction sequence.
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  • 56
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Continuous beds ; Compressed beds ; Proteins
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Continous chromatographic beds are synthesized by a simple and cost-effective procedure which does not involve the conventional, time-consuming preparation of beads. The aim of this study was to improve the flow properties of the beds by investigating how they are affected by polymerization temperature, the pH of the buffer in which the polymerization takes place, the nature of the constituents of this buffer, the concentrations of catalyst and accelerator and the concentration of the precipitating agent (ammonium sulfate). The infuence of flow rate and the time constants of the detector and recorder on peak width was also studied.
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  • 57
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Monomeric and oligomeric RP packings ; Preparation of RP stationary phases ; Polycyclic aromatic hydrocarbons
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The preparation of C18 stationary phases for the separation of polycyclic aromatic hydrocarbons has been investigated. The effect of the pore size of the silica, the endcapping procedure, the amount of reagent and the amount of water in the preparation was also examined. A good correlation between surface coverage and capacity factor was found. The maximum surface coverage available with our preparation method lies between 3–3.5 μmol m−2, slightly depending on the pore size of the silica. Oligomeric not endcapped C18 packing materials are optimal for the separation of polycyclic aromatic hydrocarbons.
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  • 58
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 743-746 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Phenolic compounds ; Green pepper berries
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An HPLC method is described for the separation and estimation of phenolic compounds in six commercial varieties of green pepper berries. Among these, two phenolic compounds namely 3,4-dihydroxyphenylethanol glucoside and 3,4-dihydroxy-6-(N-ethyl amino)benzamide that served as efficient substrates for pepper phenolase, showed wide qualitative and quantitative variation in their composition within the varieties. Quantitative estimations of these two compounds were carried out using 4-methylcatechol and epinephrine as external standards. This method is suitable for the estimation of phenolic compounds in green pepper berries in one run.
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  • 59
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 138-145 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Diode array detection ; Post-column photochemical derivatisation ; Hair dyes
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A reversed phase liquid chromatographic method is proposed for the analysis of basic hair dyes (raw materials and colourant formulations). The performance of the method was enhanced by introducing post-column on-line photochemical derivatisation in combination with a Diode Array Detector. On-line photoderivatisation provided an effective way of selectively transforming the analytes to compounds with different spectral properties. For each analyte two characteristic UV-Visible spectra (photoreactor on and off) were obtained with the same mobile phase and this information in combination with the chromatographic data (k' at pH 3.0 and 4.5) enabled the unambiguous identification of both commonly used, approved, and banned basic hair dyes. Additionally, this approach was found useful to improve the method sensitivity, allowing the determination of analytes present in low concentration (0.03%) in complex commercial formulations.
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  • 60
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Copoly(styrene/ethyl methacrylate) ; Gradient elution ; Precipitation chromatography of polymers ; Solubility of polymers
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Copolymers from styrene and ethyl methacrylate have been separated according to composition byn-heptane gradients on a C18 bonded phase after injection into acetonitrile and subsequent sudden transition to a concentration of either dichloromethane or tetrahydrofuran between 30 and 50% or 20 and 50%, respectively. Acetonitrile is a polar non-solvent for the copolymers under investigation and ensures proper retention of the samples on a non-polar stationary phase. Dichloromethane and tetrahydrofuran are good solvents of moderate polarity. The addition of, e.g., 30 vol% of one of these solvents increased the dissolution power of the starting eluent but not to the extent necessary for elution. The latter was achieved by the addition ofn-heptane, which is a non-solvent for the polymers investigated. Thus, its eluting power must be understood as the consequence of its modifying effect on the polarity of the eluent mixture. The higher the content of copolymer in ethyl methacrylate the earlier it was eluted. Since acetonitrile andn-heptane are only partly miscible, phase diagrams were measured after the addition of either tetrahydrofuran or dichloromethane as a third component. Homogeneous mixtures were obtained on addition of about 30% solvent (one of both of the latter).
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  • 61
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Membrane-extraction disks ; On-line trace enrichment ; Polar pollutants ; Surface water
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An on-line trace-enrichment system, using a bifunctional membrane extraction-disk cartridge, has been combined with a column liquid chromatography separation for the simultaneous determination of basic, neutral and acidic pollutants in surface water. The enrichment device consisted of a specially constructed holder containing both C-18 and cation-exchange disks. The holder can contain up to 25 disks of 0.5 mm thickness and 4.6 mm diameter. Before trace enrichment of 20 ml of surface water (pH 3.0), calcium ions were removed from the sample by means of an oxalic acid precipitation. Desorption of the cartridge was at elevated temperature using reversed-phase gradient elution; detection was performed with a diode-array UV absorbance detector. The detection limits for the test compounds in surface water are typically 0.5–2 μg/l; the calibration graphs are linear from the lower limit of determination up to 50 μg/l.
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  • 62
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 285-293 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Fluorinated chemically bonded silica ; Aromatic compounds ; Molecular shape vs. retention
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Fluorinated bonded silica has been evaluated as a packing material in reversed-phase liquid chromatography (RPLC) with polycyclic aromatic hydrocarbons, chlorinated benzenes and substituted benzenes as sample probes. The bonded material is useful as a reversed-phase stationary phase and for polar compounds it offers a specific selectivity not found with octadecylsilica (ODS) phases. The phase also retains non-planar compounds more than planar molecules. The results can be explained by conformational differences between ODS and the fluorinated bonded phase by MM2 calculation.
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  • 63
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 346-354 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; α-Carotene cis-isomers ; β-Carotene cis-isomers ; Polymer stationary phase
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Various methanol-based, binary and ternary solvent systems were compared with respect to resolution of cis isomers of α and β-carotene by reversed-phase HPLC. A ternary system: acetonitrile-methanol-methylene chloride (75∶15∶10), or a binary system: acetonitrilemethanol (90∶10 or 5∶95) provided the best separation of β-carotene and its four cis isomers, 9-cis, 13-cis, 15-cis and 13,15-di-cis-β-carotene. The elution order of 9-cis and 13-cis-β-carotene was dependent on the methanol concentration. Methanol-methylene chloride (99∶1) resolved α-carotene and its three cis isomers, 9-cis, 13-cis, and 15-cis-α-carotene. It also proved the best for simultaneous separation of cis isomers of α and β-carotene. Sample solvent can affect the separation efficiency of each isomer. The presence of cis isomers of α and β-carotene in fresh and cooked carrots was also determined.
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  • 64
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 419-426 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Gas chromatography ; Chirasil-Val ; Amino acid enantiomers ; N-Isobutyryl-cysteine
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Free D-amino acids (D-AA) were detected as native constituents in juices of vegetables (cultivars of cabbage, tomato, carrot, garlic) and fruits (organes, clementine, grapefruit, lemon, apples, pear, grapes) using gas chromatography (GC) or high-performance liquid chromatography (LC). For investigation by GC, AA enantiomers were converted into theirN(O)-pentafluoropropionyl 2-propyl esters and resolved on a Chirasil-L-Val capillary column. For determination by LC, precolumn derivatization of AA enantiomers usingo-phthaldialdehyde together with the chiral thiolsN-isobutyryl-L-cysteine orN-isobutyryl-D-cysteine and fluorescence detection of the diastereomeric isoindole derivatives, resolvable on an octadecylsilyl stationary phase, were used. D-Ala (0.6–3.8%) was detected in all freshly pressed plant juices usually in the highest relative amounts. Other D-AA detected were D-Asx (0.1–1.9%), D-Glx (0–1.3%), D-Ser (0–1.7%), D-Arg (0.4–1.2%, in grapes, orange, grapefruit, and clementine) and D-Leu and D-Val (1% in cabbage). Absolute amounts of native D-AA were totally 28–57 μmol L−1 in fruit juices, 14.5 μmol L−1 in a tomato juice and 8.5 μmol L−1 in a carrot juice.
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  • 65
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 453-459 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Fullerenes ; Octadecylsilicas ; Temperature effect
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The effect of column temperature, especially at low temperatures, on the separation of fullerenes on monomeric and polymeric octadecyl silica (ODS) bonded phases has been studied. Decreasing the column temperature induces an increase in selectivity. The best temperature for the separation of fullerenes was determined for both types of ODS phase with n-hexane eluent. The selectivity for higher fullerenes on monomeric phases becomes similar to that on polymeric phases to low temperature. It has been found that as the carbon content of monomeric phases is increased, the selectivity also becomes similar to polymeric phases.
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  • 66
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Phenolic compounds ; Poplar bark ; Discosporium populeum infection ; Chemometric data evaluation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Reversed-phase high performance liquid chromatography with diode array detection was used to analyze phenolic compounds contained in bark extracts of two different poplar clones known to have different resistance toDiscosporium populeum infection. Statistical treatments both monovariate and multivariate were applied to the results in order to identify regularities useful to discriminate the polar resistance and to check the importance of seasonal and cultivation site related factors. For the two clones examined phenolic compounds showed great discrimination ability not influenced by either sample collection period or cultivation site.
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  • 67
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Micellar liquid chromatography ; Catecholamines in urine ; Coulometric detection
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The determination of catecholamines by HPLC with a sodium dodecyl-sulphate (SDS), micellar mobile phase on a C18 column and with coulometric detection was studied. The eluate was conditioned at +0.25 and +0.00 V, and the current at −0.16V was recorded. A previously developed model which describes the chromatographic behaviour of solutes in HPLC with hybrid, micellar mobile phases was used to optimize the SDS and ethanol concentrations. A mobile phase of 0.15M SDS in a phosphate buffer of pH 3.4 and without ethanol is recommended. The limits of detection were 0.4–0.7 ng ml−1. The procedure was applied to the determination of unconjugated L-dopa, norepinephrine and dopamine in urine. Direct injection of the urine samples gave high results but the unconjugated catecholamines could be determined with a single solid-phase extraction step on an alumina column.
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  • 68
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Micellar electrokinetic capillary electrophoresis ; Tetrahydrocarbazole derivatives ; β-Cyclodextrin ; Taurodeoxycholate
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary 2,3,4,6-tetra-O-acetyl-β-D-glucopranosyl isothiocyanate derivatives of a number of basic compounds, containing one chiral center, have been prepared. The indirect resolution of enantiomers was achieved with a high separation efficiency by capillary electrophoresis, using a sodium taurodeoxycholate/β-cyclodextrin system. This methodology was found to be superior to the resolution of the same derivatives by reversed phase HPLC analysis. A possible mechanism for stereoselectivity is described.
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  • 69
    ISSN: 1615-6102
    Schlagwort(e): α-Amylase ; (1-3, l-4)-β-Glucanase ; Hormones ; Monensin ; Transfection ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Summary A procedure has been developed to isolate protoplasts from mature aleurone layers of the malting variety Alexis and four other barley genotypes. It combines induction of endogenous cell wall degrading enzymes together with use of Onuzuka cellulase R 10 and driselase and results in better yields for two varieties than can be obtained with the huskless variety Himalaya. The viability of the freshly isolated protoplasts is greater than 90% and in spite of the presence of gibberellic acid during isolation procedures, most of the protoplasts are at an early developmental stage, as judged by ultrastructure. Gibberellic acid-induced changes in protoplast structure resemble those reported for Himalaya protoplasts. The protoplasts secrete both α-amylase (EC 3.2.1.1) and (1-3, 1-4)-β-glucanase (EC 3.2.1.73) into the surrounding medium. Transfection studies using a low pI α-amylase promoter to direct chloramphenicol acetyltransferase expression in aleurone protoplasts from Alexis and Himalaya revealed significant differences in their hormone responsiveness. In the absence of hormones, low levels of expression of the reporter enzyme were obtained in Alexis protoplasts, while high levels were characteristic for Himalaya protoplasts. An 8-fold increase in the expression of the reporter gene was induced by supplying the transfected Alexis protoplasts with gibberellin A3, whereas expression in Himalaya protoplasts remained unchanged. When Himalaya protoplasts were isolated from aleurone layers that had not been incubated with GA3 during the initial stages of protoplasting (the classical procedure), the hormone response of the promoter was 2.5-fold. It is thus possible to optimize the aleurone protoplast isolation procedure for different barley genotypes and mutants of interest in studies of transgenic gene expression and hormone induced secretion of proteins from this unique secretory plant tissue.
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  • 70
    Digitale Medien
    Digitale Medien
    Springer
    Protoplasma 180 (1994), S. 14-28 
    ISSN: 1615-6102
    Schlagwort(e): Golgi apparatus ; Dictyosome ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Summary Golgi apparatus (GA) of eukaryotic cells consist of one or more stacks of flattened saccules (cisternae) and an array of fenestrae and tubules continuous with the peripheral edges of the saccules. Golgi apparatus also are characterized by zones of exclusion that surround each stack and by an assortment of vesicles (or vesicle buds) associated with both the stacks and the peripheral tubules of the stack cisternae. Each stack (sometimes referred to as Golgi apparatus, Golgi complex, or dictyosome) is structurally and functionally polarized, reflecting its role as an intermediate between the endoplasmic reticulum, the cell surface, and the lysosomal system of the cell. There is probably only one GA per cell, and all stacks of the GA appear to function synchronously. All Golgi apparatus are involved in the generation and movement of product and membrane within the cell or to the cell exterior, and these functions are often reflected as structural changes across the stacks. For example, in plants, both product and membrane appear to maturate from the cis to the trans poles of the stacks in a sequential, or serial, manner. However, there is also strong ultrastructural evidence in plants for a parallel input to the stack saccules, probably through the peripheral tubules. The same modes of functioning probably also occur in animal GA; although here, the parallel mode of functioning almost surely predominates. In some cells at least, GA stacks give rise to tubular-vesicular structures that resemble the trans Golgi network. Rudimentary GA, consisting of tubular-vesicular networks, have been identified in fungi and may represent an early stage of GA evolution.
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  • 71
    Digitale Medien
    Digitale Medien
    Springer
    Protoplasma 180 (1994), S. 169-184 
    ISSN: 1615-6102
    Schlagwort(e): Actin ; Cell-cell communication ; Plasmodesmata ; Regulation ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Summary We have used several methods to localise actin associated with plasmodesmata. In meristematic plant material fixed in 0.1% glutaraldehyde/1% paraformaldehyde and embedded in LR White resin, actin was localised (in TEM using 5 nm gold-labelled secondary antibody to C4 anti-actin primary antibody) in the neck region by the plasma membrane and endoplasmic reticulum, and also down the length of the plasmodesma, deep in the cell wall. When the chemical fixation was replaced by rapid freezing in liquid propane (without cryoprotectants) and substitution in acetone, the plasmodesmata were labelled in similar positions, but with less background label on sections. While only 8–20% of plasmodesmata were labelled, the label was 10 to 100 fold denser over plasmodesmata than over the surrounding wall indicating specific association with plasmodesmata. We presume the apparent extracellular location of some label was due to the size of the antibodies between the site of attachment and the observed position of the gold particle. Gold label was found in similar locations in material fixed in 3% paraformaldehyde, infiltrated with sucrose, frozen, sectioned (10–12 μm thick), then labelled with antibodies before resin embedding. Furthermore, cell walls in epidermal peels stained with rhodamine-phalloidin showed localised patches of fluorescence, presumably at the site of plasmodesmata (or primary pit-fields), which were connected on either side to fluorescent strands of actin in the cytoplasm. Suspension cultured cells ofNicotiana plumbaginifolia similarly stained showed very faint, narrow fluorescent strands crossing the walls of sister cells, which may indicate actin associated with individual plasmodesmata, shown in TEM to be sparsely distributed in these walls. In addition, the neck regions of cytochalasin-treated plasmodesmata were greatly enlarged and lacked the normal extracellular ring of particles. We propose that actin associated with plasmodesmata stabilizes the neck region and possibly also the cytoplasmic sleeve, and may be actively involved in regulating cell-to-cell transport.
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  • 72
    Digitale Medien
    Digitale Medien
    Springer
    Protoplasma 181 (1994), S. 123-141 
    ISSN: 1615-6102
    Schlagwort(e): Carbohydrates ; Chytridiomycetes ; Extracellular material ; Membranes ; Ultrastructure ; Zoospores
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Summary In development of the primitive fungi, chytridiomycetes, unwalled zoospores bearing single, posterior flagella are transformed into walled, round-cells which elaborate the thallus. Production, structural modification, or release of extracellular material are involved with each transition of developmental stage. This article reviews the variety and developmental changes of extracellular materials found at the cell surface of chytridiomycetes. A cell coat, produced from Golgi-derived vesicles during zoosporogenesis, is visible around free swimming zoospores of some chytridiomycetes. How the zoospore surface receives and transduces signals is not widely explored, but it is known that fenestrated cisternae and simple cisternae, which are integrated into the microbody-lipid globule complex, are spatially and structurally associated with the plasma membrane and flagellar apparatus. This spatial association, as well as the cytochemical localization of calcium in fenestrated cisternae, suggest a mechanism for signal transduction and for regulation of zoospore motility. Zoospores become encased in a new layer of extracellular material as the zoospore encysts. Among some chytrids the source of this material is preexisting vesicles which fuse with the plasma membrane. Among other zoospores, a readily identifiable population of encystment vesicles is not apparent, demonstrating that there is no single pattern or mechanism for zoospore encystment in chytridiomycetes. Encysted zoospores developing into thalli, typically produce cell walls with a microfibrillar substructure. Ultrastructural analysis of walls reveals distinctive architecture and remarkable sculpturing which have been used in systematics of some members of chytridiomycetes. Nothing is known as to underlying controls of cytoskeletal elements and plasma membrane enzyme complexes in wall biogenesis. Many changes in cell surface structures accompany thallus maturation. Septa, many traversed with plasmodesmata, are produced in most chytrid thallus types. As sporangia and resting spores prepare for the production and release of zoospores, additional extracellular layers of material are frequently produced. Polarized deposits of extracellular material become discharge plugs, discharge vesicles, or endoopercula. Interstitial material is also released into cleavage furrows. Circumscissile or localized digestion of walls produce operculate or inoperculate exit ports for zoospore release. Cryofixation preserves more extensive extracellular material than does conventional chemical fixation, and broader application of cryofixation may radically alter our current view of cell surface structure. Thus chytridiomycetes exhibit a range in patterns for the occurrence and subsequent modifications of extracellular materials, even for members within the same order. The most universally recognized role for these extracellular materials is protection. Although there is a reasonable view of the types of extracellular material involved in chytridiomycete development, we have only limited understandings of their biogenesis or roles in regulation and communication, areas awaiting more investigations.
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  • 73
    ISSN: 1615-6102
    Schlagwort(e): Saprolegnia ; Lectins ; Concanavalin A ; Wheat germ agglutinin ; Monoclonal antibodies ; Ultrastructure ; Pathogenesis
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Summary The importance of the surface structure and chemistry in zoospores and cysts of oomycetes is briefly reviewed and the organelle systems associated with encystment described. The surface structure and chemistry of primary and secondary zoospores and cysts ofSaprolegnia diclina (a representative saprophytic species) andS. parasitica (a representative salmonid fish pathogen) were explored using the lectins concanavilin A (Con A) and wheat germ agglutinin (WGA) and monoclonal antibodies (MAbs) raised against a mixed zoospore and cyst suspension ofS. parasitica. The binding of lectins and antibodies to spores was determined using immunofluorescence microscopy with fluorescein isothiocyanate-labelled probes and with electron microscopy with gold-conjugated probes applied to spore suspensions post-fixation. In both species Con A, which is specific for glucose and mannose sugars, bound to both the surface of primary and secondary zoospores (the surface glycocalyx) and their cyst coats and readily induced zoospore encystment. The binding to the cysts appeared to be mainly associated with the matrix material released from the primary and secondary encystment vesicles and which appeared to diminish with time. No binding to germ tube walls was observed with this lectin. The MAb labelling showed a generally similar binding pattern to the primary and secondary cysts to that observed with Con A, although the binding to zoospores was more variable. Primary zoospores bound the antibodies but secondary zoospores appeared less reactive. It is suggested that the MAbs share a common epitope with one or more of the Con A-binding components. In both species WGA, which is specific for amongst other things the sugar N-acetyl glucosamine, bound to localised apical patches on the primary zoospores. This lectin also binds to the ventral groove region of secondary zoospores ofS. diclina, which were induced to encyst by this lectin. In contrast secondary zoospores ofS. parasitica were not induced to encyst by the addition of WGA and showed a patchy dorsal binding with this lectin. WGA also binds to both the inner wall of discharged primary cysts and the young germ tube walls of both species. These observations are discussed both in relation to other oomycete spores and to their possible functional and ecological significance.
    Materialart: Digitale Medien
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  • 74
    Digitale Medien
    Digitale Medien
    Springer
    Journal of plant research 107 (1994), S. 53-62 
    ISSN: 1618-0860
    Schlagwort(e): Coccolithophorid ; Cruciplacolithus neohelis ; Flagellar apparatus ; Haptophyceae ; Prymnesiophyceae ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract The flagellar apparatus ofCruciplacolithus neohelis (McIntyre and Bé) Reinhardt including its transition region is described. The transition region contains a hat-shaped structure, which is suggested to be one of the common features of the Prymnesiophyceae. Its flagellar root system resembles that of most coccolithophorids examined so far, except that only one vestigial crystalline root is present associated with root 1. Two well-developed crystalline roots associated with roots 1 and 2, respectively, appear in the preprophase of nuclear division, suggesting conversion to a mitotic spindle. The taxonomic and evolutionary significance of the flagellar apparatus is discussed.
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  • 75
    Digitale Medien
    Digitale Medien
    Springer
    Mycopathologia 125 (1994), S. 33-39 
    ISSN: 1573-0832
    Schlagwort(e): Aflatoxin ; Lymphocytes ; Mice ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract This investigation sought to determine whether splenic lymphocytes obtained from Balb/C mice exposed to aflatoxin B1 (AFB1) showed any ultrastructural changes which could account for the immunodysfunction attributable to aflatoxins. Lymphocytes obtained from Balb/C mice administered aflatoxin B1 in olive oil daily for three weeks were studied using both transmission and scanning electron microscopy. The lymphocytes demonstrated ultrastructural changes primarily in the mitochondria where marked internal dissociation of the cristae was revealed by transmission electron microscopy. All other cellular organelles were unaffected. No significant alterations in external structure were observed under scanning electron microscopy. The findings of this study indicate that AFB1 administration does not affect the surface topography of lymphocytes, but AFB1, by causing extensive mitochondrial damage, may affect the way in which these cells function. This could be a possible explanation for the immunodysfunction associated with AFB1.
    Materialart: Digitale Medien
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  • 76
    Digitale Medien
    Digitale Medien
    Springer
    Methods in cell science 16 (1994), S. 109-115 
    ISSN: 1573-0603
    Schlagwort(e): Animal model ; Neurofibroma ; Schwann cell ; Ultrastructure
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Summary Peripheral nerve sheath (PNS) neoplasms, primarily neurofibromas, schwannomas and maliganant schwannomas, are among the most common tumors in fishes. Model systems involving PNS tumors in fishes are also valuable because mammalian models of PNS tumors are rare. Schwann cells, the primary cell type suspected of neoplastic transformation in these tumors, have been difficult to culture. We describe techniques for culturing normal and neoplastic Schwann cells from fish. We also present methods for preparing cells on culture dishes for electron microscopy which are especially useful when specific cells in a culture must be located for ultrastructural examination.
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  • 77
    Digitale Medien
    Digitale Medien
    Springer
    Hydrobiologia 292-293 (1994), S. 137-142 
    ISSN: 1573-5117
    Schlagwort(e): Ultrastructure ; morphology ; integument ; copepoda ; crustacea
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie
    Notizen: Abstract The integument of Parathalestris harpactoides (Claus, 1863) is studied by scanning and transmission electron microscopy. The general structure of the integument conforms to the common pattern known from Copepoda. Emphasis is given to the structural variation of the cuticle in different regions of the body. The cuticle measures about 6 µm in most parts of the body, and shows a laminate appearance. The epicuticle is about 60 nm thick. Numerous pore canals containing muscular tonofilaments penetrate the procuticular layer of the integument. A peculiar feature is the presence of a ‘honeycombed’ layer in the outermost zone of the cuticle of some parts of the body. The epidermal layer, muscle insertions and integumental pores are of common type. The cuticle of some specimens, both males and females, is covered with microorganisms.
    Materialart: Digitale Medien
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  • 78
    Digitale Medien
    Digitale Medien
    Springer
    Journal of comparative physiology 164 (1994), S. 76-80 
    ISSN: 1432-136X
    Schlagwort(e): Insect antennae ; Pheromones ; Second messenger ; Phosphorylation ; Moth,Heliothis virescens
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract Protein kinase C inhibitors, such a calphostin C, abolish the transient nature of pheromone-induced rapid inositol 1,4,5-triphosphate (IP3) responses, suggesting that pheromone signalling is terminated by phosphorylation of specific proteins. Challenging antennal preparations fromHeliothis virescens with species-specific pheromones in the presence of [32P]-γ-ATP led to a rapid, stimulus-dependent incorporation of32Pi into antennal proteins. Pheromone-induced phosphorylation was completely abolished by a blockade of protein kinase C. Electrophoretic analysis revealed that upon stimulation with a pheromone blend two polypeptide bands were labelled; stimulation solely with the major compound (Z-11-hexadecenal) resulted in only a single labelled band. The data indicate that pheromones cause phosphorylation of specific antennal proteins which may be receptors for pheromones.
    Materialart: Digitale Medien
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  • 79
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Carbohydrates ; Post-column fluorescence derivatization ; Post column catalytic reaction
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A method for the determination of reducing sugars such as fructose and glucose and nonreducing sugar such as sucrose by high performance liquid chromatography followed by an acidic hydrolysis and a derivatization with benzamidine has been developed. After separation of sugars on a gel column packed with a polymer-based cation exchange material (Sugar-Pak I, Waters-Millipore), the sucrose is first hydrolysed in a solid phase reactor to convert it into reducing subunits. A post-column fluorigenic reaction with benzamidine under alkaline condition allows the selective determination of both natural and converted reducing carbohydrates. This procedure has proven to be selective (fluorigenic detection) and highly sensitive (allowing detection as little as picomoles amounts), reproducible and linear over a broad range of concentrations: 5×10−4 to 1.0×10−2 M. The applicability of this method to natural matrices such as plant extracts and beverages is also described. The sugar content of a barley extract has been determined and compared with a specific enzymatic test. The determined sugar content of natural and commercial lemon juices as well as of Cola beverages has been compared with those found by the conventional LC refractive index analytical procedure. In all cases, the results were comparable and were within the experimental errors of the methods.
    Materialart: Digitale Medien
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  • 80
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Thin-layer chromatography ; Densitometry ; Spectrophotometry of extracts ; Esculin, fraxin
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Coumarin glucosides, esculin and fraxin, were determined in several older and younger layers of stems ofAesculus hippocastanum L. by three methods (TLC-densitometry, TLC-extraction and spectrophotometric determinations, HPLC) during the vegetative period (May–October). Variation of their content during these months is discussed.
    Materialart: Digitale Medien
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  • 81
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 38 (1994), S. 88-92 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Phenylurea herbicides ; Milk
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A method has been developed for the determination of thirteen phenylurea herbicide residues in milk. It involves one-step solvent extraction of the milk with methanol by ultrasonication. The extract is cleaned up on an Amberchrom resin cartridge. Reversed-phase, gradient elution, high-performance liquid chromatography with UV detection at 242 nm is used to analyse the residues. The recovery of thirteen phenylurea pesticides is quantitative, ranging from 71.4% to 97.9% for the individual herbicides investigated at concentrations around 0.05 mg kg−1 and from 65.1% to 95.6% around 0.005 mg kg−1. The method is not associated with any of the emulsion problems common to conventional solvent extraction, which considerably reduce the sample clean-up process compared with existing methods.
    Materialart: Digitale Medien
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  • 82
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Lipid class analysis ; Experimental design and optimization ; Chemometrics
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A general method for the analysis of lipid classes by liquid chromatography has been developed using a multivariate optimization strategy to target optimal system conditions. The method was validated using a ruggedness test in the form of a Plackett-Burman design thereby exploring the immediate region around the optimum to ensure stable analytical conditions. Detection and quantitation were optimized by a factorial design in the light scattering detector parameters thus ensuring maximum detector response. This method was found to be suitable for a broad range of lipid sources from vegetable and animal origin, examples of the separation achieved are given for oat kernel, soybean and bovine milk lipids.
    Materialart: Digitale Medien
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  • 83
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Micellar liquid chromatography ; Determination of catecholamines ; Aminochromes ; Thermal lens spectrometry
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The determination of catecholamines (CAs) using micellar liquid chromatography with thermal lens spectrophotometric detection has been studied. CAs are oxidized with hexacyanoferrate(III) to aminochromes which are separated with a mobile phase of 0.05 M sodium dodecyl sulphate, 7% propanol and 0.03 M citrate buffer, pH 4.8, on a partially endcapped C18 column. The aminochrome-micelles and aminochrome-stationary phase association constants are evaluated. Using the 488 nm line of an Ar+ laser with 250 mW pump power the limits of detection are about 4 ng mL−1. The technique is applied to the determination of unconjugated CAs in urine using isoproterenol as internal standard.
    Materialart: Digitale Medien
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  • 84
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Copoly(styrene/ethyl methacrylate) ; Gradient elution, sudden transition ; Precipitation chromatography of polymers ; Solubility of polymers
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Copolymers from styrene and ethyl methacrylate have been separated according to composition by methanol gradients on a cyanopropyl column after injection inton-heptane and a subsequent rapid increase of dichloromethane (DCM) concentration from zero to a constant value in the range from 10 to 40%. Retention and resolution in sudden-transition gradients increased with decreasing DCM concentration. The gradient rate was varied between 2.5 and 7.5%/min with optimum resolution at 2.5% min. At a level of 20% DCM and a gradient rate of 5%/min, the separation of a mixture of five copolymers in a sudden-transition gradient was the same as with the corresponding common gradient, i.e., with injection into a mixture ofn-heptane and 20% DCM. Elution was also achieved at a level of 20% DCM by continuous addition of tetrahydrofuran (THF) instead of methanol. With THF, the peaks appeared later than with methanol in spite of the fact that methanol is a non-solvent and THF a good solvent for the polymers investigated. This indicates that elution was, in the first instance, caused by the polarity of the eluent. The elution characteristics of the copolymers in the system heptane/methanol at constant DCM concentration were basically similar to the already known characteristics iniso-octane/methanol at constant THF concentrations.
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  • 85
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Ligand exchange ; Amino acid enantiomers ; DL-aspartic acid ; Pseudomonas dacunhae
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The separation of the D and L enantiomers of eighteen essential α amino acids has been investigated by ligand-exchange chromatography (LEC). The effect of column temperature on the retention times and resolution of individual amino acid enantiomers has been studied by varying the temperature from 25 to 50 °C for a mobile phase containing Cu2+ ions. By use of a temperature of 50 °C and Zn2+ in the mobile phase, eight of the eighteen amino acid enantiomers can be resolved sufficiently well for practical application. Only phenylalamine, tyrosine, and tryptophan can be separated by use of Ni2+ as complexation metal at 50 °C. LEC has been used to monitor the decarboxylation of racemic DL-aspartic acid byPseudomonas dacunhae. Analysis of DL amino acid enantiomers in different media was performed at column temperatures of 30 and 50°C by addition of 0.125 mM Cu2+ to the aqueous mobile phase. It was found that the analytical performance is most dependent on the identity of the metal used for complexation; the concentration of the metal was of secondary importance and the column temperature less important still.
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  • 86
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 67-70 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Reversed phase systems ; Ternary eluents ; Mono-substituted aromatics ; Retention and selectivity
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The variation in selectivity for aromatic hydrocarbons with mono-substituted polar groups is investigated in ternary mobile-phase systems on C18 stationary phases. The dependence of log k′ on the proportions of two modifiers was determined for the solutes within the concentration range of ternary systems obtained by mixing two binary eluents: methanol + water and tetrahydrofuran + water or acetonitrile + water and tetrahydrofuran + water. The nature of the relationships is explained in terms of molecular shape, molecular interactions between solute and extracted modifier and the ordering of solvated ligands on the stationary phase.
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  • 87
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Column switching ; HIV type 1 reverse transcriptase inhibitor ; Acquired immune deficiency syndrome ; L-697, 661
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A method for the determination of L-697, 661, a human immunodeficiency virus type 1 reverse transcriptase inhibitor, and its 6-hydroxy metabolite in plasma is described. Following analyte isolation via solid phase extraction, samples are analyzed by HPLC using a column switching system. Column switching allows each analyte to be simultaneously analyzed under isocratic reverse phase conditions in a run time of 21 minutes. The assay was linear in the concentration range of 10–500 ng/mL for each analyte when 1 mL aliquots of plasma were extracted. The assay has been fully validated and utilized for human pharmacokinetic studies.
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  • 88
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 663-667 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Polystyrene ; Ethyl acetate ; Dichloromethane
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The reversed phase behaviour of high molecular mass polystyrenes was investigated on C18 bonded phase columns with ethyl acetate-methanol and ethyl acetateacetonitrile mobile phases. The results are compared with the corresponding dichloromethane mobile phases. The ethyl acetate-methanol mobile phase showed anomalous elution behaviour, similar to other previously investigated solvent combinations with methanol. The ethyl acetate-acetonitrile mobile phase showed no anomalous behaviour, increased retention and, elution over a wider composition range compared with the dichloromethane-acetonitrile system. However, resolution between adjacent molecular masses was considerably worse.
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  • 89
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; LC/MS coupling ; Particle Beam interface ; Plasma and urine samples ; BN50730 and its metabolites
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A simple and sensitive assay has been developed for the quantitative measurement of a new platelet activating factor antagonist (BN50730), and its two main metabolites (BN50727 and BN50922), at the picomole level in human plasma and urine. The three compounds of interest and the internal standard (BN50765) were measured by combined LC-negative chemical ionization MS. A simple solid-liquid extraction procedure was used to isolate the parent drug and the two metabolites. The MS was tuned to monitor the intense ionm/z 333 generated in the ion source by a dissociative capture process. The assay was on 1 ml plasma or 0.1 ml urine and the quantitation limit was calculated as 1 ng·ml−1. The very low relative standard deviations and mean percentages of error calculated for within-day or between-day repeatability assays demonstrate the ruggedness of the technique for routine determination in biological fluids. Some preliminary results on the pharmacokinetics of the parent drug and its two main metabolites illustrate the applicability of this method.
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  • 90
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 279-284 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Capillary columns for LC ; Micro-gradient generation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The generation of a micro-gradient for micro HPLC capillary columns is described. The system used is a modified and improved version of a split flow gradient elution device. Gradient tests have been performed and have shown good reproducibility under all conditions. The system has been successfully coupled with a particle beam LC-MS interface and the analysis of a mixture of twenty seven basic or neutral pesticides is reported.
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  • 91
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 409-418 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Ion-exchange chromatography ; Protein purification ; Pentosan polysulfate displacers ; Dextran sulfate displacers
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Experimental studies were carried out to investigate the utility of pentosan polysulfate as a low molecular weight polyelectrolyte displacer for the purification of proteins in anion-exchange displacement systems. In addition, the influence of mobile phase salt concentration on displacer efficacy, protein-protein resolution, and displacement development were studied for several anionic displacers. It was found that while large polyelectrolytes (50 kd dextran sulfate) were efficient displacers for a wide range of salt concentrations, relatively small polyelectrolytes (3 kd pentosan polysulfate) were seen to act as an efficient displacer only under conditions of high salt micro-environments. In addition, for proteins exhibiting similar affinities, zone mixing at the protein-protein boundary was found to be quite sensitive to the salt concentration. Finally, displacement chromatography was successfully implemented for the separation of proteins from milk whey.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 92
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Mycotoxins ; Chlamydosporol epimers ; Solvent optimisation ; Fusarium species
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Two epimers of the mycotoxin chlamydosporol were separated by HPLC on an RP-18 column using a quaternary mobile phase consisting of water (79.1%), methanol (10.0%), acetonitrile (10.4%) and tetrahydrofuran (0.5%), with a flow rate of 1 ml min−1. This optimal composition of mobile phase, with which the resolution value for the two epimers (1 and2) was 2.73 with retention times of 5.88 and 7.12 min, respectively, was achieved by the application of Philips Solvent Optimisation Software PU 6100. The presence of free silanols on the stationary phase was shown to be an essential requirement for the separation of the chlamydosporol epimers.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 93
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Precolumn derivatization ; Dansylhydrazine ; Fluorescence detection ; Tacrolimus (FK 506) in blood
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A sensitive and selective liquid chromatographic method, using precolumn derivatization with dansylhydrazine followed by fluorescence detection, has been developed for the determination of tacrolimus (FK 506) in whole blood. After haemolysis, whole blood samples are extracted with diethyl ether and derivatized. After on-line removal of excess dansylhydrazine on a C18 precolumn, the derivative is loaded on to a C18 clean-up column, and a heart cut is subsequently transferred to a graphitized carbon column, where the final separation takes place. The method requires 1 ml of sample and has a limit of quantitation of 3 ng/ml. At the 15 ng/ml level the precision isca 10%, and the response is linear from the limit of quantitation toca 200 ng/ml of FK 506 in whole blood. The capacity of the method is 50 samples/day and about 1000 1-ml samples can be analyzed without changing either clean-up or separation column. Finally, the applicability of the method for therapeutic drug monitoring is shown.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 94
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 520-528 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; New bonded phases ; 13C and29Si CP-MAS NMR ; DRIFT ; ESCA
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A variety of olefins were bonded to silaceous supports through a hydride modified substrate. The products were then examined by13C and29Si solid state-NMR with cross-polarization (CP) and magic angle spinning (MAS). Information about the surface was also obtained by diffuse reflectance infrared Fourier transform spectroscopy (DRIFT) and the related photoelectron spectroscopic technique (ESCA). Carbon analysis on bonded silicas was carried out and surface coverage was calculated. Confirmation of the organic groups bound to the silica support was possible. The hydride intermediate is shown to be a versatile material for bonding a wide variety of organic moieties to silica surfaces.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 95
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 39 (1994), S. 577-580 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography-mass spectrometry ; Column liquid chromatography ; Cholesteryl acetate ; Hydroperoxide formation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Gas chromatographic, high performance liquid chromatographic and GC-ion trap detector mass spectrometric analyses of the hydroperoxides formed during thermal peroxidation of cholesteryl acetate, are reported and discussed. The hydroperoxides were separated from the thermal-oxidised mixture by solid-phase extraction, fractionated and individually collected by HPLC. Each hydroperoxide was then chemically reduced with NaBH4 to a hydroxy-derivative. The GC and MS characteristics of hydroxy- and TMS-derivatives were compared against available standards. Only 7β-hydroperoxide and 7α-hydro-peroxide of cholesteryl acetate were found, as reported in the literature for cholesterol.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 96
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Ion-exchange-induced stationary phase ; Retention behavior ; Aromatic hydrocarbons
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The retention behavior of aromatic hydrocarbons on anion-exchangers modified with alkylsulfate or alkanesulfonate has been examined by column liquid chromatography. Several parameters affected the retention of analytes, involving concentration of the modifier in the mobile phase, its alkyl chain length and mobile phase composition. Stationary phases modified with a reagent having longer alkyl chains achieved better column efficiency. The separation factor achieved on ion-exchange-induced stationary phases foro-terphenyl and triphenylene was larger than that on alkyl-bonded silica gel.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 97
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Gas chromatography ; Particle beam MS detection ; Polycyclic aromatic metabolites ; Biodegradation in water
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Two liquid chromatography-particle beam mass spectrometry (LC-PBMS) systems have been used for analysis of polycyclic aromatic hydrocarbon metabolites in water samples from a biological decomposition model experiment. The results were compared with those obtained by classical gas chromatography-mass spectrometry. Evaluation of spectral data indicated the presence of six main metabolites; 1H,3H-naphtho [1,8-cd]pyran-1,3-dione, 1-(hydroxymethyl)naphthalene, and 1,2-acenaphthenedione were identified by use of standard substances and spiking experiments. Enrichment of the investigated water samples with online pre-column (C18) concentration, freeze-drying, and solvent extraction led to similar results with only slight differences. The application of microbore separation columns proved to be a promising tool in particle beam LC-MS measurements.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 98
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Hydrophilic polymer-based packing material ; Direct injection of serum
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A size monodispersed restricted-access polymeric packing material has been prepared through a simple and easy one-step method of co-polymerization of glycerol monomethacrylate and glycerol dimethacrylate with cyclohexanol as prorogen. A typical seeded polymerization (two step swelling and polymerization method) in an aqueous medium gave a 90 % yield of porous beads which could be utilized as a packing material in high performance liquid chromatography (HPLC) without any size classification due to the excellent size monodispersity. A BET measurement and size exclusion chromatography in either tetrahydrofuran or water revealed that the prepared material had only small pores (around 100 Å in diameter). It showed ample hydrophobicity for the separation of hydrophilic drug molecules in 10% aqueous acetonitrile buffer, while polypeptides such as bovine serum albumin were excluded and eluted before the void volume of the column with quantitative recovery.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 99
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Nitro-PAHs ; Diesel particulate extract ; Column switching
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A multicolumn (MC) HPLC method for the determination of 1-nitropyrene (1-NP) at trace-levels via on-line reduction to 1-aminopyrene and fluorescence detection is presented. On the first column, packed with a pyrenebutyric acid amide stationary phase, the nitro-derivatives of PAHs are strongly retained and separated from other matrix components. The nitro-PAHs-containing fractions are transferred onto a RP18-column via stepwise gradient elution and finally separated according to their various lipophilicities and sizes. To increase the overall selectivity and sensitivity of the multidimensional method (MD-HPLC system) post-column, on-line reduction of the nitro-PAHs to the respective amino-PAHs via a short catalysis column is performed thus enhancing the sensitivity significantly (to low pg levels). The applicability of this method for the determination of trace amounts of 1-NP in real samples (diesel particulate extracts) is demonstrated.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 100
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Liquid crystal phases ; Molecular shape recognition ; Polycyclic aromatic hydrocarbons
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The chromatographic retention behaviour of two liquidcrystal bonded phases have been evaluated using polycyclic aromatic hydrocarbons (PAHs) as the probe samples in reversed-phase high performance liquid chromatography (RP-HPLC). The results clearly indicate that these phases have better planarity and shape recognition capabilities than commercially-avaialble polymeric octadecylsilica (ODS) phases whose strong planarity and shape selectivities were found earlier. It can also be concluded from the chromatographic observations that the shape recognition capability of these phases is dependent on both mobile phase composition and column temperature, but that the effect of mobile phase and temperature on the shape selectivity work independently. The retention behaviour can be explained by changes in the phase structure with changes of eluent composition and temperature.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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