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  • Chromatographie, Dünnschicht  (41)
  • Lysosomes
  • Springer  (56)
  • Cham :Springer International Publishing :
  • Frontiers Media SA
  • 2020-2024
  • 2020-2022
  • 1970-1974  (56)
  • 1974  (35)
  • 1973  (14)
  • 1971  (7)
Collection
Publisher
  • Springer  (56)
  • Cham :Springer International Publishing :
  • Frontiers Media SA
Years
  • 2020-2024
  • 2020-2022
  • 1970-1974  (56)
Year
  • 1
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    Springer
    Calcified tissue international 14 (1974), S. 153-160 
    ISSN: 1432-0827
    Keywords: Lysosomes ; Bone ; Resorption ; Osteoclast
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine , Physics
    Description / Table of Contents: Résumé Des techniques histochimiques de microscope photonique et électronique montrent que les ostéoclastes métaphysaires chez des rats “sans incisive” présentent des quantités plus importantes de phosphatase acide, d'acryl sulfatase et de trimétaphosphatase acide lysosomiales. L'activité en phosphatase lysosomiale à pH neutre est aussi plus élevée dans les ostéoclastes métaphysaires, sauf dans les cellules situées sous la métaphyse, où l'enzyme est absente. L'absence de résorption de la matrice organique semble en rapport avec l'absence de bordures en brosse et une absence d'enzyme lysosomiale extracellulaire. Malgré cette absence, une dissolution de cristaux inorganiques a été mise en évidence au microscope électronique, suggérant que la dissolution minérale est un processus distinct de la désintégration enzymatique de la matrice organique.
    Abstract: Zusammenfassung Histochemische Techniken für Licht- und Elektronenmikroskopie zeigten, daß metaphysäre Osteoklasten “Schneidezahl-loser” (SL) Ratten erhöhte Mengen von lysosomaler saurer Phosphatase, von Arylsulfatase und von saurer Trimetaphosphatase enthielten. Die Aktivität der lysosomalen Phosphatase bei neutralem pH war in den metaphysären Osteoklasten ebenfalls erhöht, außer in den Zellen direkt unterhalb der Wachstumsplatte, wo dieses Enzym nicht vorkam. Es konnte überhaupt keine Resorption der organischen Matrix festgestellt werden, was übereinzustimmen schien mit der Abwesenheit eines gekräuselten Saumes und einer gleichzeitigen Abwesenheit des extrazellulären lysosomalen Enzyms. Trotzdem wurde im Elektronenmikroskop das Verschwinden anorganischer Kristalle festgestellt, was darauf schließen läßt, daß die Auflösung des Minerals nicht derselbe Vorgang ist wie die enzymatische Auflösung der organischen Matrix.
    Notes: Abstract Histochemical techniques for light and electron microscopy showed that metaphyseal osteoclasts in “incisors absent” rats contained greater than normal amounts of lysosomal acid phosphatase, aryl sulfatase and acid trimetaphosphatase. Lysosomal phosphatase activity at neutral pH was also elevated in the metaphyseal osteoclasts except in those cells immediately beneath the growth plate, where this enzyme was absent. The failure of any discernable resorption of organic matrix appeared to correlate with the absence of a ruffled border and a concomittant absence of extracellular lysosomal enzyme. Despite this failure, electron microscopic evidence of inorganic crystal removal was noted, suggesting that mineral dissolution represents a separate process from the enzymatic breakdown of organic matrix.
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  • 2
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    Archives of microbiology 98 (1974), S. 115-126 
    ISSN: 1432-072X
    Keywords: Endocytosis ; Tetrahymena ; Lysosomes ; Exocytosis ; Acid Hydrolases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Endocytosis of yeast cells by Tetrahymena pyriformis GL for a period of 2.5 h produced changes in cellular acid hydrolases. Acid phosphatase, acid deoxyribonuclease and acid proteinase activities were markedly increased, whereas there was a decrease in acid ribonuclease activity and little change in α-glucosidase activity. These alterations do not appear to be due to any alteration in the rates of secretion of these enzymes into the milieu. Evidence is presented that the cellular enzyme increases found upon endocytosis of yeast reflect changes in lysosomal enzymes, because it was shown that the acid phosphatase activity increase resulted in an increased amount of latent enzyme within the cell. The results also support the idea that there are at least 3 distinct populations of lysosomes, in addition to phagolysosomes, present in Tetrahymena pyriformis GL, with different modes of formation. There appears to be a large excess of lysosomes, uncombined with phagosomes, present in these fed cells since latency averaged 66% in broken-cell preparations which contained very few intact phagolysosomes. The phagolysosomal acid phophatase activity cannot account for more than 34% of that present in the cell. The endocytosis of yeast in the presence of growth medium resulted in a marked drop in the rate of cell division as compared to cells growing in the growth medium alone. The results are discussed.
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  • 3
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    Cell & tissue research 112 (1971), S. 97-119 
    ISSN: 1432-0878
    Keywords: Insects ; Epicuticle secretion ; Golgi system ; Lysosomes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Description / Table of Contents: Résumé Les modifications cytologiques des cellules épidermiques sécrétant la cuticule sternale et pleurale de l'adulte deT. molitor sont étudiées pendant la formation et l'évolution de l'épicuticule externe et interne. L'épicuticule externe et interne sont sécrétées de la même façon par condensation de matériel diffus au-dessus de l'apex des microvillosités. Un cycle hétérolytique est mis en évidence par l'emploi de peroxydase injectée dans l'espace exuvial: la peroxydase est captée par de grosses vésicules revêtues et incorporée dans des corps multivésiculaires apicaux. Par comptage des différentes populations de vésicules, des variations nettes dans l'intensité de la pinocytose sont mises en évidence. Ces variations semblent en rapport non pas avec la digestion de l'ancienne cuticule mais avec les différences de nature et de structure des composants cuticulaires. L'hypothèse du contrôle de la sécrétion épidermique par les phénomènes de pinocytose énoncée par Locke (1969) est confirmée. Des vésicules d'origine golgiennes sont secrétées surtout après la formation de l'épicuticule et ne sont donc pas à l'origine du matériel épicuticulaire, mais il est possible qu'elles jouent un rôle dans l'évolution ultérieure des structures épicuticulaires.
    Notes: Summary The cytological modifications of the epidermal cells secreting sternal and pleural cuticle of adultTenebrio are studied, specially during the formation and evolution of the outer and inner epicuticle. Both layers are secreted by condensation of diffuse material just above the epidermal microvilli. There is no peculiar phase without microvilli when inner epicuticle is formed. During the secretion of pre-ecdysial cuticle, the epidermal cell is characterized by an heterolytic process which is demonstrated by peroxidase injection into the ecdysial space: horseradish peroxidase is absorbed by large pinocytic coated vesicles which discharge their content into multivesicular bodies, after the loss of their coat. The intensity of pinocytosis is studied by vesicles counts at different stages of the pupal life. These counts show a pinocytic peak when the inner epicuticle is formed. When the epicuticular barrier is completely secreted, exogenous peroxidase is no more absorbed, but morphological study and counts show that pinocytosis still occurs. This demonstrates that epidermis cannot absorb macromolecules arising from the digested old cuticle since digestion occurs after the completion of adult epicuticle. Locke's hypothesis about the “control of the extracellular subcuticular environment” by pinocytosis is confirmed. The Golgi complexes are involved in lytic process with their small coated vesicles and in secretion of cuticular material with their large dense secretory vesicles, but according to vesicle counts, the secretory vesicles are not concerned in epicuticle formation since their apparition is posterior to the deposition of the inner epicuticle.
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  • 4
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    Cell & tissue research 115 (1971), S. 524-542 
    ISSN: 1432-0878
    Keywords: Spleen ; Rat-Marginal sinus ; Reticuloendothelial system ; Lysosomes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary In the rat spleen cells are found staining with aldehyde fuchsin (AF-cells). Most of these cells are localized at the periphery of the follicles, at the inner border of the marginal sinus. They probably develop in situ. Comparable cells occur in other lymphoid organs. They are able to phagocytize, and resemble also histochemically red pulp macrophages. The aldehydefuchsinophilic granules do not stain for mucopolysaccharides. On the ultrastructural level the aldehydefuchsinophilic granules are represented by cytoplasmic bodies with a faintly granulated matrix. Because of their single membrane and the varying positive reaction on acid phosphatase these bodies are considered to be secondary lysosomes or residual bodies. They contain different materials of unknown endogenous origin. In non-immunized animals the AF-cells fail to show the characteristic dendritic protrusions and infoldings of antigen trapping cells. The cells possess some characteristics of reticular cells e.g. association with reticulin, and electron dense patches on the innerside of the cell membrane at the contact areas. They can be classified among the phagocytic reticular cells forming part of the metalophilic cells in the spleen.
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  • 5
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    Cell & tissue research 118 (1971), S. 283-296 
    ISSN: 1432-0878
    Keywords: Blood platelets ; Lysosomes ; Acid phosphatase ; Aggregation ; Cell fractionation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Description / Table of Contents: Zusammenfassung Aufgrund biophysikalischer, biochemischer und ultrastruktureller Eigenschaften lassen sich in intakten oder fraktionierten Blutplättchen von Mensch und Schwein verschiedene Funktionstypen von alpha-Granulomer unterscheiden. Ein elektronen dichter, oft Mikrotubuli aufweisender Typ ist durch Zentrifugation von einem helleren mit fibrillärer Streifung abzusetzen. Außerdem läßt sich eine Fraktion vesikulärer Strukturen darstellen. Bei biochemischer Analyse ist die Hauptmenge der lysosomalen Hydrolasen Cathepsin und beta-Glucuronidase mit dem weniger dichten Typ der alpha-Granula vergesellschaftet, während sich der Hauptteil der sauren Phosphatase in der Vesikelfraktion befindet. Zytotopochemisch erscheint dieses Enzym immer strukturgebunden, sowohl an beiden Typen von alpha-Granula, als auch in den Vesikeln. Das Vesikelsystem spielt bei der Stoffaufnahme in Plättchen eine Rolle und wird auch als gamma-Granulomer, surface connected system oder canaliculäres System bezeichnet. Bei der Degranulation der Plättchen wird — wie die Enzymlokalisation in diesem Falle zeigt — Granulainhalt über das vesikuläre System in das Außenmedium abgegeben. Saure Phosphatase kann auch in Phagozytosevakuolen nachgewiesen werden. Elektronenoptisch läßt sich der Übergang von alpha-Granula in vesikuläre Strukturen erkennen. Die Befunde zeigen, daß zwischen alpha-Granula und Vesikelsystem enge Beziehungen bestehen. Zusammen bilden sie eine funktionelle Einheit, die neben der Stoffaufnahme auch die Funktion der Abgabe von Substanzen aus den Plättchen erfüllt. Schließlich findet die Digestion aufgenommener Stoffe dort statt.
    Notes: Summary Biochemical and ultrastructural findings from intact and fractionated pig and human blood platelets indicate the presence of different types of alpha granules. An electron dense type can be distinguished from a lighter one with a fibrillar matrix. The major part of the lysosomal hydrolases beta-glucuronidase and cathepsin is associated with the lighter granules. Most of the acid phosphatase appears in the vesicle fraction. The ultracytochemical investigation shows the acid phosphatase bound to both types of granules or vesicles. This enzyme is visible in the narrow spaces between the outer membranes of aggregated thrombocytes. Furthermore, there can be seen the transformation of alpha granules into vesicles and vesicles, which contain acid phosphatase releasing their contents into the extracellular medium. Thus the significance of the vesicle system for the release of substances out of the platelet seems to be proved. From this point of view the different types could be considered as alpha granules in different functional stages.
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  • 6
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    Cell & tissue research 141 (1973), S. 529-544 
    ISSN: 1432-0878
    Keywords: Osteoclast ; Parathyroid hormone ; Lysosomes ; Bone resorption ; Electron microscopy ; Histochemistry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary Young rats were treated with high doses of parathyroid hormone (PTH). Osteoclasts from these animals revealed characteristic alterations in comparison to control cells: a) The cytoplasm contained large vacuoles with phagocytosed cells, some of which resembled osteoblasts or osteocytes. The vacuoles were interpreted as lysosomes because the engulfed cells often appeared partly digested and the vacuoles contained acid phosphatase as demonstrated histochemically, b) lipid droplets were present in the cytoplasm and usually located close to the endoplasmic reticulum and/or in regions with many free ribosomes, c) the Golgi complex was more frequently separated from the nuclei than in control cells, d) small coated cytoplasmic bodies were numerous in the peripheral cytoplasm, e) the membranes of the endoplasmic reticulum were fused in some places, f) cytoplasmic regions with numerous free ribosomes were frequent, g) large ring-shaped granules occurred in some mitochondria. Energy dispersive X-ray analysis of these granules provided evidence that they contained calcium and probably phosphorus, h) in some osteoclasts the mitochondria were enlarged. — The findings are consistent with an increased activity of osteoclasts and in particular a stimulation of the lysosomal system in these cells.
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  • 7
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    Cell & tissue research 155 (1974), S. 455-473 
    ISSN: 1432-0878
    Keywords: Lysosomes ; Liver ; Ageing ; Exocytosis ; Thorotrast ; Electron microscopy, Morphometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary Lysosomes in mouse liver parenchymal cells have been marked by intravenous injection of Thorotrast. They were subsequently followed in a time sequence from five hours up to sixteen weeks after injection. At two days after injection the majority of the lysosomes was heavily loaded with marker particles, while endocytosis was no longer observed. From six days after injection Thorotrast was partly accumulated in very large lysosomes (conglomerates) with mean diameters up to 2.5 μm. As the time after injection advanced the Thorotrast content of the cells was reduced while most of the remaining marker substance became concentrated in the conglomerates. Many Thorotrast conglomerates were shown to contain acid phosphatase and some of them were able to fuse with functionally younger lysosomes which were marked with colloidal gold. Morphometric analysis showed an increase in the volume density of the dense body population between 0 and 2 days after injection, followed by a decrease between 2 and 11 days. The observed decrease is probably caused by exocytosis of the contents of Thorotrast containing lysosomes in bile capillaries.
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  • 8
    ISSN: 1432-0878
    Keywords: Avian follicles ; Oocytes ; Transosomes ; Lysosomes ; Electron microscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary Electron microscopy has been utilized to determine fates of sacs of ribosomes (variously termed “transosomes”, “unique organelles”, or “lining bodies”) formed in the follicular cells of avian follicles and subsequently entering-or being taken in-by the oocytes. Small follicles (0.5 mm diameter) of laying hens, a hen afflicted with Marek's disease and prelaying pullets were examined in this regard. In the case of the hen with Marek's disease and the prelaying pullets, sacs of ribosomes were found to be present within the oocyte but those present in the interior of the cell were in the form of digestive vacuoles. In a fourth group of hens, receiving actinomycin D, larger oocytes (2.0 mm diameter) exhibited breakdown of the membranous vesicles in which the sacs of ribosomes entered the oocyte, as well as dissolution of membranes surrounding the forming yolk granules and the membranes of coated vesicles. Annulate lamellae were present in oocytes of the hen afflicted with Marek's disease and appeared within at least 24 hours in oocytes from hens receiving actinomycin D.
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  • 9
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    Cell & tissue research 143 (1973), S. 135-141 
    ISSN: 1432-0878
    Keywords: Branchiostoma ; Endothelial cells ; Endocytosis ; Lysosomes ; Cytochemistry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary The endothelial cell of Amphioxus has an endocytotic capability since both ferritin and horseradish peroxidase, when injected into the endostylar artery, became localized within endothelial cell cytoplasmic vesicles. The endothelial cells also contain vesicles within which the lysosomal enzyme acid phosphatase has been localized. Because of the presence of an endocytotic capability and lysosomes, these cells possess both the means and the method for the acquisition and disposal of exogenous proteins.
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  • 10
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    Cell & tissue research 112 (1971), S. 247-265 
    ISSN: 1432-0878
    Keywords: Parafollicular cells (C-cells) ; Secretory cycle ; Ca-Metabolism ; Lysosomes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Description / Table of Contents: Zusammenfassung Die parafollikulären Zellen der Rattenschilddrüse zeigen eine vom jeweiligen Funktionszustand abhängige Feinstruktur: 1. Zellen mit zahlreichen Granula, einem ausgeprägten Golgi-Apparat, gering entwickeltem granuliertem endoplasmatischem Retikulum und manchmal einigen dichten Körpern mit myelinähnlichen Figuren. 2. Zellen mit wenigen Granula und einem stark entwickelten endoplasmatischen Retikulum mit erweiterten Zisternen; diese Zellen können das Lumen des Follikels erreichen. 3. Einige degranulierte Zellen. — In den Schilddrüsen-Follikeln des Hundes konnten wir nur die ersten beiden Zellformen, aber keine degranulierten parafollikulären Zellen beobachten. Nach Ca++-Injektion findet man als Zeichen der Funktionsabhängigkeit der Feinstruktur eine Zunahme der Zellen mit stark entwickeltem endoplasmatischem Retikulum und nur geringer Granulation. Die dichten Körper mit myelinähnlichen Figuren zeigen saure Phosphataseaktivität. Es handelt sich deshalb wahrscheinlich um Restkörper, die aus Autolysosomen entstanden sind. Trotzdem zeigt sich nach Zufuhr von Ca++ und anschließender EDTA-Gabe keine eindeutige Zunahme der Lysosomenzahl. Zwischen follikulären und parafollikulären Zellen sind Axonanschnitte zu finden.
    Notes: Summary The parafollicular cells of the thyroid of the rat show different fine structures most likely in relation with different functional states: 1. Some cells contain numerous secretory granules, a well developed Golgi complex, a moderately developed rough endoplasmic reticulum and some dense bodies containing myelin figures. 2. Other parafollicular cells have few granules and a strongly developed rough endoplasmic reticulum with enlarged cisternes. They sometimes reach the lumen of the follicle. 3. Finally, a few parafollicular cells appear degranulated.—In dogs the degranulated parafollicular cells could not be observed. Following administration of Ca++ ions there is an increase of cells with strongly developed endoplasmic reticulum and only few granules. The dense bodies with myelin figures show acid phosphatase activity. Most likely they are residual bodies derived from autolysosomes. However, EDTA after stimulation of the cells by Ca++ does not significantly increase the number of parafollicular cells containing autolysosomes. Axons can be found between follicular and parafollicular cells.
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  • 11
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    Cell & tissue research 116 (1971), S. 464-476 
    ISSN: 1432-0878
    Keywords: Lung ; Alveolar macrophages ; Lysosomes ; Erythrophagocytosis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary Erythrophagoeytosis in vivo by cat alveolar macrophages was studied under the electron microscope by collecting the macrophages at 2 hours and 48 hours following the intratracheal injection of autologous blood. Considering the progressive ultrastructural modifications of the red blood cell plasma membrane, different successive stages were observed, corresponding to the hemolysis of the erythrocytes: 1. A recently engulfed erythrocyte appears unaltered within the phagocytic vacuole. 2. A dense layer, surrounding the plasma membrane of the red cell, is observed within the phagocytic vacuole. 3. The content of the vacuole is uniformly dense and the plasma membrane of the red cell exhibits discontinuous thickenings. 4. The whole vacuole appears very dense (hyperdense stage) and the plasma membrane is shown altered. The whole process of erythrophagocytosis is accompanied by an active fusion of the phagocytic vacuole with typical lysosomes and lysosomes containing crystal-like material. It is suggested that hemolysis may be explained in terms of enzymic digestion of the proteinic part of the plasma membrane of the erythrocyte.
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  • 12
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    Cell & tissue research 116 (1971), S. 477-486 
    ISSN: 1432-0878
    Keywords: Lung ; Alveolar macrophage ; Lysosomes ; Erythrophagocytosis ; Heinz bodies
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary The ultrastructural analysis of the in vivo erythrophagocytosis by cat alveolar macrophages demonstrates a sequence of two successive events. The first consists of the destruction of the red blood cell membrane (hemolysis). The second corresponds to digestion of hemoglobin. This process is observed as a progressive and uniform clearing of the content of the phagocytic vacuole. An active fusion of typical lysosomes and of lysosomes containing crystal-like masses with the phagocytic vacuole continues to occur. At the terminal period small dense ferritin-like granules appear within the dissolving hemoglobin. During this process the swollen fragmented erythrocyte membrane, sometimes simulating Heinz bodies, persists along with lysosomal crystal-like masses. A lamellar structure of the altered erythrocyte plasma membrane is seldom observed. A diagram summarizes the entire process of destruction of the red blood cell (hemolysis and digestion) as observed following its engulfment by a cat alveolar macrophage.
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  • 13
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    Cell & tissue research 120 (1971), S. 80-93 
    ISSN: 1432-0878
    Keywords: Tunicate ; Neural gland ; Hypophysial homologue ; Lysosomes ; Ultrastructure ; Phosphatase localization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary The cells comprising the neural gland in the ascidians Ciona, Styela, and Botryllus have been examined for their fine structural features and enzyme cytochemistry. The gland cells are either cuboidal or irregular in outline. They are full of small vesicles, of which some are pinocytotic, as well as larger vacuoles; they become increasingly vacuolated as their shape decreases in regularity. At the same time, glycogen deposits accumulate and the cisternae of the endoplasmic reticulum become distended. Some of the vacuoles contain an electron dense material or a fibrillar substance, but the cells contain no obvious electron opaque secretory granules associated with an extensive Golgi complex such as occur in the vertebrate adenohypophysis. Acid phosphatase is localized in some of the vesicles and vacuoles, indicating that they are a kind of lysosome, the latter possibly representing autophagic vacuoles. Thiamine pyrophosphatase is also found in many vacuoles as well as in the saccules of the Golgi apparatus which in these cells is in the form of dictyosomes. The results suggest a developmental cycle of increasing cytoplasmic vacuolation, ultimately leading to a breakdown and release of the vacuolar products. The significance of these observations is considered, particularly with respect to the hypothesis that the gland represents the ascidian equivalent of the vertebrate pituitary.
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  • 14
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    Fresenius' Zeitschrift für analytische Chemie 268 (1974), S. 102-108 
    ISSN: 1618-2650
    Keywords: Zinkstaubdestillation ; Ultramikrobereich, Apparatur, TAS-Verfahren. Thermofraktographie, TAS-Verfahren ; Chromatographie, Dünnschicht ; Zinkstaubdestillation, Ultramikrobereich. Analyse von Naphthalinderivaten, Anthracenderivaten, Phenanthrenderivaten, Tetracenderivaten, Indolderivaten ; Chromatographie, Dünnschicht ; Zinkstaubdestillation, TAS-Verfahren
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Es wird eine Methode beschrieben, die es erlaubt, unter kontrollierten Bedingungen mit 20–200 μg Ausgangsmaterial eine Zinkstaubdestillation durchzuführen. Hierzu wird die Probe auf Cu-aktiviertes Zink in einer TAS-Patrone für einige Minuten auf 350–450° C erhitzt. Die dabei entstehenden sauerstofffreien Aromaten bzw. stabilen Heterocyclen werden durch einen Stickstoffstrom von 15 ml/min direkt auf den Startpunkt einer DC-Schicht transferiert. Anschließend wird chromatographiert und die auftretenden Reaktionsprodukte werden identifiziert. Zum Studium der Reaktionsvorgänge und der optimalen Temperaturbereiche dient die Thermofraktographie. Es sind Anwendungsbeispiele aus der Gruppe der Naphthalin-,Anthracen-, Phenanthren-, Tetracen- und Indolderivate gegeben.
    Notes: Abstract A method for zinc dust distillation of 20–200 μg of substance under controlled conditions is described. The sample is heated on copper-activated zinc up to 350–450° C for several minutes in a TAS-cartridge. The resulting oxygen-free aromatic resp. the stable heterocyclic components are transferred directly to the starting point of a TLC-plate by a stream of nitrogen at 15 ml/min and identified after chromatography. Thermography is applied to study the reaction process and to determine the optimal temperature ranges. Examples of application to the groups of naphthalene-, anthracene-, phenanthrene-,tetracene- and indol derivatives are listed.
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  • 15
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    Fresenius' Zeitschrift für analytische Chemie 268 (1974), S. 126-127 
    ISSN: 1618-2650
    Keywords: Chromatographie, Dünnschicht ; Rückgewinnung geringer Substanzen
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
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  • 16
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    Fresenius' Zeitschrift für analytische Chemie 268 (1974), S. 119-123 
    ISSN: 1618-2650
    Keywords: Best. von 8-Hydroxychinolinderivaten, 8-Hydroxychinaldinderivaten in Pharmazeut. Produkten ; Chromatographie, Dünnschicht ; ÄDTA-behand. Platten
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Es wird eine Methode beschrieben, mit der 8-Hydroxychinolin- und 8-Hydroxychinaldin-Derivate nach erfolgter Entwicklung auf Kieselgelplatten direkt quantitativ mit einem Chromatogramm-Spektralphotometer bestimmt werden können. Durch Vorbehandlung der Platten mit Komplexbildnern, wie Äthylendiamintetraessigsäure, Diäthylentriaminpentaessigsäure oder Triäthylentetraminhexaessigsäure, wird im Gegensatz zur unbehandelten Platte erreicht, daß die Substanzen runde Flecken ausbilden, die zur quantitativen Bestimmung geeignet sind. Die Methode hat sich auch bei der Bestimmung der Wirkstoffe aus Arzneiformen, wie Dragees und Salben, bewährt und läßt sich mit einer maximalen relativen Standardabweichung von ± 3,4% gut reproduzieren.
    Notes: Abstract A method is described allowing direct quantitative determination of 8-hydroxyquinoline and 8-hydroxyquinaldine derivatives with a chromatogram spectrophotometer after development on silicagel plates. In contrast to untreated plates, pretreatment of the plates with complexing agents like ethylene-diamine-tetraacetic acid, diethylenetriamine-pentaacetic acid, or triethylenetetramine-hexaacetic acid, results in formation by the compounds of round areals which are suitable for quantitative measurement. This method proved also valuable for the quantitative measurement of the active contents of pharmaceutical formulations, like tablets or ointments. It is reproducible with a maximal relative standard deviation of ± 3.4%.
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  • 17
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    Fresenius' Zeitschrift für analytische Chemie 268 (1974), S. 124-126 
    ISSN: 1618-2650
    Keywords: Trenn. von Pesticiden, phosphorhaltig ; Chromatographie, Dünnschicht ; Schicht aus bas. Zinkcarbonat
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Dünnschichten von basischem Zinkcarbonat eignen sich zur Trennung von Insecticiden aus der Gruppe der Organophosphorsäuren. Mit Petroläther/Aceton-Gemischen zwischen 98∶2–86∶14 werden günstige Rf-Werte und gute Fleckzeichnungen erreicht. Die Substanzen sind entweder im kurzwelligen UV-Licht zu erkennen, wenn man der Dünnschicht Fluorescenz-Indicator F 254 der Fa. Merck zusetzt, oder aber im Tageslicht nach Sprühen mit Pd(II)Cl2-Lösung, wobei rotbraune Flecken entstehen. Die Wirkstoffe lassen sich mit Aceton quantitativ eluieren; Die Trennung kann auch säulen-chromatographisch durchgeführt werden. Die Trenneffekte sind ähnlich denjenigen, wie sie auf Kieselgel erreicht werden. Das basische Zinkcarbonat hat aber den Vorteil geringerer chemischer Aktivität, so daß weniger Artefakte entstehen.
    Notes: Abstract Thin layers of basic zinc carbonate can be used with good results to separate organophosphorous pesticides. With a petroleumether/acetone mixture (between 98∶2 and 86∶14) good Rf-values and clearly defined spots are obtained. The substances are either recognizable in short-wave UV-light, when the fluorescence indicator F 254 from Fa. Merck is added to the thin layer, or in day-light, after having been sprayed with a solution of Pd(II)Cl2, which leads to the formation of reddish-brown spots. The pesticides can be eluted quantitatively with acetone; the separation can also be carried out by means of column chromatography. The effects of separation are similar to those obtained on silica gel, but basic zinc carbonate has the advantage of lower chemical activity, which means that less artifacts are formed.
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    Fresenius' Zeitschrift für analytische Chemie 269 (1974), S. 125-126 
    ISSN: 1618-2650
    Keywords: Nachw. von Xylenolen, Dimethylphenolen ; Chromatographie, Dünnschicht ; versch. Schichten u. Reagentien
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
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  • 19
    ISSN: 1618-2650
    Keywords: Nachw. von Kresolen, Phenol ; Chromatographie, Dünnschicht ; versch. Schichten und Reagentien
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    Cell & tissue research 137 (1973), S. 125-140 
    ISSN: 1432-0878
    Keywords: Vital staining ; Phenothiazine dyes ; Purification of dyes ; Lysosomes ; Metachromasia
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Description / Table of Contents: Zusammenfassung Zellkulturen wurden vergleichend mit Handelsfarbstoffen und gereinigten Farbstoffen aus der Phenothiazingruppe (Thionin und seine methylierten Homologe — Azurfarbstoffe — bis zum Methylenblau vitalgefärbt. „Granuläre Farbstoffspeicherung“ wird erst dann beobachtet, wenn im zweifach aminosubstituierten Phenothiazin (Thionin) mindestens zwei Methylgruppen gegen Protonen an den Aminogruppen ausgetauscht worden sind, wie dies bei Azur A der Fall ist. Dieser Befund läßt sich nur bei Verwendung gereinigter Farbstoffe erheben. Die hier verwendeten Handelsfarbstoffe „Azur C“ sind in solchem Ausmaß mit höher methylierten Homologen vermischt, daß deren Effekt eine Eignung des Azur C zur granulären Farbstoffspeicherung vortäuscht. Gereinigtes Azur C ist dazu jedoch ungeeignet. Phasenoptisch erscheint die mit Azur A, Azur B und Methylenblau erreichte Farbstoffspeicherung mehr vakuolär als granulär. Die vom jeweils verwendeten Farbstoff induzierten vakuolären Einschlüsse zeigen morphologische Eigenheiten. Die Befunde werden diskutiert, unter besonderer Berücksichtigung der mit den kationischen Farbstoffen vermutlich reagierenden anionischen zellulären Bestandteilen.
    Notes: Summary In a comparative study cells grown in monolayer have been vitally stained with commercial dye samples and dyes purified by thin layer chromatography and column chromatography. The dyes used were derivatives of amino-substituted phenothiazine (thionine to methylene blue). “Granular storage of dyes” has been observed only after the protons of the amino groups had at least been substituted by two methyl groups, as represented by the compound azure A. This observation is based on the use of purified dyes. Commercial samples of “azure C” are mixed with fractions of the higher methylated homologues of thionine to a degree that these impurities imply suitability of azure C for intracytoplasmic granular storage. Purified azure C, however, does not induce formation of cytoplasmic vacuoles. In the phase contrast microscope, inclusions formed under the influence of azure A, azure B and methylene blue exhibit a more vacuolar than granular appearance. There are morphologic differences, between vacuoles formed under the influence of the respective dyes. The observations are discussed with special regard to the anionic cellular constituents supposed to react with the cationic dyes.
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    Cell & tissue research 147 (1974), S. 219-235 
    ISSN: 1432-0878
    Keywords: Lysosomes ; Mouse fibroblasts ; Dye treatment ; Cell culture ; Electron microscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary Mouse fibroblasts were grown in a ‘deficient’ medium consisting solely of Hank's salt solution. Treatment of cells after 48 hours in deficient medium with the cationic dye, mepacrine, resulted in an altered formation of lysosomes. Cells grown in full medium form dense, multi-vesiculated lysosomes in response to mepacrine. Cells grown in deficient medium form large electron lucent vacuoles containing peripherally located dense globules. The significance of the observations in relation to the deficiency of the medium is discussed.
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    Fresenius' Zeitschrift für analytische Chemie 268 (1974), S. 203-205 
    ISSN: 1618-2650
    Keywords: Strukturaufklärung von Sesquiterpenalkoholen ; TAS-Verfahren, Mikrodehydrierung ; Chromatographie, Dünnschicht ; bicyclisch, mit Decalin-Grundgerüst
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Aus dem ätherischen Öl der Haselwurz wurden erstmalig die 4 Sesquiterpenalkohole α-Eudesmol, β-Eudesmol, Selinan-7,11-diol und Selin-6(7)en-11-ol isoliert und identifiziert. Dabei wurde zur Einengung der Strukturmöglichkeiten die dehydrierende TAS-Methode (Schwefel-Dehydrierung) eingesetzt. Sie lieferte bei ungesättigten C15-Alkoholen gute Ergebnisse. Gesättigte Sesquiterpenalkohole mit Decalin-Grundgerüst ließen sich besser nach der Selenmethode dehydrieren. Von den entstandenen Naphthalin-Derivaten wurden die UV-Spektren direkt von der DC-Platte aufgenommen und zur Identifizierung herangezogen. Durch diese Kombination der Mikroverfahren konnte das Grundgerüst der Alkohole mit Mikrogramm-Mengen eindeutig bestimmt werden.
    Notes: Abstract In the essential oil of Asarum europaeum L. the four sesquiterpene alcohols α-eudesmol, β-eudesmol, selinane-7,11-diol and seline-6(7)en-11-ol have been isolated and identified. For limiting the possibilities of structure the dehydrogenating TAS method (sulphur dehydrogenation) has been employed. Good results have been obtained with unsaturated C15-alcohols. Saturated sesquiterpene alcohols with decalin structure could be better dehydrogenated by the selenium method. UV spectra have been recorded of the naphthalene derivatives formed directly from the thin-layer plate and employed for identification. By this combination of micro methods the basic structure of the alcohols could be determined unequivocally with μg amounts.
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    Fresenius' Zeitschrift für analytische Chemie 268 (1974), S. 337-342 
    ISSN: 1618-2650
    Keywords: Analyse der Metallchelate von o,o′-Dihydroxyazoverbindungen ; Chromatographie, Dünnschicht
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung In einer früheren Veröffentlichung [4] ist auf die Möglichkeit der chromatographischen Trennung strukturisomerer Metallchelate hingewiesen worden; sie soll hier ausführlicher dargestellt werden. Weiterhin wird die Trennung von 1:2-Mischkomplexen von Azofarbstoffen und von 1:2-Metallkomplex-Mischungen durch Dünnschicht-Chromatographie (DC) an Polyamid beschrieben. Unter bestimmten Voraussetzungen kann durch DC an Kieselgel zwischen 1:2-Metallkomplexfarbstoffen mit Sulfonsäureamid- bzw. Alkylsulfongruppen und solchen ohne diese Substituenten unterschieden werden. Die beschriebenen DC-Methoden ermöglichen bei richtiger Interpretation eine eindeutige Unterscheidung zwischen strukturisomeren Metallkomplexen der 1:1- und 1:2-Reihe, sowie Mischkomplexen und Komplexmischungen vom 1:2-Metall-chelattyp unsulfierter o,o′-Dihydroxyazoverbindungen. Symmetrische o,o′-Dihydroxyazoverbindungen, wie z.B. das 2,2′-Dihydroxy-5,5′-dimethyl-azobenzol(7), sind geeignete Komplexbildner für Schwermetallkationen, um diese als farbige Chelate mit Hilfe der DC voneinander zu trennen. Strukturisomere sind wegen der Molekülsymmetrie ausgeschlossen, so daß die Ergebnisse eindeutig sind.
    Notes: Abstract In an earlier publication [4] the possibility of the Chromatographic separation of structurally isomeric metal chelates was mentioned; this is dealt with here in more detail. Further the separation of 1:2 mixed complexes from azo dyes and 1:2 metal-complex mixtures by thin-layer chromatography (TLC) on polyamide is described. In certain circumstances it is possible to distinguish between 1:2 metal-complex dyes with sulphonamide or alkylsulphonyl groups and those without these substituents by TLC on silica gel. The TCL methods described allow-when correctly interpreted-an unambiguous distinction between structurally isomeric metal complexes of the 1:1 and 1:2 series, and mixed complexes and mixtures of complexes of the 1:2 metal-chelate type of unsulphonated o,o′-dihydroxyazo compounds. Symmetrical o,o′-dihydroxyazo compounds, such as 2,2′-dihydroxy-5,5′-dimethylazobenzene(7), are suitable as complex-formers for heavy-metal ions, allowing the separation of the latter as their coloured chelates with aid of TLC. Structural isomers are excluded because of the molecular symmetry, so that the results are unambiguous.
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    Fresenius' Zeitschrift für analytische Chemie 269 (1974), S. 10-15 
    ISSN: 1618-2650
    Keywords: Chromatographie, Dünnschicht ; Vergleich von Zweistrahldensitometern
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Zur Eliminierung von Störungen der quantitativen Auswertung von Dünnschicht-Chromatogrammen durch Unregelmäßigkeiten der Sorptionsschicht werden öfters Zweistrahlgeräte verwendet. Diese Arbeit berichtet über die Simulation verschiedener Zweistrahlgeräte auf einem Einstrahlgerät mit Hilfe von Digitalrechnern, um auf diesem Wege eindeutige Aussagen über den Genauigkeitsgewinn treffen zu können. Die relativen genäherten Standardabweichungen aus einer größeren Anzahl von Messungen ergaben folgende Werte: Einstrahlgerät 3–5%, Zweistrahlgerät 2–4% und Zweiwellenlängengerät 2,5–4%.
    Notes: Abstract To avoid errors caused by irregularities of chromatoplates in quantitative TLC often double beam densitometers are used. This paper describes the simulation of different double beam instruments using a single beam scanner and digital computers, to obtain distinct data on the increase in accuracy. The relative standard deviations from a greater number of experiments are: single beam scanner 3–5%, double beam instrument 2–4% and dual wave-length scanner 2.5–4%.
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  • 25
    ISSN: 1618-2650
    Keywords: Best. von Toluidinen ; Chromatographie, Dünnschicht ; diazidodisulfostilbenimprägnierte Schichten
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    Fresenius' Zeitschrift für analytische Chemie 271 (1974), S. 177-181 
    ISSN: 1618-2650
    Keywords: Untersuchung der Autoxidation von Fettsäureestern ; Chromatographie, Dünnschicht
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Mittels Dünnschicht-Chromatographie kann man den Ablauf von Autoxidationsprozessen an Lipiden qualitativ anhand der auftretenden Reaktionsprodukte verfolgen. In vorliegender Arbeit wurden verschiedene Laufmittel auf Silicagel hinsichtlich ihres Trennvermögens für Gruppen von Autoxidations-produkten erprobt. Ferner werden aufgrund umfangreicher Untersuchungen Sprühmittel zur Erkennung solcher Stoffgruppen auf dem Dünnschicht-Chromatogramm benannt. Am Beispiel der Autoxidation von c-9-Octadecensäuremethylester ohne und mit Zusatz von DDE wird die Leistungsfähigkeit der beschriebenen Arbeitsweise belegt.
    Notes: Abstract The autoxidation of lipids has been followed qualitatively by means of the reaction products. The separating ability of different solvents on silica gel for groups of autoxidation products has been tested. Furthermore, spraying agents for the detection of these groups on the chromatogram are given. The autoxidation of c-9-octadecenic methyl ester with and without addition of DDE serves as an example for the efficiency of the method.
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    Fresenius' Zeitschrift für analytische Chemie 271 (1974), S. 257-264 
    ISSN: 1618-2650
    Keywords: Schwefeldehydrierung, Selendehydrierung ; Ultramikrobereich, Apparatur, TAS-Verfahren. Thermofraktographie/TAS-Verfahren/Chromatographie, Dünnschicht ; Schwefel- und Selendehydrierung, Ultramikrobereich. Analyse von Sesquiterpenderivaten, Abietinsäure. Steroiden ; Chromatographie, Dünnschicht ; Schwefel- und Selendehydrierung, TAS-Verfahren
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Es wird eine Schnellmethode beschrieben, die es erlaubt, unter kontrollierten Bedingungen mit 50–300 μg Ausgangsmaterial eine gekoppelte Dehydratisierung und Schwefel- bzw. Selendehydrierung durchzuführen. Hierbei wird die Probe mit einer Kaliumhydrogensulfat-Schwefel- bzw. Selenmischung für einige Minuten bei vorbestimmten Temperaturen zwischen 160–400° C im TAS-Ofen bzw. Tasomat erhitzt. Die entstehenden Aromaten werden durch einen Stickstoffstrom von 10 ml/min direkt auf den Startpunkt einer DC-Schicht transferiert. Anschließend wird chromatographiert und die auftretenden Reaktionsprodukte werden identifiziert. Zum Studium der Reaktionsvorgänge und der optimalen Temperaturbereiche dient die Thermofraktographie. Es sind Anwendungsbeispiele aus der Sesquiterpen-, Diterpen- und aus der Steroidreihe gegeben.
    Notes: Abstract A rapid method is described which permits to carry out a coupled dehydratization and sulphur resp. selenium dehydrogenation with 50–300 μg of starting material under controlled conditions. The sample is heated on a potassium hydrogen sulphate-sulphur resp. selenium mixture at preselected temperatures of between 160–400° C for several minutes in the TAS-oven resp. the Tasomat. The resulting aromatic components are transferred directly to the starting point of a TLC-plate by a stream of nitrogen at 10 ml/min and the reaction products are identified after chromatography. Thermofractography is applied to study the reaction processes and to determine the optical temperature ranges. Examples of application to the groups of sesquiterpenes, diterpenes and steroids are listed.
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    Fresenius' Zeitschrift für analytische Chemie 271 (1974), S. 285-286 
    ISSN: 1618-2650
    Keywords: Nachw. von Canthaxanthin in Biolog. Material ; Chromatographie, Dünnschicht ; Fertigfolien UV 254
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  • 29
    ISSN: 1618-2650
    Keywords: Best. von Kresolen, Phenol, Xylenolen, Dimethylphenolen ; Chromatographie, Dünnschicht ; imprägn. Fertigfolien u. Kieselgel, Nachweisgrenzen
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    Fresenius' Zeitschrift für analytische Chemie 271 (1974), S. 337-340 
    ISSN: 1618-2650
    Keywords: Abtrenn. des 2,4-Dinitrophenylhydrazons von Formaldehyd, Acetaldehyd, Acrolein, Crotonaldehyd, Furfurol ; Chromatographie, Dünnschicht
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Es wird ein dünnschicht-chromatographisches Verfahren zur Trennung von Formaldehyd, Acetaldehyd, Furfurol, Acrolein und Crotonaldehyd in Form der 2,4-Dinitrophenylhydrazone beschrieben. Die Derivate werden aus Pyridin, Tetrahydrofuran oder Dioxan aufgetragen und innerhalb von 6 h nach der Durchlauftechnik an Kieselgel F 254-Rapidplatten mit Tetrachlorkohlenstoff/Pyridin (90∶10) aufsteigend entwickelt. Die Laufstrecken verhalten sich wie 1∶1,3∶1,7∶2,1∶2,3.
    Notes: Abstract The derivatives are applied on rapid plates silica gel F 254 from pyridine, tetrahydrofuran or dioxan solution and separated during 6 h by ascending overrun development using carbon tetrachloride/pyridine (90∶10) as a solvent. The distances travelled from the starting point are in the ratio 1∶1.3∶1.7∶2.1∶2.3.
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    Fresenius' Zeitschrift für analytische Chemie 271 (1974), S. 365-366 
    ISSN: 1618-2650
    Keywords: Turigeran, Multivitaminpräparate ; Chromatographie, Dünnschicht ; Fertigfolien
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    Fresenius' Zeitschrift für analytische Chemie 271 (1974), S. 367-368 
    ISSN: 1618-2650
    Keywords: Uran(VI) ; Chromatographie, Dünnschicht ; DEAE-Cellulose, Phosphorsäure
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    Fresenius' Zeitschrift für analytische Chemie 272 (1974), S. 206-206 
    ISSN: 1618-2650
    Keywords: Nachw. von Diphenyl ; Chromatographie, Dünnschicht ; verschiedene Reagentien u. Schichten
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    Fresenius' Zeitschrift für analytische Chemie 272 (1974), S. 286-286 
    ISSN: 1618-2650
    Keywords: Nachweis von Herbiciden, Pesticiden ; Chromatographie, Dünnschicht ; Fertigfolien, Nachweisgrenzen
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    Fresenius' Zeitschrift für analytische Chemie 272 (1974), S. 368-368 
    ISSN: 1618-2650
    Keywords: Best. von DDT in Eiern ; Chromatographie, Dünnschicht
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    Fresenius' Zeitschrift für analytische Chemie 268 (1974), S. 128-128 
    ISSN: 1618-2650
    Keywords: Nachw. von Alkoholen als Co-Xanthate ; Chromatographie, Dünnschicht
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    Fresenius' Zeitschrift für analytische Chemie 268 (1974), S. 272-274 
    ISSN: 1618-2650
    Keywords: Best. von Gramicidin ; Chromatographie, Dünnschicht ; CAMAG Eluchrom
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    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Eine quantitative Methode zur Bestimmung von Gramicidin in Fermentationsproben, Extraktionslösungen und Tyrothricin- bzw. Gramicidin-Fertigprodukten wird beschrieben. Nach der dünnschicht-chromatographischen Trennung des Gramicidins von den Begleitstoffen erfolgt eine quantitative Elution des Fleckes mit dem CAMAC Eluchrom, die so gewonnenen Lösungen werden spektralphotometrisch ausgewertet.
    Notes: Abstract A quantitative method is described for the determination of gramicidine in fermentation broths, extracts and finished products of tyrothricine and gramicidine, respectively. After TLC-separation of gramicidine from accompanying substances a quantitative elution of the gramicidine spot is performed with the CAMAG Eluchrom. The solutions obtained are measured spectrophotometrically.
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    Fresenius' Zeitschrift für analytische Chemie 268 (1974), S. 268-272 
    ISSN: 1618-2650
    Keywords: Chromatographie, Dünnschicht ; Peakerkennung u. Auswertung mit Digitalrechnern
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    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Die Arbeit beschreibt den prinzipiellen Aufbau eines Programms für Digitalrechner zur numerischen Peakerkennung und numerischen Integration von Remissionsgrad-Ortskurven bei der quantitativen DC. Durch integrierende Analog-Digitalwandlung und digitales Glätten wird das Signal/Rausch-Verhältnis verbessert. Die Peakerkennung erfolgt mit Hilfe der über eine Ausgleichsparabel numerisch differenzierten Meßkurve. Die Basislinienkorrektur bei nicht aufgelösten Peaks beruht auf einem Vergleich der Tangenten zwischen den Peakminima.
    Notes: Abstract The paper describes the principles of a programm for numerical peak detection and numerical integration for area determination by digital computers with respect to thin-layer chromatography. Integrating analog to digital conversion and digital smoothing will improve the signal to noise ratio. The first derivative will be found by smoothed numerical differentiation and is used for peak detection. The actual base line is corrected by eomparision of the tangents between the minima of the peaks.
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    Fresenius' Zeitschrift für analytische Chemie 269 (1974), S. 206-208 
    ISSN: 1618-2650
    Keywords: Best. von Dimethylsulfat in Luft ; Chromatographie, Dünnschicht ; Umsetzung zu Nitroanisol
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Es wird eine Methode beschrieben, die es gestattet, Dimethylsulfat (DMS) im Bereich der maximalen Arbeitsplatzkonzentration von 0,05 mg/m3 entsprechend 0,01 ppm zu bestimmen. Zunächst wird DMS zur Anreicherung an Kieselgel adsorbiert. Nach Desorption mit Aceton wird DMS mit 4-Nitrophenol-Na zu 4-Nitroanisol umgesetzt und dünnschicht-chromatographisch durch Intensitätsvergleich mit Standards bestimmt. Zur Erfassung des MAK-Wertes sind mindestens 500 l Probevolumen nötig. Bei einer Sauggeschwindigkeit von 3–4 l/min dauert daher eine Probenahme 2–2,5 Std. Über diesen Zeitraum sollten bei einer Raumluftuntersuchung möglichst ähnliche Konzentrationsverhältnisse vorliegen.
    Notes: Abstract A method is reported which allows the determination of dimethyl sulphate (DMS) in the range of the threshold limit of 0.05 mg/m3 resp. 0.01 ppm. At first DMS is concentrated by adsorption on silica gel. After extraction with acetone and reaction with 4-nitrophenol sodium salt to 4-nitroanisol the DMS is determined by thin-layer chromatography. Evaluation by comparison of intensity with standard spots. For the determination of the threshold limit at least 500 l of sample volume are needed. With an air sampling rate of 3 to 4 l/min the duration of sampling is 2 to 2.5 h. During this time the concentration of the examined air should not vary too much.
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    ISSN: 1618-2650
    Keywords: Nachw. von Mandelsäurebenzylester, Phenacetin, Coffein, Phenazon, Aminophenazon ; Chromatographie, Dünnschicht ; Fertigfolien mit Luminescenzindicator
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    Fresenius' Zeitschrift für analytische Chemie 264 (1973), S. 32-32 
    ISSN: 1618-2650
    Keywords: Best. von Toxaphen und γ-Hexachlorcyclohexan ; Chromatographie, Dünnschicht ; Fertigfolien mit Luminescenzindicator
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    Fresenius' Zeitschrift für analytische Chemie 265 (1973), S. 271-271 
    ISSN: 1618-2650
    Keywords: Trenn. von Kresolen und Phenol ; Chromatographie, Dünnschicht
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    Fresenius' Zeitschrift für analytische Chemie 266 (1973), S. 208-208 
    ISSN: 1618-2650
    Keywords: Trenn, von Isomeren von Hexachlorcyclohexan ; Chromatographie, Dünnschicht ; Fertigfolien
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 266 (1973), S. 286-287 
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    Keywords: Nachw. von Pepsin-Inhibitoren ; Chromatographie, Dünnschicht
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 266 (1973), S. 287-288 
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    Keywords: Best. von DDT in Milch ; Chromatographie, Dünnschicht ; Fertigfolien, Humanmilch
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    Fresenius' Zeitschrift für analytische Chemie 267 (1973), S. 45-45 
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    Keywords: Trenn. von Phenolen, mehrwertige ; Chromatographie, Dünnschicht ; Fertigfolien
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    Keywords: Trenn. von Adrenalin und Noradrenalin ; Chromatographie, Dünnschicht ; Fertigfolien
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    Fresenius' Zeitschrift für analytische Chemie 267 (1973), S. 46-46 
    ISSN: 1618-2650
    Keywords: Trenn. von Kupfer, Nickel, Kobalt, Wismut ; Chromatographie, Dünnschicht ; DDC-Komplexe
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 267 (1973), S. 127-128 
    ISSN: 1618-2650
    Keywords: Best. von Phthalsäureestern in Polyvinylchlorid, Weichmachern ; Chromatographie, Dünnschicht ; Spektralphotometrie
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Eine dünnschicht-chromatographische Methode zur quantitativen Bestimmung von Phthalsäureestern in wäßrigen Weich-PVC-Extrakten wurde entwickelt. Als Lösungsmittel dient Petroläther-Diäthyläther-Eisessig (8∶2∶0,1); die Beschichtung besteht aus 0,2 mm Silicagel mit Fluorescenzzusatz. Nach Auftrennung und Elution erfolgt eine photometrische Auswertung.
    Notes: Abstract A thinlayer chromatographic method for the quantitative determination of phthalic acid esters in aqueous PVC-plastic extracts has been developed. Petroleum ether/diethyl ether/glacial acetic acid (8∶2∶0.1) is used as solvent; the plates are coated with 0.2 mm of silica gel with fluorescent agent. After separation and elution a photometric determination is performed.
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    Fresenius' Zeitschrift für analytische Chemie 267 (1973), S. 368-368 
    ISSN: 1618-2650
    Keywords: Trenn. von Aminen, aromatische ; Chromatographie, Dünnschicht ; Charge-Transfer-Komplexe
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    Topics: Chemistry and Pharmacology
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    Fresenius' Zeitschrift für analytische Chemie 270 (1974), S. 19-23 
    ISSN: 1618-2650
    Keywords: Best. von Phthalsäure ; Chromatographie, Dünnschicht ; Remissionsmessung, Kopplung mit Tischrechner
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Am Beispiel der Bestimmung von Phthalsäure wird die on line-Kopplung eines programmierbaren elektronischen Tischrechners über einen Integrator zur automatischen quantitativen Auswertung von Dünnschicht-Chromatogrammen durch Messung der Remission beschrieben. Das Verfahren arbeitet mit Mittelwertbildung der Integratorwerte der Scans in und gegen die Fließrichtung, um Basislinienfehler zu eliminieren. Der Rechner ermittelt aus den Vergleichsflecken über die Methode der kleinsten Summe der Fehlerquadrate die Eichgerade und berechnet hierüber die Substanzmenge in den Analysenflecken. Für die Auswertung wird eine quadratische Abhängigkeit der Fläche unter der Remissionsgrad-Ortskurve von der Substanzkonzentration angenommen. Die erreichte Genauigkeit lag bei etwa 2–2,5% (genäherte relative Standardabweichung).
    Notes: Abstract The paper describes the coupling of TLC-photometer, electronic integrator and desk calculator for the determination of phthalic acid by measurement of the remission at 280.3 nm. The average of integrator counts by scanning in and against development of the plate avoids errors caused by base line-drifts. From standards on the plate results a straight line by least squares using the quadratic proportionality of peak area to concentration. From this straight line the concentrations will be determined. The error of this method is in the range of 2–2.5% (relative standard deviation).
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    Fresenius' Zeitschrift für analytische Chemie 270 (1974), S. 16-19 
    ISSN: 1618-2650
    Keywords: Best. von Organ. Säuren ; Chromatographie, Dünnschicht ; aliphatisch, aromatisch, Reisstärkeschichten
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary Aliphatic monocarboxylic, dicarboxylic, hydroxy, keto and amino acids were separated on rice starch thin layers with the solvent system: ethanol/water/ammonia (78∶20∶13). Different aromatic acids were separated on the same support with the solvent system: ethanol/n-butanol/water/ammonia (40∶30∶15∶15). Rf- and RM-values were determined and the validity of Martin's theoretical postulates on the relationship between chemical structure and Rf-values in partition chromatography was displayed. Calculation of group and basic constants was also carried out.
    Notes: Zusammenfassung Aliphatische Monocarbon-, Dicarbon-, Hydroxy-, Keto und Aminosäuren wurden dünnschicht-chromatographisch auf Reisstärke getrennt (Fließmittel: Äthanol/ Wasser/Ammoniak [78∶20∶13]). Verschiedene aromatische Säuren wurden auf der gleichen Schicht mit dem Fließmittel Äthanol/n-Butanol/Wasser/Ammoniak (40∶30∶15∶15) getrennt. Rf- und RM-Werte wurden bestimmt. Aufgrund der theoretischen Aufstellungen von Martin für die Beziehung zwischen Rf-Werten in der Verteilungs- chromatographie und chemischen Strukturen wurden Gruppen- und Grundkonstanten bestimmt.
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    Fresenius' Zeitschrift für analytische Chemie 270 (1974), S. 128-128 
    ISSN: 1618-2650
    Keywords: Trenn. von Pseudohalogeniden ; Chromatographie, Dünnschicht ; Fertigfolien, Nachweisgrenzen
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    Fresenius' Zeitschrift für analytische Chemie 270 (1974), S. 356-359 
    ISSN: 1618-2650
    Keywords: Nachw. von Pesticiden ; Chromatographie, Dünnschicht ; Nitroverbindungen
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Es wird eine Analysenmethode zum Nachweis und zur Trennung von 16 Nitro-Pesticiden beschrieben. Nach einer dünnschicht-chromatographischen Trennung werden die Nitroverbindungen in primäre aromatische Amine übergeführt, die durch Diazotierung und Kupplung mit Bratton-Marshall Reagens nachgewiesen werden. Die photometrische Messung des eluierten Azofarbstoffes gestattet eine quantitative Bestimmung.
    Notes: Abstract An analysis method for the detection and separation of sixteen nitro-pesticides is described. After thin-layer chromatographical separation, the nitro-compounds are converted to primary aromatic amines which are detected by diazotization and subsequent coupling with Bratton-Marshall reagent. The photometric measuring of the azo-dye, obtained by elution, permits quantitative determination.
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    Fresenius' Zeitschrift für analytische Chemie 270 (1974), S. 366-367 
    ISSN: 1618-2650
    Keywords: Nachw. von δ-Aminolävulinsäure-Dehydratase-Inhibitoren ; Chromatographie, Dünnschicht
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    Fresenius' Zeitschrift für analytische Chemie 270 (1974), S. 367-368 
    ISSN: 1618-2650
    Keywords: Nachw. von Peroxidase-Inhibitoren ; Chromatographie, Dünnschicht
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    Topics: Chemistry and Pharmacology
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