DE19712708A1 - Dried hydrocolloid or hydrogel based on polysaccharide(s) - Google Patents
Dried hydrocolloid or hydrogel based on polysaccharide(s)Info
- Publication number
- DE19712708A1 DE19712708A1 DE1997112708 DE19712708A DE19712708A1 DE 19712708 A1 DE19712708 A1 DE 19712708A1 DE 1997112708 DE1997112708 DE 1997112708 DE 19712708 A DE19712708 A DE 19712708A DE 19712708 A1 DE19712708 A1 DE 19712708A1
- Authority
- DE
- Germany
- Prior art keywords
- mass
- hydrocolloids
- hydrogels
- dried
- microwaves
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
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Abstract
Description
Die Erfindung betrifft getrocknete kontaminationsarme Hydrokolloide und/oder Hydrogele auf Basis von Polysacchariden für den Einsatz in Pharmazie, Kosmetik, Medizintechnik und Biotechnologie.The invention relates to dried, low-contamination hydrocolloids and / or Hydrogels based on polysaccharides for use in pharmacy, cosmetics, Medical technology and biotechnology.
Lösliche Kolloide in Form von Hydrokolloiden und nicht lösliche Kolloide in Form von Hydrogelen auf Basis von Polysacchariden sind bekannt.Soluble colloids in the form of hydrocolloids and insoluble colloids in the form of Hydrogels based on polysaccharides are known.
Die für den spezifischen Einsatz erforderliche Trocknung der Hydrokolloide bzw. Hydrogele kann zu einem unerwünschten Abfall der Molmasse und zu unerwünsch ten chemischen Veränderungen gegenüber dem Ausgangsprodukt führen.The drying of the hydrocolloids or Hydrogels can lead to an undesirable drop in molecular weight and undesirable lead to chemical changes compared to the starting product.
Bekannte Trocknungsverfahren für Polysaccharide sind die thermische Trocknung durch Wärmekonvektion sowie die Gefriertrocknung im Vacuum.Known drying processes for polysaccharides are thermal drying through heat convection and freeze drying in a vacuum.
WO 95 25751 beschreibt die Herstellung von Flächengebilden aus dem Polysaccha rid Hyaluronsäure durch Heißlufttrocknung. Die Herstellung gefriergetrockneter Biomatrices auf Basis natürlicher und modifizierter Polysaccharide ist Gegenstand von DE 43 28 329. Diese Biomatrices besitzen eine Hohlraumstruktur, in die Flüssigkeiten schnell und ungehindert eindringen kann. Die Gefriertrocknung bei der Herstellung von Kollagenschwämmen wird in den Patenten DE 27 34 503, DE 29 43 520 und DE 40 28 622 beschrieben. Ebenfalls hier liefert das Trocknungsverfahren eine schwammartige Struktur der Biomatrix. Die Herstellung von Flächengebilden mit poröser Struktur auf Basis von Hyaluronsäure und Hyaluronsäurederivaten durch Gefriertrocknung ist Gegenstand von DE 40 24 180.WO 95 25751 describes the production of fabrics from the polysaccha rid hyaluronic acid by hot air drying. The production of freeze-dried Biomatrices based on natural and modified polysaccharides are the subject from DE 43 28 329. These biomatrices have a cavity structure into which Liquids can penetrate quickly and freely. Freeze drying at The production of collagen sponges is described in the patents DE 27 34 503, DE 29 43 520 and DE 40 28 622. The drying process also delivers here a spongy structure of the biomatrix. The manufacture of fabrics with a porous structure based on hyaluronic acid and hyaluronic acid derivatives Freeze drying is the subject of DE 40 24 180.
Die Nachteile der thermischen Trocknung von Polysacchariden durch Wärmekonvektion bilden der inhomogene Trocknungsablauf sowie die thermische Schädigung der Polysaccharide durch Molmassenabbau und chemische Veränderungen. Bei kurzen Trocknungszeiten resultieren lokale Überhitzungen, da das Produkt zuerst an der Oberfläche trocknet. Die bestehende äußere harte trockene Kruste erschwert den weiteren Trocknungsvorgang im Inneren des Materials, es treten chemischen Schädigung durch Molmassenabbau und chemische Veränderungen wie Decarboxylierungen auf und es resultieren inhomogene Produkte bezüglich des Feuchtigkeitsgehalts. Längere Trocknungszeiten bei niedrigeren Temperaturen ergeben einheitlichere Produkte bezüglich des Feuchtigkeitsgehalts, führen jedoch bei hitzelabilen Polysacchariden in der Regel zu einer beträchtlichen Molmassendegradation, verbunden mit oxidativen Veränderungen und einem Abfall der Werkstoffeigenschaften, insbesondere der elastischen Eigenschaften. Eine weitere Folge von langen Trocknungszeiten kann in der mikrobiellen Kontamination der Polysaccharide und dem damit verbundenen Abbau durch Mikroorganismen bestehen.The disadvantages of thermal drying of polysaccharides The inhomogeneous drying process and the thermal form convection Damage to the polysaccharides due to molecular weight degradation and chemical Changes. With short drying times, local overheating results because the product dries on the surface first. The existing outer hard dry crust complicates the further drying process inside the Materials, chemical damage from molecular weight degradation and chemical damage occur Changes such as decarboxylations occur and the results are inhomogeneous Products related to moisture content. Longer drying times at lower temperatures result in more uniform products in terms of Moisture content, however, usually lead to heat unstable polysaccharides considerable molecular mass degradation combined with oxidative Changes and a decrease in material properties, especially the elastic properties. Another consequence of long drying times can be in the microbial contamination of the polysaccharides and the associated Degradation by microorganisms exist.
Die Nachteile der Gefriertrocknung von Polysacchariden bestehen in der schwammartigen Struktur der gefriergetrockneten Produkte. In die Hohlräume der gefriergetrockneten Polysaccharide können Flüssigkeiten schnell und ungehindert eindringen und damit einen spontanen Zerfall des Netzwerkes der Matrix herbeiführen. Durch diesen Instanteffekt wird die Eigenschaft der Wasser- und Wirksubstanzspeicherung der Matrix schnell aufgehoben.The disadvantages of freeze-drying polysaccharides are sponge-like structure of freeze-dried products. Into the cavities of the Freeze-dried polysaccharides can handle liquids quickly and freely penetrate and thus a spontaneous decay of the network of the matrix bring about. Through this instant effect, the property of water and Active substance storage of the matrix quickly removed.
Für Beschichtungen werden kompakte Oberflächenschichten mit guten Werkstoffeigenschaften und Langzeitstabilität gefordert, schwammartige Strukturen sind für dieses Einsatzgebiet ungeeignet.For coatings, compact surface layers with good Material properties and long-term stability required, sponge-like structures are unsuitable for this application.
Ziel der Erfindung sind daher getrocknete Hydrokolloide und/oder Hydrogele auf Basis von Polysacchariden, die sich durch eine hohe Produkthomogenität auszeich nen, kontaminationsarm sind und die gegenüber den Ausgangsprodukten nur einen geringen Abfall der Molmasse besitzen und höchstens geringfügig chemisch verän dert sind.The aim of the invention is therefore dried hydrocolloids and / or hydrogels Basis of polysaccharides, which is characterized by a high product homogeneity are low in contamination and only one compared to the starting products have a small drop in molecular weight and at most slightly change chemically changed.
Die erfindungsgemäße Aufgabe wurde durch getrocknete kontaminationsarme Hydrokolloide und/oder Hydrogele, gegebenenfalls in Form von Flächengebilden, mit einer Dichte von 0,05 bis 1,50 g/cm3 und einem Restwassergehalt von 1 bis 80 Masse% auf Basis von nichtmodifizierten und/oder modifizierten natürlichen , bio technisch erzeugten und/oder halbsynthetischen Polysacchariden und gegebenen falls 0,01 bis 60 Masse%, bezogen auf die Hydrokolloide und/oder Hydrogele, an Zusatzstoffen, gelöst, wobei die Trocknung der Hydrokolloide und/oder Hydrogele unter der Einwirkung der thermischen Energie von Mikrowellen und gegebenenfalls der thermischen Energie von erwärmten Gasen und/oder IR-Strahlern gleichmäßig und schonend unter weitgehendem Erhalt der Ausgangsmolmasse erfolgt ist.The object of the invention was achieved by dried low-contamination hydrocolloids and / or hydrogels, optionally in the form of fabrics, with a density of 0.05 to 1.50 g / cm 3 and a residual water content of 1 to 80% by mass based on unmodified and / or modified natural, bio-technically produced and / or semi-synthetic polysaccharides and, if appropriate, 0.01 to 60% by mass, based on the hydrocolloids and / or hydrogels, of additives, dissolved, the drying of the hydrocolloids and / or hydrogels under the action of the thermal Energy from microwaves and possibly the thermal energy from heated gases and / or IR emitters has been carried out evenly and gently while largely maintaining the initial molar mass.
Die getrockneten kontaminationsarmen Hydrokolloide und/oder Hydrogele besitzen als Folge der Mikrowellenbehandlung Keimzahlen von maximal 100 Keimen/g getrocknetes Hydrokolloid bzw. Hydrogel.Have the dried low-contamination hydrocolloids and / or hydrogels as a result of the microwave treatment, bacterial counts of maximum 100 germs / g dried hydrocolloid or hydrogel.
Die nichtmodifizierten und/oder modifizierten natürlichen, biotechnisch erzeugten und/oder halbsynthetischen Polysaccharide sind bevorzugt nichtmodifizierte und/oder modifizierte Pektine, Chitine, Chondroitine, Heparine, Stärken, Dextrane, Pullulane, Xanthane, Welane, Rhamsane, Curdlane, Alginate, Carrageenane, Keratane, Hyaluronsäuren, Dermatane, Gellane, Schizophyllane und/oder Polysaccharide aus Johannisbrotmehl, Agar, Arabisch Gummi, Tragant, Guar gum, Fenugreek gum, Locust bean gum und/oder Tara gum.The unmodified and / or modified natural, biotechnologically produced and / or semi-synthetic polysaccharides are preferably unmodified and / or modified pectins, chitins, chondroitins, heparins, starches, dextrans, Pullulane, Xanthane, Welane, Rhamsane, Curdlane, Alginate, Carrageenane, Keratans, hyaluronic acids, dermatans, gellans, schizophyllans and / or Polysaccharides from carob flour, agar, Arabic gum, tragacanth, guar gum, Fenugreek gum, Locust bean gum and / or Tara gum.
Beispiele für modifizierte Polysaccharide sind Carboxymethylstarke, Hydrnxyethylstärke, Dialdehydstärke, Pektinester, Chitosane, verätherter Guar gum, acetylierte Hyaluronsäuren, Hyaluronsäureester und vernetzte bzw. teilvernetzte Hyaluronsäuren.Examples of modified polysaccharides are carboxymethyl-strong, Hydroxyethyl starch, dialdehyde starch, pectin esters, chitosans, etherified guar gum, acetylated hyaluronic acids, hyaluronic acid esters and cross-linked or partially cross-linked Hyaluronic acids.
Die gegebenenfalls enthaltenen Zusatzstoffe sind bevorzugt 0,1 Masse% bis 25 Masse% filmbildende Binde- und/oder Verdickungsmittel, 0,01 Masse% bis 0,25 Masse% Konservierungsmittel, 1 Masse% bis 30 Masse% stabilitätsverbessernde faser-förmige Trägermaterialien und/oder stabilitätsverbessernde Trägermaterialien in Form von textilen und/oder gitterartigen Flächengebilden, 0,05 bis 10 Masse% Mineralstoffe, 0,05 bis 3 Masse% micellbildende Stoffe, 1 bis 25 Masse% Weichmacher, 0,05 bis 30 Masse% kosmetische und/oder pharmazeutische Wirkstoffe, 1 bis 30 Masse% Vehikel für Wirkstoffe, 0.05 bis 2 Masse% Antioxi dantien, 0,05 bis 2% Duftstoffe und/oder 0,05 bis 5 Masse% Farbstoffe, wobei sich die Anteile jeweils auf die Hydrokolloide und/oder Hydrogele beziehen.The additives optionally contained are preferably 0.1% by mass to 25% % By mass of film-forming binders and / or thickeners, 0.01% by mass to 0.25 Mass% preservative, 1 mass% to 30 mass% stability-improving fibrous carrier materials and / or stability-improving carrier materials in the form of textile and / or grid-like fabrics, 0.05 to 10 mass% Minerals, 0.05 to 3 mass% micelle-forming substances, 1 to 25 mass% Plasticizers, 0.05 to 30% by mass cosmetic and / or pharmaceutical Active substances, 1 to 30 mass% vehicle for active substances, 0.05 to 2 mass% antioxidant dantien, 0.05 to 2% fragrances and / or 0.05 to 5% by mass of dyes, whereby the proportions each relate to the hydrocolloids and / or hydrogels.
Die filmbildenden Binde- und/oder Verdickungsmittel bestehen aus Kunststoffen und/oder semisynthetischen modifizierten Naturstoffen, bevorzugt aus Stärkeäthern, Natriumalginat, Cellulosederivaten wie Carboxymethylcellulose, Celluloseäther, Celluloseestern und Alkylcellulosen, Polyvinylacetat, Polyvinylalkohol, teilverseifte Polyacrylsäureester und/oder teilverseiften Polymethacrylsäureestern. Ein besonders bevorzugtes filmbildendes Binde- und/oder Verdickungsmittel ist Carboxymethylcellulose auf Grund der reversiblen Wasserlöslichkeit und guten Verträglichkeit, insbesondere bei medizinischen und kosmetischen Anwendungen.The film-forming binders and / or thickeners consist of plastics and / or semi-synthetic modified natural substances, preferably from starch ethers, Sodium alginate, cellulose derivatives such as carboxymethyl cellulose, cellulose ether, Cellulose esters and alkyl celluloses, polyvinyl acetate, polyvinyl alcohol, partially saponified Polyacrylic acid esters and / or partially saponified polymethacrylic acid esters. A is particularly preferred film-forming binder and / or thickener Carboxymethyl cellulose due to the reversible water solubility and good Compatibility, especially in medical and cosmetic applications.
Beispiele für geeignete Konservierungsmittel sind p-Hydroxybenzoesäure, Benzylalkohol und Propylenglycol. Für medizinische und kosmetische Anwen dungen, bei denen Hautirritationen ausgeschlossen werden müssen, sind p-Hy droxybenzoesäureester und Sorbinsäure besonders geeignet.Examples of suitable preservatives are p-hydroxybenzoic acid, Benzyl alcohol and propylene glycol. For medical and cosmetic applications Applications where skin irritation has to be excluded are p-Hy droxybenzoic acid ester and sorbic acid are particularly suitable.
Die stabilitätsverbessernden faserförmigen Trägermaterialien und/oder stabilitäts verbessernden Trägermaterialien in Form von textilen und/oder gitterartigen Flächengebilden bestehen bevorzugt aus Cellulose, Celluloseestern, Calciumal ginat, Wolle, Baumwolle, Seide, Polyamiden, Polyestern, Polyethern, Polyvinylal kohol und/oder Polyolefinen. Diese Trägermaterialien erhöhen die mechanische Trockenstabilität der getrockneten Hydrokolloide und Hydrogele, die Auswahl der Form der Trägermaterialien erfolgt in Abhängigkeit von der Applikation, z. B. sind Nähfadenvliesgewirke auf Baumwollbasis geeignete Trägermaterialien für Hydrokolloide mit Wirkstoffeigenschaften bei der Wundversorgung.The stability-improving fibrous carrier materials and / or stability improving carrier materials in the form of textile and / or grid-like Sheets preferably consist of cellulose, cellulose esters, calciumal ginate, wool, cotton, silk, polyamides, polyesters, polyethers, polyvinylal alcohol and / or polyolefins. These carrier materials increase the mechanical Dry stability of the dried hydrocolloids and hydrogels, the selection of the The shape of the carrier materials depends on the application, e.g. B. are Sewing thread nonwoven fabrics on the basis of cotton suitable carrier materials for Hydrocolloids with active ingredient properties in wound care.
Geeignete Mineralstoffe als Zusatzstoffe in getrockneten Hydrokolloiden und Hydrogelen sind Aluminiumhydroxid, Magnesiumhydroxid, Zinkoxid, Calcium carbonat, Talkum, Bentonit, Kieselerde und/oder Wollastonit. Diese Mineralstoffe stabilisieren das Hydrokolloid bzw. das Hydrogel und/oder regulieren bei medizi nischen Anwendungen den Elektrolythaushalt an der entsprechenden Applikations stelle.Suitable minerals as additives in dried hydrocolloids and Hydrogels are aluminum hydroxide, magnesium hydroxide, zinc oxide, calcium carbonate, talc, bentonite, silica and / or wollastonite. These minerals stabilize the hydrocolloid or the hydrogel and / or regulate with medication applications, the electrolyte balance on the corresponding application Job.
Beispiele für micellbildende Stoffe sind höhere Alkohole wie Cetylalkohol, Stearylalkohol und Wollwachsalkohole, Natriumlaurylethersulfat, Fettsäureamide, Natriumsalze von Fettsäuren und Lecithin. Bevorzugt werden als micellbildende Stoffe nichtionische Emulgatoren wie Polyglycolester und Polyglycolether.Examples of micelle-forming substances are higher alcohols such as cetyl alcohol, Stearyl alcohol and wool wax alcohols, sodium lauryl ether sulfate, fatty acid amides, Sodium salts of fatty acids and lecithin. Are preferred as micelle-forming Substances non-ionic emulsifiers such as polyglycol esters and polyglycol ethers.
Geeignete Weichmacher als flexibilisierende Zusatzstoffe in getrockneten Hydro kolloiden und Hydrogelen sind Glycerin, Glycerinalkylätherncetat, Polyethylen glycoldiethylhexoat, 2-Ethylhexyl-p-hydroxybenzoat, Stearylcitrat und Polyvinyl methyläther. Für medizinische und kosmetische Anwendungen ist Glycerin bevor zugt geeignet.Suitable plasticizers as flexibilizing additives in dried hydro Colloids and hydrogels are glycerin, glyceryl alkyl ether acetate, polyethylene glycol diethylhexoate, 2-ethylhexyl p-hydroxybenzoate, stearyl citrate and polyvinyl methyl ether. Glycerin is coming for medical and cosmetic applications suitable.
Beispiele für kosmetische und pharmazeutische Wirkstoffe sind ätherische Öle, Corticosteroide, Pyribenzamine, Pilocarpinnitrat, Tyrothricin, Folsäure, Nicotinsäureamid, Nicotinsäureester. Bevorzugt eingesetzt werden Vitamine wie Vitamin A, Vitamin B1, Vitamin B6, Vitamin E sowie hautpenetrationsfördernde Mittel wie Polyoxyethylennonylphenol.Examples of cosmetic and pharmaceutical active ingredients are essential oils, Corticosteroids, pyribenzamines, pilocarpine nitrate, tyrothricin, folic acid, Nicotinic acid amide, nicotinic acid ester. Vitamins such as are preferably used Vitamin A, Vitamin B1, Vitamin B6, Vitamin E and skin penetration-promoting agents such as polyoxyethylene nonylphenol.
Als Vehikel für den Transport von Wirkstoffen, die die getrockneten Hydrokolloide und/oder Hydrogele als Zusatzstoffe enthalten, sind Liposome geeignet.As a vehicle for the transport of active ingredients, the dried hydrocolloids and / or contain hydrogels as additives, liposomes are suitable.
Beispiele für geeignete Antioxidantien sind Thiodipropionsäure, Tocopherol und α lonon. Bevorzugt geeignet ist Ascorbinsäure.Examples of suitable antioxidants are thiodipropionic acid, tocopherol and α lonon. Ascorbic acid is particularly suitable.
Die Riechstoffe können aus natürlichen Riechstoffkomplexen, insbesondere ätherischen Ölen, sowie synthetischen einheitlichen Riechstoffen wie Limonen, Phellandren, Zimtalkohol, Fenchylalkohol oder Geraneol bestehen. Bevorzugt werden Riechstoffe auf Basis ätherischer Öle.The fragrances can be composed of natural fragrance complexes, in particular essential oils, as well as synthetic uniform fragrances such as limonene, Phellandrene, cinnamon alcohol, fenchyl alcohol or geraneol exist. Prefers become fragrance substances based on essential oils.
Als Zusatzstoffe zur Markierung und Einfärbung in den getrockneten Hydrokolloiden und/oder Hydrogelen enthaltenen Farbstoffe sind bevorzugt natürliche pflanzliche. As additives for marking and coloring in the dried hydrocolloids and / or hydrogels contained dyes are preferably natural vegetable.
Als Zusatzstoffe zur Markierung und Einfärbung in den getrockneten Hydrokolloiden und/oder Hydrogelen enthaltenen Farbstoffe sind bevorzugt natürliche pflanzliche Farbstoffe wie Alkanna, Calendula, Crocus, lndicum, Carotin, Lactoflavin, Chlorophyll und Santalum rubrum, Farbpigmente wie Bariumsulfat, Zinkoxid, Titandioxid und Eisenoxid sowie synthetische Farbstoffe, z. B. auf Triphenyl methanbasis oder Anthrachinonbasis, geeignet.As additives for marking and coloring in the dried hydrocolloids and / or hydrogels contained dyes are preferably natural vegetable Dyes such as alkanna, calendula, crocus, indicum, carotene, lactoflavin, Chlorophyll and santalum rubrum, color pigments such as barium sulfate, zinc oxide, Titanium dioxide and iron oxide as well as synthetic dyes, e.g. B. on triphenyl methane-based or anthraquinone-based.
Bevorzugt besitzen die unter der Einwirkung der thermischen Energie von Mikrowellen und gegebenenfalls der thermischen Energie von erwärmten Gasen und/oder IR-Strahlern getrockneten Hydrokolloide ein Molmassen-Zahlenmittel von mindestens 75% des Molmassen-Zahlenmittels der als Ausgangsprodukt einge setzten Hydrokolloide. Die Ermittlung der Molmassen-Zahlenmittel von Hyddro kolloiden kann durch GPC-Analyse in Verbindung mit Lichtstreuungsmessungen erfolgen [Orvisky, E., Chromatographia (1994), 39 (5/6), 366-368; Vercruysse, K, J. Chromatogr., Pt. B Biomed.Appl. (1994), 656 (1), 179-190].Under the influence of the thermal energy of Microwaves and possibly the thermal energy of heated gases and / or IR radiators dried hydrocolloids a number average molecular weight of at least 75% of the number average molecular weight is used as the starting product put hydrocolloids. Determining the number average molecular weight of Hyddro Colloids can be measured by GPC analysis in conjunction with light scattering measurements [Orvisky, E., Chromatographia (1994), 39 (5/6), 366-368; Vercruysse, K, J. Chromatogr., Pt. B Biomed.Appl. (1994), 656 (1), 179-190].
Erfindungsgemäß erfolgt die Herstellung der gleichmäßig und schonend unter weitgehendem Erhalt der Ausgangsmolmasse getrockneten kontaminationsarmen Hydrokolloide und/oder Hydrogele, gegebenenfalls in Form von Flächengebilden, mit Dichten im Bereich von 0,05 bis 1,50 g/cm3 und einem Restwassergehalt von 1 bis 80 Masse% auf Basis von nichtmodifizierten und/oder modifizierten natürlichen, biotechnisch erzeugten und/oder halbsynthetischen Polysacchariden und gegebenenfalls 0,01 bis 60 Masse%, bezogen auf die Hydrokolloide und/oder Hydrogele, an Zusatzstoffen sowie gegebenenfalls 0,1 bis 10 Masse%, bezogen auf die Hydrokolloide und/oder Hydrogele, an Treibmitteln, nach einem Trocknungs verfahren unter der Einwirkung der thermischen Energie von Mikrowellen und gegebenenfalls der thermischen Energie von erwärmten Gasen und/oder IR- Strahlern.According to the invention, the low-contamination hydrocolloids and / or hydrogels dried evenly and gently while largely maintaining the starting molar mass are produced, optionally in the form of sheet-like structures, with densities in the range from 0.05 to 1.50 g / cm 3 and a residual water content of 1 to 80 % By mass based on unmodified and / or modified natural, biotechnologically produced and / or semi-synthetic polysaccharides and optionally 0.01 to 60% by mass, based on the hydrocolloids and / or hydrogels, of additives and optionally 0.1 to 10% by mass, based on the hydrocolloids and / or hydrogels, of blowing agents, after a drying process under the action of the thermal energy of microwaves and, if appropriate, the thermal energy of heated gases and / or IR radiators.
Bei der gegebenenfalls zusätzlichen Einwirkung der thermischen Energie von erwärmten Gasen und/oder IR-Strahlern bei der Trocknung von Hydrokolloiden und/oder Hydrogelen erfolgt die Einwirkung der thermischen Energie der Mikro wellen gleichzeitig und/oder nach der Einwirkung der thermischen Energie von erwärmten Gasen und/oder IR-Strahlern. Dabei wird das Verhältnis von Mikro wellenenergie zur Temperatur und zur Durchsatzmenge des Gases so gewählt, daß der Anteil der Mikrowellenenergie an der zur Trocknung der Hydrokolloide aufgewendeten Gesamtenergie 95 bis 10% beträgt. Die zur Trocknung der Hydro kolloide eingesetzten Gase werden bevorzugt ganz oder teilweise im Wärmeaustauscher der Mikrowellengeneratoren erwärmt.In the event of additional exposure to the thermal energy of heated gases and / or IR emitters when drying hydrocolloids and / or hydrogels, the thermal energy of the micro acts waves simultaneously and / or after exposure to thermal energy heated gases and / or IR emitters. The ratio of micro wave energy to the temperature and flow rate of the gas selected so that the proportion of microwave energy in the drying of the hydrocolloids total energy used is 95 to 10%. The for drying the Hydro Colloidal gases are preferably wholly or partly in the Heat exchanger of the microwave generators heated.
Vorteilhaft ist, daß durch das erfindungsgemäße Verfahren ebenfalls getrocknete Hydrokolloide und/oder Hydrogele in geschäumter Form hergestellt werden können. Beispiele für Treibmittel, die die Hydrokolloide und/oder Hydrogele bei der Trocknung gegebenenfalls zur einer definierten Einstellung der Porosität und Dichte bei der Herstellung von geschäumten getrockneten Materialien enthalten können, sind gasabspaltende Treibmittel wie Azodicarbonamid oder Cyanursäuretrihydrazid, leichtflüchtige Kohlenwasserstoffe und Halogenkohlenwasserstoffe wie Pentan, Isobutan, Monofluortrichlormethan oder Difluormonochlormethan oder Gase wie Stickstoff, Argon oder Kohlendioxid. Getrocknete geschäumte Hydrokolloide bzw. Hydrogele mit Dichten im Bereich von 0,50 bis 1,50 g/cm3 erfordern im allgemeinen keinen zusätzlichen Einsatz von Treibmitteln, da die Dichte des geschlossenzelligen geschäumten Materials bzw. die Porosität des offenzelligen geschäumten Materials durch den Energieeintrag der Mikrowellenbehandlung und die daraus resultierende Diffusionskinetik des Wasserdampfes gesteuert werden kann. Die Schaumdichte bzw. die Porosität des getrockneten Materials bestimmt dabei die Quellungs- bzw. Absorptionsgeschwindigkeit bei der Applikation.It is advantageous that dried hydrocolloids and / or hydrogels can also be produced in foamed form by the process according to the invention. Examples of blowing agents which the hydrocolloids and / or hydrogels may contain during drying to adjust the porosity and density in the production of foamed dried materials, are gas-releasing blowing agents such as azodicarbonamide or cyanuric acid trihydrazide, volatile hydrocarbons and halogenated hydrocarbons such as pentane, isobutane, Monofluorotrichloromethane or difluoromonochloromethane or gases such as nitrogen, argon or carbon dioxide. Dried foamed hydrocolloids or hydrogels with densities in the range from 0.50 to 1.50 g / cm 3 generally do not require any additional blowing agents, since the density of the closed-cell foamed material or the porosity of the open-cell foamed material due to the energy input Microwave treatment and the resulting diffusion kinetics of water vapor can be controlled. The foam density or the porosity of the dried material determines the swelling or absorption rate during application.
Das Einbringen der thermischen Energie von Mikrowellen einer Frequenz von bevorzugt 2,4 bis 2,5 GHz erfolgt erfindungsgemäß als kontinuierliche Leistung oder als modulierte und/oder impulsförmige Leistung. Dabei wird die anzuwendende Modulation und/ oder Impulsform und die Amplitude der Mikrowellenenergie durch die erforderlichen Eigenschaften des konkreten getrockneten Materials bestimmt. So erfordern weitgehende hohlraumfreie Folien geringe Mikrowellenleistungen und/oder kurze Mikrowellenimpulse und lange Pausen. Die Impulsdauer der Mikrowel lenbestrahlung soll erfindungsgemäß 10 bis 95% der Periodendauer des Leistungsprofils betragen. The introduction of the thermal energy of microwaves with a frequency of preferably 2.4 to 2.5 GHz takes place according to the invention as a continuous power or as modulated and / or pulsed power. The applicable one Modulation and / or pulse shape and the amplitude of the microwave energy by determines the required properties of the specific dried material. So extensive void-free foils require low microwave power and / or short microwave pulses and long pauses. The pulse duration of the microwave Len irradiation according to the invention is 10 to 95% of the period of the Performance profile.
Bei Applikationen, bei denen die Trocknung dünner Schichten erforderlich ist, ist die Anwendung von Applikatoren, die Ein- oder Mehrmodenresonatoren darstellen, vor teilhaft.For applications that require the drying of thin layers, the Application of applicators that represent single or multimode resonators partial.
Weiterhin ist die Anwendung mehrerer unterschiedlich angekoppelter Resonatoren von Vorteil, um den sich verändernden dielektrischen Eigenschaften des zu trocknenden Materials zu entsprechen die die erforderliche Mikrowellenleistung am entsprechenden Ort und/oder zur entsprechenden Zeit auf das Material wirken zu lassen. Bei Anwendung eines Mikrowellentunnels mit mehreren Einspeisungen wird die Ankopplung der unterschiedlichen Einspeisstellen entsprechend dem Trock nungsgrad und der erforderlichen Trocknungsgeschwindigkeit eingerichtet.Furthermore, the use of several differently coupled resonators beneficial to the changing dielectric properties of the drying material to meet the required microwave power on appropriate place and / or at the appropriate time act on the material to let. When using a microwave tunnel with multiple feeds the coupling of the different feed points according to the dry Degree of efficiency and the required drying rate set up.
Bei Anwendung von Ein- oder Mehrmodenresonatoren mit bekannter Modenform kann bei Transport des zu trocknenden Materials durch den Resonator die erforderliche Modulation der Mikrowellenbestrahlung durch die Anpassung der Länge des Resonators und der Transportgeschwindigkeit erfolgen.When using single or multi-mode resonators with a known mode shape can transport the material to be dried through the resonator required modulation of the microwave radiation by adjusting the The length of the resonator and the transport speed take place.
Die unter der Einwirkung der thermischen Energie von Mikrowellen gleichmäßig und schonend unter weitgehendem Erhalt der Ausgangsmolmasse getrockneten kontaminationsarmen Hydrokolloide und/oder Hydrogele mit einer Dichte von 0,05 bis 1,50g/cm3 und einem Restwassergehalt von 1 bis 80 Masse%, gegebenenfalls in Form von Flächengebilden, auf Basis von natürlichen , biotechnisch erzeugten und/oder halbsynthetischen Polysacchariden und gegebenenfalls 0,01 bis 60 Masse%, bezogen auf die Hydrokolloide und/oder Hydrogele, an Zusatzstoffen sind insbesondere als Kosmetika, zur topischen ophthamologischen, dermalen und/oder transdermalen Applikation von Wirkstoffen, insbesondere als "drug delivery system", als Komponenten für Implantate, als Komponenten zur Behandlung von von Arteriosklerose, Arthritis, Thrombosen und/oder traumatischen Beschwerden, zur Förderung von Angiogenese, Wundheilung und entzündungshemmenden Prozessen sowie als Support-Matrix für den Einsatz in der Zellkulturtechnik geeignet.The low-contamination hydrocolloids and / or hydrogels dried evenly and gently under the influence of the thermal energy of microwaves while largely maintaining the starting molar mass, with a density of 0.05 to 1.50 g / cm 3 and a residual water content of 1 to 80 mass%, optionally in Form of sheet-like structures, based on natural, biotechnologically produced and / or semi-synthetic polysaccharides and optionally 0.01 to 60% by mass, based on the hydrocolloids and / or hydrogels, of additives are in particular as cosmetics, for topical ophthalmic, dermal and / or transdermal application of active ingredients, in particular as a "drug delivery system", as components for implants, as components for the treatment of arteriosclerosis, arthritis, thromboses and / or traumatic complaints, for promoting angiogenesis, wound healing and anti-inflammatory processes and as a support matrix for use in cell culture technology k suitable.
Dabei erfolgt die Anwendung bevorzugt in Form von beschichteten und/oder getränkten Trägermaterialien, insbesondere von Geweben, Gewirken, Vliesen, Gestricken oder polsterartigen Stoffen sowie in Form von Gelen, Membranen, Filmen, Microspheres, Salben und/oder Schäumen.The application is preferably in the form of coated and / or impregnated carrier materials, in particular fabrics, knitted fabrics, nonwovens, Knitted or cushion-like fabrics as well as in the form of gels, membranes, Films, microspheres, ointments and / or foams.
Eine weitere Anwendung der unter der Einwirkung der thermischen Energie von Mikrowellen gleichmäßig und schonend unter weitgehendem Erhalt der Ausgangsmolmasse getrockneten kontaminationsarmen Hydrokolloiden und/oder Hydrogelen mit einem Restwassergehalt von 1 bis 80 Masse% bildet die Verbesserung der Gleitfähigkeit von Medikamenten, Erzeugnissen und Geräten aus Glas, Keramik, Kunststoffen und/oder Naturstoffen, insbesondere von prothetischen Erzeugnissen, Kathetern, Ultraschallmeßköpfen und Endoskopieinstrumenten. Die Erhöhung der Gleitfähigkeit resultiert aus der Wasseraufnahme der Kolloide in der Beschichtung bei Flüssigkeitszufuhr. Die erhöhte Gleitfähigkeit bewirkt eine Herabsetzung der Reizung der Epidermis bei der medizinischen Anwendung und erleichtert dadurch insbesondere das Einführen von Kathetern in Körperöffnungen.Another application of under the influence of thermal energy Microwaves evenly and gently while largely maintaining the Starting molar mass of dried low-contamination hydrocolloids and / or Hydrogels with a residual water content of 1 to 80% by mass form the Improve the lubricity of drugs, products and devices Glass, ceramics, plastics and / or natural materials, especially prosthetic ones Products, catheters, ultrasound probes and endoscopic instruments. The Increased lubricity results from the water absorption of the colloids in the Coating when hydrated. The increased lubricity causes Reduction of the irritation of the epidermis in the medical application and This particularly facilitates the insertion of catheters into body openings.
In beschichteten Medikamenten wirken die eingesetzten Hydrokoloide oder Hydrogele gleichzeitig als "drug delivery system".The hydrocoloids or act in coated drugs Hydrogels simultaneously as a "drug delivery system".
Die Erfindung wird durch nachfolgende Beispiele erläutert:The invention is illustrated by the following examples:
Gehäuse von Ultraschallmeßköpfen mit einer Oberfläche von rd. 85 cm2 aus Polypropylen durchlaufen kontinuierlich eine Tauchstation, die eine Beschichtungsrezeptur aus 22g Hyaluronsäure, 12g Carboxymethylcellulose, 4 g Glycerin und 0,3g Sorbinsäure in 1 l Wasser gelöst enthält, und nachfolgend bei einer Durchlaufgeschwindigkeit von 0,17m//min einen 2,5 m langen Mikrowel lentunnel mit vier, entsprechend dem Trocknungsgrad des Materials unterschiedlich angepaßten Einspeisstellen einer Gesamtleistungsaufnahme von rd. 8,5 kW, durch den gleichzeitig die auf 40 bis 45°C erwärmte Luft aus den Wärmetauschern der Mikrowellengeneratoren geführt wird. Die resultierende abriebfeste Beschichtung des Meßkopfgehäuses besitzt eine Dicke von 250 µm, einen Wassergehalt von 12 Masse% und zeigt keinerlei Verfärbung als Folge der Wärmebehandlung. Housing of ultrasonic measuring heads with a surface of approx. 85 cm 2 of polypropylene continuously pass through a dipping station which contains a coating formulation of 22 g hyaluronic acid, 12 g carboxymethyl cellulose, 4 g glycerol and 0.3 g sorbic acid dissolved in 1 l water, and subsequently a 2 at a throughput speed of 0.17 m // min. 5 m long microwave tunnel with four, depending on the degree of drying of the material, differently adapted feed points with a total power consumption of approx. 8.5 kW, through which the air heated to 40 to 45 ° C is led from the heat exchangers of the microwave generators. The resulting abrasion-resistant coating of the measuring head housing has a thickness of 250 µm, a water content of 12% by mass and shows no discoloration as a result of the heat treatment.
Für die Herstellung von Schuheinlagematerial gegen Schweißfüße wird auf ein 3,5mm dickes Baumwollgewebe, das mit einer 0,05M Calciumchloridlösung getränkt ist, eine wäßrige hochviscose Lösung, die 2 Gew.-% Carboxymethylcellulose, 5 Masse% Alginsäure, 10 Masse% Guar gum, 2 Masse% Natriumhyaluronat, 0,05 Masse% Aluminiumstearat, 0,01 Masse% Isodorant® und 1mM Phosphatpuffer enthält, in Form einer 8mm dicken Schicht aufgerakelt und bei einer Durchlaufgeschwindigkeit von 0,25m/min. im Mikrowellentunnel nach Beispiel 1 getrocknet. Der Restwassergehalt des beschichteten Baumwollgewebes beträgt 5,5 Masse%.For the production of shoe insert material against sweaty feet is on a 3.5mm thick cotton fabric soaked in a 0.05M calcium chloride solution is an aqueous highly viscous solution containing 2% by weight carboxymethyl cellulose, 5 Mass% alginic acid, 10 mass% guar gum, 2 mass% sodium hyaluronate, 0.05 Mass% aluminum stearate, 0.01 mass% Isodorant® and 1mM phosphate buffer contains, doctored in the form of an 8mm thick layer and at one Throughput speed of 0.25m / min. in the microwave tunnel according to example 1 dried. The residual water content of the coated cotton fabric is 5.5 Dimensions%.
Auf das Teflon-beschichtete Transportband des Mikrowellentunnels nach Beispiel 1 wird eine 5% Lösung von Hyalursäurebenzylester (Molmassen-Gewichtsmittel durch GPC-Analyse 2,8×106) aufgebracht und nach Durchlaufen des Mikrowellentunnels mit 0,08 m/min als 750 µm-Folie mit einem Restwassergehalt von 8,5% abgeschält.A 5% solution of hyaluronic acid benzyl ester (molar mass weight average by GPC analysis 2.8 × 10 6 ) is applied to the Teflon-coated conveyor belt of the microwave tunnel according to Example 1 and, after passing through the microwave tunnel at 0.08 m / min, as 750 μm Peeled off film with a residual water content of 8.5%.
Die GPC-Analyse der abgeschälten Folie ergibt ein Molmassen-Gewichtsmittel des getrockneten Hyalursäurebenzylesters von 2,4×106.GPC analysis of the peeled-off film gives a weight-average molecular weight of the dried hyaluric acid benzyl ester of 2.4 × 10 6 .
Auf die innere Grundfläche von Zellkulturflaschen aus Polyethylen (Durchmesser 75 mm) werden 0,5 ml/cm2 einer Natriumhyaluronatlösung aufgegeben und durch eine Rütteleinrichtung gleichmäßig verteilt. Die Zellkulturflaschen durchlaufen mit 0, 55m/ min den Mikrowellentunnel nach Beispiel 1 und nachfolgend eine Sterilisations- und Verpackungsstation. Die Analyse der in den Zellkulturflaschen durch die Mikro welleneinwirkung getrockneten Natriumhyaluratbeschichtung ergibt einen Wassergehalt von 16,5 Masse%. Die Flaschen werden zur Züchtung von Zell kulturen, insbesondere zur Züchtung von Keratinozyten, eingesetzt.0.5 ml / cm 2 of a sodium hyaluronate solution are applied to the inner base of cell culture bottles made of polyethylene (diameter 75 mm) and distributed evenly by a vibrating device. The cell culture bottles pass at 0.55 m / min through the microwave tunnel according to Example 1 and subsequently through a sterilization and packaging station. The analysis of the sodium hyalurate coating dried in the cell culture bottles by the action of microwaves shows a water content of 16.5% by mass. The bottles are used for the cultivation of cell cultures, in particular for the cultivation of keratinocytes.
Claims (10)
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| Application Number | Priority Date | Filing Date | Title |
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| DE1997112708 DE19712708A1 (en) | 1997-03-26 | 1997-03-26 | Dried hydrocolloid or hydrogel based on polysaccharide(s) |
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