WO2001089588A1 - Sterilisation de preparations de silicone - Google Patents

Sterilisation de preparations de silicone Download PDF

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Publication number
WO2001089588A1
WO2001089588A1 PCT/JP2001/004203 JP0104203W WO0189588A1 WO 2001089588 A1 WO2001089588 A1 WO 2001089588A1 JP 0104203 W JP0104203 W JP 0104203W WO 0189588 A1 WO0189588 A1 WO 0189588A1
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Prior art keywords
raw material
silicone raw
silicone
pressure steam
sterilization
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PCT/JP2001/004203
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English (en)
Inventor
Masako Kajihara
Toshihiko Sugie
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Sumitomo Pharmaceuticals Company, Limited
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Publication date
Application filed by Sumitomo Pharmaceuticals Company, Limited filed Critical Sumitomo Pharmaceuticals Company, Limited
Priority to AU2001258785A priority Critical patent/AU2001258785A1/en
Priority to JP2001585829A priority patent/JP2003534054A/ja
Publication of WO2001089588A1 publication Critical patent/WO2001089588A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04—Polysiloxanes
    • C08G77/32—Post-polymerisation treatment
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
    • A61L2/04—Heat
    • A61L2/06—Hot gas
    • A61L2/07—Steam

Definitions

  • This invention relates to a process for sterilizing a silicone raw material for producing silicone preparations.
  • a preparation to be administered to a living body directly e.g., intravenously, subcutaneously, intramuscularly or topically, is preferably administered in a sterilized, sterile state in view of safety reasons.
  • Most of such preparations are solutions, which can be sterilized by filtering.
  • Drug delivery systems being recently under development, on the other hand, have provided some solid preparations to be administered subcutaneously, intramuscularly, or topically into a living body. Methods for the sterilization of such solid preparations include a dry-heat sterilization, high-pressure steam sterilization, gaseous ethylene oxide sterilization, radiation irradiation, all of which are general sterilization methods for a solid product.
  • silicone preparations have been developed recently for use in implanting in a living body, and such preparations have been treated with a gaseous ethylene oxide sterilization to achieve sterilization.
  • gaseous ethylene oxide is much chemically reactive and is associated with problems such that it may react with an active ingredient.
  • Dry heat sterilization and high-pressure steam sterilization are hardly applicable to silicone preparations containing an active ingredient that is unstable to heat or is susceptible to steam.
  • radiation sterilization is so large in radiation energy that a substance sterilized by this method may be denaturated although it can be carried out at room temperature. According, this method has not been used widely as a sterilization for preparations containing an active ingredient. Under the circumstances, in order to produce sterile silicone preparations containing an active ingredient, of which the stability and properties may be widely varied, it is necessary to sterilize the active ingredient and silicone raw material separately, prior to mixing and curing.
  • Silicone raw material for producing silicone preparations is composed of Component group I that contains organopolysiloxane as a primary agent, a filler, a curing catalyzer etc., and Component group II that contains organopolysiloxane as a primary agent, a filler, a crosslinking agent, etc. By mixing these two Components, the curing reaction is proceeded to give an elastomer. Both Components cannot be sterile-filtrated as they are either highly viscous liquid or in a slimelike state. Silicone raw material has not been investigated for a sterilizing method therefor and its thermal stability.
  • the present inventors investigated to find that the silicone raw material deteriorates when exposed to high temperature for a long time, thus loosing its utility. Further, any method for sterilizing up to the deep inner part of such silicone raw material that is very viscous highly liquids or in slime state has been also unknown.
  • the present invention provides a process for sterilizing a silicone raw material up to the inner part without inducing deterioration of the silicone raw material for producing a silicone preparation containing an unstable active ingredient.
  • silicone preparations can be prepared by sterilizing a silicone raw material for producing the preparation using a high-pressure steam sterilization to give a sterile silicone raw material, followed by mixing it with an active ingredient, additives, or the like each of which has been separately sterilized, and curing the mixture.
  • a high-pressure steam sterilization to give a sterile silicone raw material
  • the present invention relates to:
  • a process for sterilizing a silicone raw material for producing a silicone preparation which comprises a step of conducting a high-pressure steam sterilization on the silicone raw material prior to curing;
  • a silicone preparation containing an active ingredient which preparation is produced from a silicone raw material sterilized by the process according to ( 1), (2), (3), (4), (5), (6) or (7);
  • a process for sterilizing a silicone raw material by a high- pressure steam sterilization method which comprises: a. a step of shaping a silicone raw material into a sheet form, and b. a step of sterilizing the sheet in a high-pressure steam sterilization apparatus;
  • a process for sterilizing a silicone raw material by a high- pressure steam sterilization method which comprises: a. a step of shaping a silicone raw material into a sheet form, and b. a step of putting the silicone raw material of a sheet form in a sterilizing bag, c. a step of sterilizing it in a high-pressure steam sterilization apparatus;
  • a process for sterilizing a silicone raw material by a high- pressure steam sterilization method which comprises: a. a step of shaping a silicone raw material into a sheet form having a thickness of about 10 mm or less, b. a step of putting the silicone raw material of a sheet form in a sterilizing bag, c. a step of sterilizing it in a high-pressure steam sterilization apparatus;
  • a process for sterilizing a silicone raw material by a high- pressure steam sterilization method which comprises: a. a step of shaping the silicone raw material into a sheet form having a thickness of about 5 mm or less, b. a step of putting the silicone raw material of a sheet form in a sterilizing bag, c. a step of sterilizing it in a high-pressure steam sterilization apparatus;
  • a process for sterilizing a silicone raw material by a high- pressure steam sterilization method which comprises: a. a step of shaping the silicone raw material into a sheet form having a thickness of about 10 mm or less, b. a step of putting the silicone raw material of a sheet form in a sterilizing bag, c. a step of sterilizing at a temperature ranging from about 115 °C to about 135 °C for from about 30 minutes to about 24 hours by generating or introducing a saturated steam at a pressure of from about 0.7 to about 2.2 kgf/cm 2 in a high-pressure steam sterilization apparatus.
  • a process for sterilizing a silicone raw material by a high- pressure steam sterilization method which comprises: a. step of shaping the silicone raw material into a sheet form having a thickness of about 5 mm or less, b. a step of putting a biological indicator on the center of said sheet, followed by folding said sheet at a thickness of about 10 mm or less, c. a step of putting the folded sheet in a sterilizing bag, d. a step of sterilizing at a temperature ranging from about 115 °C to about 135 °C for from about 30 minutes to about 24 hours by generating or introducing a saturated steam at a pressure of from about 0.7 to about 2.2 kgf/cm 2 in a high-pressure steam sterilization apparatus.
  • a process for sterilizing a silicone raw material by a high- pressure steam sterilization method which comprises: a. a step of shaping the silicone raw material into a sheet form having a thickness of about 5 mm or less, b. a step of putting a biological indicator of 10 6 on the center of said sheet, followed by folding said sheet at a thickness of about 10 mm or less, c. a step of putting the folded sheet in a sterilizing bag, d. a step of sterilizing at a temperature ranging from about 115 °C to about 135 °C for from about 30 minutes to about 24 hours by generating or introducing a saturated steam at a pressure of from about 0.7 to about 2.2 kgf/cm 2 in a high-pressure steam sterilization apparatus.
  • a process for sterilizing a silicone raw material by a high- pressure steam sterilization method which comprises: a. a step of shaping the silicone raw material into a sheet form having a thickness of about 5 mm or less, b. a step of putting Bacillus Stearothermophilus as a biological indicator on the center of said sheet, followed by folding said sheet at a thickness of about 10 mm or less, c. a step of putting the folded sheet in a sterilizing bag, d.
  • a process for sterilizing a silicone raw material by a high- pressure steam sterilization method which comprises: a. a step of shaping the silicone raw material into a sheet form having a thickness of about 5 mm or less, b. a step of putting Bacillus Stearothermophilus of 10 6 as a biological indicator on the center of said sheet, followed by folding said sheet at a thickness of about 10 mm or less, c. a step of putting the folded sheet in a sterilizing bag, d.
  • a process for sterilizing a silicone raw material by a high- pressure steam sterilization method which comprises: a. a step of shaping the silicone raw material into a sheet form having a thickness of about 5 mm or less, b. a step of putting Bacillus Stearothermophilus of 10 6 as a biological indicator on the center of said sheet, followed by folding said sheet at a thickness of about 10 mm or less, c. a step of putting the folded sheet in a sterilizing bag, d.
  • a process for sterilizing a silicone raw material by a high- pressure steam sterilization method which comprises: a. a step of shaping the silicone raw material into a sheet form having a thickness of about 5 mm or less, b. a step of putting Bacillus Stearothermophilus of 10 6 as a biological indicator on the center of said sheet, followed by folding said sheet at a thickness of about 10 mm or less, c. a step of putting the folded sheet in a sterilizing bag, d.
  • Silicone raw material is not limited to a particular species as long as it forms a gummy substance by curing, and preferably it is of an addition-polymerizable type caused by catalytic action of a platinum compound.
  • it is a millable type or a two component LTV (Low Temperature Vulcanizing), and, most preferably, it is SILASTIC (registered trade mark) medical grade ETR elastomer Q7- 4750, or Dow Corning (registered trade mark) MDX-4-4210 medical grade elastomer, or the like.
  • SILASTIC registered trade mark
  • ETR elastomer Q7- 4750 or Dow Corning (registered trade mark) MDX-4-4210 medical grade elastomer, or the like.
  • Active ingredients include, but are not limited to, a low molecular weight compound, a peptide, a protein, a glycoprotein, a polysaccharide, a toxoid useful as a vaccine, an antigen, an antibody, a gene, a virus, or the like.
  • low molecular weight compounds include, but not limited to, antibiotics such as avermectin, ivermectin, spiramycin, ceftiofur, mero- penem, phosphomycin; antibacterial such as amoxicillin, erythromycin, oxy- tetracyclin, lincomycin; antiinflammatory agents such as dexametazone, phenyl- butazone; hormones such as levothyroxine; adrenocortical steroids such as dexametazone palmitate, triamcinolone acetonide, halopredone acetate; nonsteroidal antiinflammatory agents such as indometacin, aspirin; arterial occlusion drugs such as prostaglandin El; anticancer agents such as actinomycin, daunomycin, bleomycin, mitomycin, fluorouracil, peplomycin, hydroxyurea, neocarzinostatin, sizofiran, estra-
  • cytokines such as an interferon, an interleukin
  • hematopoietic factors such as a colony stimulating factor, an erythropoietin
  • hormones such as a growth hormone, a growth hormone releasing factor, a calcitonin, a lutenizing hormone, a lutenizing hormone releasing hormone, an insulin
  • growth factors such as a somatomedin, a nerve growth factor, a neurotrophic factor, a fibroblast growth factor, a hepatocyte growth factor
  • cell adhesive factor such as an immunosuppressive agent
  • enzymes such as an asparaginase, a superoxide dismutase, a tissue plasminogen activating factor, an urokinase, a prourokinase
  • a bone metabolism related proteins such as BMP (Bone Morphogenetic Protein); antigens; antibodies; and the like
  • the active ingredient includes not only those exhibiting therapeutic effect by themselves, but also those showing physiological activity or those assisting or inducing physiological activity.
  • Such active ingredients include, for example, adjuvants used in vaccine as typified by saponin.
  • a vaccine may be comprised in the preparation so as to prepare a sustained-release formulation containing the vaccine.
  • Active ingredient can be used solely or together with other several active ingredients depending on the disease or route of administration.
  • An additive can be comprised if required for the purpose of stabilizing an active ingredient or of controlling the release of an active ingredient.
  • the additive shall be pharmaceutically acceptable and include, but not limited to, a salt such as sodium chloride, sodium citrate; an amino acid such as glycine, alanin, sodium glutamate; a carbohydrate such as lactose, mannitol; a protein such as gelatin, collagen, albumin; a synthetic polymer such as polyethylene glycol; and a surface active agent such as sodium laurylsulfate, sodium deoxycholate.
  • a salt such as sodium chloride, sodium citrate
  • an amino acid such as glycine, alanin, sodium glutamate
  • a carbohydrate such as lactose, mannitol
  • a protein such as gelatin, collagen, albumin
  • a synthetic polymer such as polyethylene glycol
  • a surface active agent such as sodium laurylsulfate, sodium deoxycholate.
  • the process and the silicone raw material of the present invention are applicable for producing any preparation having various shape, construction, or composition.
  • Such preparations include those as disclosed in Japanese Patent Nos. 2033056 and 2056085; and Japanese Patent application Nos. 331467/ 1993, 256170/ 1998, 148591/ 1998, 155343/ 1998 and 319108/ 1999.
  • Step 1 Sterilization
  • Silicone raw material can be shaped in any form that allows infiltration of steam required for sterilization into the inner part. It may preferably be processed to give a shape in which the distance from the surface exposed to external environment through the deepest part is 5 mm or less, and more preferably the distance is 2.5 mm or less.
  • the silicone raw material is processed to give a sheet form using a roll or press machine.
  • the thickness of the sheet is not limited as far as it allows infiltration of a steam into the inner part necessary for sterilization. It is preferably 10 mm or less, more preferably 5 mm or less.
  • an insection can be made at an appropriate spacing to form a path for passing the steam.
  • the appropriate spacing is not limited as far as it allows infiltration of the steam necessary for sterilization into all part of the block. It is preferably 10 mm or less, more preferably 5 mm or less.
  • the silicone raw material thus processed is packaged in a sterilizing bag, sealed it, and the bag is placed in a high-pressure steam sterilization apparatus.
  • the sterilizing bag refers to a packing material for sterilization that is used for the purpose of blocking penetration of microorganisms to keep a sterile condition after sterilization, and includes for example those made of paper or paper film for a high- pressure steam sterilization.
  • Temperature for sterilization is an appropriate temperature ranging from about 115 to about 135°C, preferably from about 120 - about 125 °C, and more preferably about 121 °C.
  • the pressure in a high-pressure steam sterilization apparatus can be from about 0.7 to about 2.2 kgf/cm 2 .
  • Retention time after reaching a sterilizing temperature is set depending on the temperature, the thickness of silicone raw material, or the spacing of insection.
  • it is preferably from about 30 minutes to about 24 hours, more preferably from about 30 minutes to about 12 hours, most preferably from about 30 minutes to about four hours.
  • it is preferably from about 15 minutes to about 12 hours, more preferably from about 15 minutes to about eight hours, most preferably from about 15 minutes to about four hours.
  • At about 135 °C for example, it is preferably from about three minutes to about three hours, more preferably from about three minutes to about two hours, most preferably from about three minutes to about one hour.
  • the thickness of silicone raw material and the spacing of insection are constant, higher the sterilizing temperature, shorter the retention time.
  • the thickness of silicone raw material or the spacing of insection is larger, a higher sterilization temperature and/or a longer retention time is necessary.
  • Successful sterilization can be checked, for example, as follows:
  • a suitable biological indicator (herein after called BI.
  • BI Bacillus stearothermophilus
  • 10 6 Bacillus stearothermophilus is usually used as BI
  • the BI is then taken out and incubated under an appropriate condition to check negative results.
  • SCD soybean casein digestive
  • Sterile silicone preparation is produced by mixing the silicone raw material sterilized as shown in Step 1 , a sterilized powder containing an active ingredient, and optionally a sterilized powder of additives, etc, shaping the mixture, and curing the same.
  • the powder containing a sterilized active ingredient may be a powder comprising only an active ingredient, or a mixed powder containing an active ingredient and additive(s), or may be a homogeneous solid containing an active ingredient and additive(s).
  • the sterilized powder containing an active ingredient can be produced by preparing a homogeneous solution of an active ingredient and additive(s), sterile filtering, and drying the solution to obtain a solid, followed by optionally powdering the solid and/or sieving.
  • the drying can be done in conventional methods including as representatives flow drying using nitrogen, helium or air, vacuum drying, air drying, granulation, spray drying using spray dryer, or the like or a combination of them. These procedures are carried out under a sterile condition using a sterilized appliance and apparatus.
  • the powder comprising only an active ingredient and the additive(s) may be also produced by a method similar to above one. Others include a method in which the production is conducted under a sterile condition from the beginning, a method in which the material at first is powdered before subjected to sterilization under dry heat or radiation, etc.
  • a silicone preparation having a single layer structure can be produced by mixing homogeneously a sterile silicone raw material, a sterile powder containing an active ingredient, and optionally a sterile powder of additive(s) with a kneader, a two-roll mill, etc., extruding the mixture through a nozzle to give a shape, and curing the same at 10 °C to 200 °C, which temperature depends on stability or property of the active agent and additive(s). All of the procedures are carried out under a sterile condition.
  • each layer can be produced separately or at the same time.
  • the following methods can be used, but are not restrictive: a method in which an inner layer in a stick form is prepared, then coated with a solution of an outer layer substance, and the material is dried; a method in which an inner layer produced separately is inserted into a tube prepared from an outer layer substance; a method in which an inner layer is shaped within a tube prepared from an outer layer substance; a method in which an inner layer and an outer layer are extruded at the same time using a nozzle to give a shape.
  • the stick composition thus prepared may be cut in an appropriate length to give a desired preparation. Examples
  • SILASTIC (registered trade mark) medical grade ETR elastomer Q7-4750 Component A (containing a primary agent organopolysiloxane, a filler and a curing catalyst) ( 12.5 g) was shaped to a sheet using a two-roll mill so that the thickness was adjusted to 5 mm.
  • SILASTIC (registered trade mark) medical grade ETR elastomer Q7- 4750 Component A (12.5 g) was shaped to a sheet using a two-roll mill so that the thickness was adjusted to about 2.5 mm.
  • a BI ⁇ Bacillus stearothermophilus 10 6 ATCC No.
  • Component B- 1 (containing a primary agent organopolysiloxane, a filler, a crosslinking agent, and a curing inhibitor) was also sterilized to obtain a sterilized silicone raw material, Component B- 1.
  • Untreated BI-3 was prepared for a reference. These Bis were incubated in SCD medium at 55° C - 60° C for seven days and assayed.
  • SILASTIC (registered trade mark) medical grade ETR elastomer Q7-4750 Component A (25 g) was shaped to a sheet using a two-roll mill so that the thickness was adjusted to 10 mm.
  • SILASTIC (registered trade mark) medical grade ETR elastomer Q7- 4750 Component A (25 g) was shaped to a sheet, using a two-roll mill.
  • a BI Bactus stearothermophilus 10 6 , ATCC No.
  • SILASTIC (registered trade mark) medical grade ETR elastomer Q7-4750 Component A (12.5 g) was shaped to a sheet, using a two-roll mill so that the thickness was adjusted to 5 mm.
  • SILASTIC (registered trade mark) medical grade ETR elastomer Q7- 4750 Component A (12.5 g) was shaped to a sheet, using a two-roll mill.
  • a BI Bactus stearothermophilus 10 6 , ATCC No.
  • SILASTIC (registered trade mark) medical grade ETR elastomer Q7-4750 Component A (12.5 g) was shaped to a sheet using a two-roll mill so that the thickness was adjusted to 5 mm.
  • SILASTIC (registered trade mark) medical grade ETR elastomer Q7- 4750 Component A ( 12.5 g) was shaped to a sheet, using a two-roll mill.
  • a BI Bactus stearothermophilus 10 6 , ATCC No.
  • SILASTIC (registered trade mark) medical grade ETR elastomer Q7-4750 Component A (10 g) was shaped to a sheet using a two-roll mill so that the thickness was adjusted to 10 mm. This is enclosed in a Tetoron sheet, packed in a sterile bag, and placed in a high- pressure steam sterilization apparatus (Auto high-pressure steam sterilizer personal clave HA-300 MIIC, Hirayama). The apparatus was set at 121 °C and 240 minutes, and the sterilization was carried out. After sterilizing, the samples were taken out and dried to obtain a silicone raw material, Component A-5. Similarly, SILASTIC (registered trade mark) medical grade ETR elastomer Q7-4750, Component B was also sterilized to obtain a sterilized silicone raw material, Component B-5. Experiment 5
  • Example 6 SILASTIC (registered trade mark) medical grade ETR elastomer Q7-4750, Component A (5 g) was shaped to a sheet using a two-roll mill so that the thickness was adjusted to 5 mm. This is enclosed in a Tetoron sheet, packed in a sterile bag, and placed in a high- pressure steam sterilization apparatus (Auto high-pressure steam sterilizer personal clave HA-300 MIIC, Hirayama). The apparatus was set at 123 °C and 80 minutes, and the sterilization was carried out.
  • SILASTIC registered trade mark
  • ETR elastomer Q7-4750 Component A
  • the sterilized silicone raw material, Component A-6 ( 1 g) and the sterilized silicone raw material, Component B-6 ( 1 g) were mixed and the mixture was extruded through a nozzle of 0.5 mm diameter.
  • Separately non- sterilized silicone raw materials, Component A ( 1 g) and Component B ( 1 g) were mixed and the mixture was extruded through a nozzle of 0.5 mm diameter.
  • These extruded rods of the products were allowed to stand for five days at 25 °C to cure.
  • the cured rods were cut to give pieces having a length of 5 cm and tensile test was conducted on the pieces (EZ-test, Shimadzu) to determine their tensile stress (stress at 300% extension).
  • Human serum albumin powder (0.6 g) was dissolved in an aqueous solution of interferon ( 100 MU/mL, 347 mL) and the solution was sterile filtered using a 0.22 ⁇ m filter, and lyophilized under a sterile condition. The following procedures were all carried out using sterile appliances under a sterilized environment. The lyophilized cake was powdered to give Powder 1. Sterilized silicone raw material, Component A- l (0.35 g) and sterilized silicone raw material, Component B- l (0.35 g) were mixed together. Immediately after the mixing, Powder 1 (0.3 g) was kneaded within the mixture. The kneaded material was extruded through a nozzle of diameter 2 mm by pressure and was allowed to stand for three days at 25 °C to cure. The product was cut to give a sterile silicone preparation.
  • SILASTIC (registered trade mark) medical grade ETR elastomer Q7-4750 Component A ( 10 g) was shaped to a sheet using a two-roll mill so that the thickness was adjusted to 5 mm. Each sample was heated at 180°C for one hour or 135° C for five hours to obtain Reference silicone raw materials, Components A-7 and A-8. In a similar manner, SILASTIC (registered trade mark) medical grade ETR elastomer Q7-4750, Component B ( 10 g) was heated to obtain Reference silicone raw materials, Components B-l and B-2. Experiment 8
  • Reference silicone raw materials, Components A-7 and A-8, Reference silicone raw materials, Components B-l and B-2, and untreated silicone raw materials, Components A and B were masticated using a two-roll mill. Usually, mastication with a two-roll mill improves plasticity. However, when the silicone raw materials are deteriorated, the masticated materials lose their plasticity and become brittle. The characters of each sample after mastication were compared.
  • corch is referred to as a state where a curing develops to some extent that a process for shaping a material cannot be done.
  • the present invention provides a sterile silicone raw material.
  • the invention enables to produce a sterile silicone preparation containing any active ingredient, irrespective of stability of the active ingredient that would be affected under various sterilization conditions.

Abstract

L'invention concerne un procédé de production de préparations stériles de silicone, qui consiste à stériliser une matière brute de silicone, avant durcissement, selon un procédé de stérilisation à vapeur haute pression.
PCT/JP2001/004203 2000-05-25 2001-05-21 Sterilisation de preparations de silicone WO2001089588A1 (fr)

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AU2001258785A AU2001258785A1 (en) 2000-05-25 2001-05-21 Sterilization of silicone preparations
JP2001585829A JP2003534054A (ja) 2000-05-25 2001-05-21 シリコーン製剤の滅菌方法

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JP2000154721 2000-05-25
JP2000-154721 2000-05-25

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EP1857123A1 (fr) * 2006-05-15 2007-11-21 Kettenbach GmbH & CO. KG Procédé de stérilisation des matériaux d'empreinte et matériaux d'empreinte stérilisables
US7592377B2 (en) 2003-05-16 2009-09-22 Zhermack S.P.A. Radiopaque and aseptic material for impression-taking
EP2643027A1 (fr) 2010-11-25 2013-10-02 Smith & Nephew, PLC Compositions i-i et produits et utilisations de celles-ci
US10537657B2 (en) 2010-11-25 2020-01-21 Smith & Nephew Plc Composition I-II and products and uses thereof
CN113878895A (zh) * 2021-09-15 2022-01-04 河北景港橡塑科技有限公司 橡胶塑料配件生产制造工艺
US11638666B2 (en) 2011-11-25 2023-05-02 Smith & Nephew Plc Composition, apparatus, kit and method and uses thereof
US11931226B2 (en) 2013-03-15 2024-03-19 Smith & Nephew Plc Wound dressing sealant and use thereof

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