US3810473A - Liquid-laid, non-woven, fibrous collagen derived surgical web having hemostatic and wound sealing properties - Google Patents

Liquid-laid, non-woven, fibrous collagen derived surgical web having hemostatic and wound sealing properties Download PDF

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Publication number
US3810473A
US3810473A US00312210A US31221072A US3810473A US 3810473 A US3810473 A US 3810473A US 00312210 A US00312210 A US 00312210A US 31221072 A US31221072 A US 31221072A US 3810473 A US3810473 A US 3810473A
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Prior art keywords
fibers
mesh screen
water
volumes
web
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US00312210A
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M Cruz
C Cirolla
O Battista
L Tressler
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Alcon Puerto Rico Inc
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Avicon Inc
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Priority to US00312210A priority Critical patent/US3810473A/en
Priority to GB5528273A priority patent/GB1426198A/en
Priority to CA186,862A priority patent/CA1020462A/en
Priority to DE2359949A priority patent/DE2359949C3/de
Priority to FR7343057A priority patent/FR2281745A1/fr
Priority to JP13598973A priority patent/JPS5436641B2/ja
Priority to IT54111/73A priority patent/IT1016029B/it
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Assigned to ALCON (PUERTO RICO) INC. reassignment ALCON (PUERTO RICO) INC. CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: AVICON, INC.
Assigned to SIGNAL CAPITAL EQUITIES, INC., A DE. CORP. reassignment SIGNAL CAPITAL EQUITIES, INC., A DE. CORP. SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MEDCHEM PRODUCTS, INC.
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00—Bandages or dressings; Absorbent pads
    • A61F13/02—Adhesive plasters or dressings
    • A61F13/0276—Apparatus or processes for manufacturing adhesive dressings or bandages
    • A61F13/0289—Apparatus or processes for manufacturing adhesive dressings or bandages manufacturing of adhesive dressings
    • A61F13/01034—
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00—Bandages or dressings; Absorbent pads
    • A61F13/02—Adhesive plasters or dressings
    • A61F13/0203—Adhesive plasters or dressings having a fluid handling member
    • A61F13/0223—Adhesive plasters or dressings having a fluid handling member characterized by parametric properties of the fluid handling layer, e.g. absorbency, wicking capacity, liquid distribution
    • 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
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
    • A61L15/32—Proteins, polypeptides; Degradation products or derivatives thereof, e.g. albumin, collagen, fibrin, gelatin
    • A61L15/325—Collagen
    • 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
    • A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42—Use of materials characterised by their function or physical properties
    • A61L15/58—Adhesives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00—Bandages or dressings; Absorbent pads
    • A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
    • A61F13/84—Accessories, not otherwise provided for, for absorbent pads
    • A61F13/8405—Additives, e.g. for odour, disinfectant or pH control
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00—Bandages or dressings; Absorbent pads
    • A61F2013/00089—Wound bandages
    • A61F2013/00217—Wound bandages not adhering to the wound
    • A61F2013/00221—Wound bandages not adhering to the wound biodegradable, non-irritating
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00—Bandages or dressings; Absorbent pads
    • A61F2013/00361—Plasters
    • A61F2013/00365—Plasters use
    • A61F2013/00463—Plasters use haemostatic
    • A61F2013/00472—Plasters use haemostatic with chemical means
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00—Bandages or dressings; Absorbent pads
    • A61F2013/00361—Plasters
    • A61F2013/00727—Plasters means for wound humidity control
    • A61F2013/00731—Plasters means for wound humidity control with absorbing pads
    • A61F2013/00744—Plasters means for wound humidity control with absorbing pads containing non-woven
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61F—FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F13/00—Bandages or dressings; Absorbent pads
    • A61F13/15—Absorbent pads, e.g. sanitary towels, swabs or tampons for external or internal application to the body; Supporting or fastening means therefor; Tampon applicators
    • A61F13/15577—Apparatus or processes for manufacturing
    • A61F2013/15821—Apparatus or processes for manufacturing characterized by the apparatus for manufacturing
    • 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
    • A61L2400/00—Materials characterised by their function or physical properties
    • A61L2400/04—Materials for stopping bleeding
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S128/00—Surgery
    • Y10S128/08—Collagen

Definitions

  • the hemostat-adhesive material is in a fluffy, finely-divided fibrous form and the form for use in this invention consists essentially of a water-insoluble, ionizable, partial salt of collagen, the fibrous mass having a density of not more than about 8 pounds per cubic foot, preferably the bulk density is between 1.5 and 6.0 pounds per cubic foot.
  • the mass when combinedwith blood in a wound forms a mass that is self-adherent to the tissue surfaces and will seal the wound without the use of sutures.
  • the partial salt of collagen consists essentially of an ionizable, water-insoluble, partial acid salt of collagen consisting from about 5 percent to about 90 percent of the theoretical stoichiometric amount of the ionizable acid.
  • the fluffy, finely-divided fibers for use in the present invention may be prepared as described in the aforementioned application.
  • the fluffy, finely divided fibrous collagen product may be converted into non-woven webs by a wet method such as commonly employed in forming papers. It is also stated that in such method the fibrous collagen is slurried in a water-miscible organic liquid of the type used in producing the fibrous collagen.
  • waterlaid fibrous sheets or webs formed from such fibers are harsh and boardy and parchment-like in structure with complete loss of hemostatic and adhesive properties thereby rendering such sheets unsatisfactory for surgical purposes.
  • the principal purpose of the present invention is to provide a liquid-laid, non-woven web which retains the hemostatic-adhesive properties of the fluffy, fibrous partial salt of collagen.
  • a further purpose of the invention is to provide a method of forming the liquid-laid, non-woven sheet or web of the fluffy, finely-dividedfibrous collagen derived product which is flexible, non-flaking, and has sufficient strength to permit its application to a wound without separation into individual fibers.
  • a further purpose of the present invention is to provide a method of forming a liquid-laid, non-woven fibrous web of the finely-divided fibrous collagen derived product which retains the hemostatic and unique adhesive properties of a finely-divided fibrous mass as described in the aforementioned application.
  • the present invention is based upon the discovery that non-woven webs or sheets which retain the hemostatic and unique adhesiveproperties of the fluffy, finely-divided fibers of the'partial'salt of collagen, can be In the drawings:
  • FIG. 1 is a graph illustrating the freeness of the fibers when-slurried in ethanol and ethanol-water mixtures of varying composition
  • FIGS. 2 through 7 are graphs illustrating the variations in the physical properties of theliquid-laid, nonwoven sheets orwebs prepared from slurries of the fibers in ethanol and ethanol-water mixtures of varying composition.
  • the slurrying liquid consists-of a mixture having a composition, by volume, in the range of from 95 percent organic liquid and 5 percent water to about percent organic liquid and 15 percent water.
  • the amount of water is less than about 5 volumes of water to volumes of the organic liquid, the finished product is unsatisfactory in that it has no dry web strength and is extremely flaky; that is, upon handling, fibers readily separate from the sheet. At least this minimum amount of v water must be present so as to provide a sufficient degree of bonding between the fibers to form a coherent and handleable sheet.
  • the amount of water preferably should not exceed about 15 volumes of water to 85 volumes of organic liquid, preferably 95 volumes of organic liquid and 5 volumes of water. if the amount of water exceeds this ratio, the fibers become so firmly bonded together that there is a loss in absorbency and flexibility and a marked loss of the hemostatic and adhesive properties of the sheet.
  • the liquid may consist of up to about 20 volumes of water to 80 volumes of organic liquid, preferably 90 volumes of organic liquid and volumes of water.
  • the amount of water exceeds this value there is a loss in the desired properties.
  • the water-miscible organic liquid consists of low molecular weight alcohols, ketones and the like such as, for example, methanol, ethanol, isopropanol, amyl alcohol, methylethyl ketone, acetone, and mixtures of these organic liquids. It is possible to increase the amount of water providing that a salt which hydrates is present such as sodium sulfate and calcium chloride.
  • a salt which hydrates is present such as sodium sulfate and calcium chloride.
  • the use of the organic liquids other than ethanol is feasible, however, where the product is intended for surgical uses it is essential that the product be freed of such solvent.
  • the fibrous collagen product can be prepared from any undenatured collagen in the natural state or delimed edible forms of collagen including, for example, hide, gut, tendon, cartilage or other high fibrous collagen source material preferably chopped up for easier handling.
  • the collagen is preferably in a wet and never-dried state or, if dried, drying has been effected under conditions which minimize denaturation.
  • Satisfactory raw materials for the collagen include, for example, fresh cowhides and calfhides, salted down cowhides, wet moosehide, pigskins, sheepskins and goatskins as conventionally used for making leather. Special technical hide collagen prepared from hide splits and possessing a minimal reduced bacteria count is also satisfactory.
  • the preferred raw material because of availability is corium derived from never-dried cowhide or technical grades of collagen prepared from cowhide and other animal hides.
  • the wet collagen source material such as hide is diced or chopped into small fragments of from onefourth to one-half inch sizes in a cutting or grinding mill, such as, for example, an Urschel Mill.
  • a cutting or grinding mill such as, for example, an Urschel Mill.
  • these fragments may be mixed with crushed ice and then passed through the Urschel Mill with cutting heads of smaller dimension to fiberizethe collagen into a coarse fibrous product.
  • the wet or moist collagen source material is mechanically dispersed or slurried in an aqueous liquid which controls the swelling of the fibers.
  • the aqueous liquid comprises water and a water-miscible organic liquid such as low molecular weight alcohols, ketones, and the like, such as, for example, methanol, ethanol, isopropanol, methylethyl ketone, acetone and the like in a weight range of between about 90 percent of the organic liquid and 10 percent water and about 50 percent organic liquid and 50 percent water. Where the proportion of water is too high, the collagen fibers swell to such a great extent that they lose their fiber identity with an attendant densification during the subsequent drying step.
  • the bulk of the liquid is drained from the mass and the fibrous collagen slurried and washed with a watermiscible organic liquid such as the alcohol and again the bulk of the liquid is separated from the partially swollen wet collagen material.
  • a watermiscible organic liquid such as the alcohol
  • the collagen material is slurried in the organic liquid to reduce the water content to a minimum.
  • the use of three slurrying steps with the organic liquid will reduce the amount of water present to about 1 percent.
  • the organic liquid is removed as by centrifugation and final drying. Drying may be effected either by oven drying or vacuum drying as at, for example, 40C. under a 29 inch vacuum for about 16 hours. In general, this vacuum drying will reduce the volatile content to under 1 percent.
  • the partial acid salt of collagen is formed by incorporating the required amount of an ionizable acid in the aqueous liquid wherein the collagen is dispersed or slurried.
  • the amount of acid incorporated in the aqueous liquid is such as to provide the product with a bound acid content of from about 50 percent to 90 percent preferably about 60 percent to percent of the theoretical stoichiometric bound acid content.
  • the fibrous material Before the final deaggregation into constituent fibers or fluffing operation to produce the product having the required bulk density, the fibrous material is preferably conditioned to contain about 8 percent to l5 percent volatiles. This conditioning may be readily effected by allowing the product to remain at normal atmospheric temperatures and humidities (for example, 70 75F., 40% 60% R.H.) for from about 8 to 24 hours.
  • the final fiber deaggregation or fluffing operation is necessary to provide the requisite bulk density. This operation is an opening operation whereby the diced material is converted into bundles of individual fibers.
  • the final fiber deaggregation or fluffing operation does not separate all of the dried bundles into ultimate individual fibrils but the product does contain finer fiber bundles (smaller in diameter) as compared to the coarser fiber bundles obtained at the end of the drying and conditioning operations.
  • This deaggregation or tluffing may be effected by apparatus such as a hammer mill type comminution mill such as a Fitz Mill.
  • the wet collagen source material is merely diced or chopped into small fragments as described hereinbefore and then introduced into and mixed in a water-miscible organic liquid such as ethanol or isopropanol. Mixing is continued for about 1 hour so as to permit thorough penetration of the organic liquid into the smallfragments. The bulk of the liquid is then separated as by draining or centrifuging and the recovered fragments again introduced into and mixed in the organic liquid for about 1 hour. Again, the bulk of the liquid is separated and the procedure repeated. At the end of this period, the liquid is centrifuged from the mixture and the wet fragments dried as by oven drying or vacuum drying. The resulting product, after conditioning as described above, is then subjected to a fiberizing and deaggregation or fluffing operation.
  • the desired amount of acid may be mixed with the organic liquid in any one of the above described steps, preferably .in the second step. in such instances, the
  • time of treatment with the organic liquid containingthe acid should be prolonged to permit the required reac- I ranges.
  • the effective-fiber lengths may be determined in accordance with TAPPI Standard Method T233 su-64 utilizing a McNett Classifier having four tanks provided with a 20 mesh screen (openings 840 microns), a 35 mesh screen (openings 500 microns), a 65 mesh screen (openings 230 microns) and a 150 mesh screen (openings 100 microns), respectively.
  • the partial salt fibers are converted to collagen fibers while preventing excessive swelling of the partial salt fibers.
  • Such conversion may be effected as by slurrying the partial salt fibers at a solids concentration of about 1 percent for about 30 minutes in a mixture of 90 volumes ethanol and 10 volumes water adjusted to and maintained at a pH of 10.5 by addition of ammonium hydroxide solution.
  • the fibers are recovered by the use utes to wash out soluble salt and the fibers recovered by the same type filtration.
  • the recovered fibers are then given two additional washes using 100 percent ethanol.
  • the finally recovered alcohol-wet fibers should not be allowed to dry but are slurried in the required volume of water at the recommended solids content for the specific classifier.
  • a measure of the fiuffiness and a rough indication of a satisfactory fiber length distribution of the fibers is bulk density.
  • the bulk density is measured by adding the fibrous collagen products as initially fluffedto a 100 ml. graduate cylinder without any compression step and deter-' mining the Weight of the added 100 mls. of the product.
  • hydrochloric acid is the preferred acid and is used in the examples which follow merely because it is relatively inexpensive and allows ready flexibility and ease of control.
  • Other ionizable acids both inorganic and ionizable organic acids, such as, for example, sulfuric acid, hydrobromic acid, phosphoric acid, cyanoacetic acid, acetic acid, citric acid and lactic acid are satisfactory.
  • Sulfuric acid for example, is satisfactory, but control of the action is difficult.
  • Citric acid may be substituted for hydrochloric acid with about equal results. Ease of control" has reference to the ability to arrest the swelling and hydrolysis of the collagen fibers so as to prevent the'rapid degradation of the material to a water-soluble product.
  • the fiber length distribution of the fibrous partial salt of collagen determined by the use of a McNett Classifier was about 48 percent retained on a 20 mesh screen 22 percent retained on a 35 mesh screen 3.6 percent retained on a 65 mesh screen 0.7 percent retained on a 150 mesh screen 25.7 percent passing a 150 mesh screen.
  • the bulk density of the fluffed, fibrous partial salt of collagen was 2.0 2.5 pounds per cubic foot.
  • a stable dispersion was formed having a pH of
  • conventional apparatus such as used in the papermaking industry and in the production of non-woven webs may be used.
  • the finelydivided, fibrous collagen product is slurried in the water-miscible organic liquid-water mixture by the use of a suitable mixing device such as a beater wherein the beater is used solely as a mixing device since the fibrous product does not require hydration or fibrillation.
  • the slurry or furnish may contain from about 0.1 percent to about 3 percent of the fibrous product, preferably about 0.5 percent.
  • the slurry or furnish is then passed to a suitable collecting screen where the fibrous product is sheeted or deposited. Fourd'rinier, cylinder vat, Rotoformer and other sheet forming devices are satisfactory. After removing the wet-laid sheet or web from the collecting screen, excess liquid may be removed by passing the sheet between press rolls and then drying the sheet.
  • the degree of swelling or hydration of the fibers in ethanol and ethanol-water mixtures is illustrated by a fr'eeness test using a Canadian Standard Freeness Tester.
  • the method of testing was in accord with TAPPl Standard Test Method T227 m-58. ln this series of tests, slurries containing 0.3% fibers were formed in ethanol and ethanol-water mixtures, as set forth in Table l, by adding the fibers to the liquid and manually agitating with a wide blade spatula for 5 minutes. 1,000 mls of the slurry were then poured into the cylinder of the Freeness Tester and measuring the volume ofliquid discharged from the side discharge tube. This volume in mls. is reported in Table 1 as CSF No. and the data illustrated in FIG. 1. This test illustrates that as the proportion of water in the slurrying liquid increases, the swelling of the fibers increases and, accordingly, the freeness decreases. 7
  • the variations in absorbency, tear strength, burst factor, tensile strength, stiffness as well as other properties of the he'mostatic-adhesive non-woven webs of the present invention may be illustrated by reference to the preparation of handsheets utilizing liquids varying in relative proportions of ethanol and water. 1n the preparation of these handsheets a modified 8 inch X 8 inch Williams handsheet mold was utilized. The normal wire mesh screen at the bottom of the handsheet mold was covered with a polypropylene filter fabric consisting of a 2/2 twill weave structure, the fabric having a porosity of 85-90 CFM (Chicopee Polypropylene 6016800 fabric) the edges of the fabric being sealed to the wire mesh.
  • CFM Chopee Polypropylene 6016800 fabric
  • the mold was then opened and the formed wet nonwoven web covered with a plain weave polypropylene filter fabric having a porosity of about CFM (Chicopee Polypropylene 6970500 fabric). Dry blotting paper was sandwiched between very fine Dacron cloths and then placed over the polypropylene fabric and gently pressed to absorb some of the liquid. This procedure with the sandwiched blotting paper was repeated a second time. A similar sandwich of dry blotting paper and Dacron'cloth' was then placed over the polypropylene fabric and the formingplate with the sandwiched wet laid web removed from the mold and gently placed upside down with the sandwiched blotting paper being placed on a sheet of polyester film.
  • CFM Chopee Polypropylene 6970500 fabric
  • the forming plate was then lifted and the wet laid web gently peeled from the polypropylene filter fabric covering the forming plate wire mesh.
  • the exposed side of the removed wet laid web was then covered with a polypropylene filter fabric (Chicopee Polypropylene 697050 fabric) and a sandwiched blotting paper between Dacron cloth placed over the fabric.
  • the assembly was then gently rolled with a printers rubber roller to remove additional liquid and this procedure repeated by rolling at 90 to the direction of the first rolling.
  • a dry sheet of sandwiched blotting paper was then applied after removal of the wetted sandwiched blotting paper and the assembly turned over and a dry sheet of sandwiched blotting paper placed on the upper side and the rolling procedure was repeated.
  • the sandwiched blotting paper and polypropylene filter fabrics were then removed and the wet laid web placed between polyester films and both sides gently rolled with a printers roller.
  • the wet-laid webs between polyester films were then stored in polyethylene bags until sufficient numbers of the sheets were prepared to subject them to a drying step using either a photographic dryer, freeze dryer, Noble and Wood hot plate or vacuum oven.
  • Model 40 with an initial shelf temperature of about 40C., a vacuum of 50 microns, heating cycle to 38"C. over a period of 2 hours and a condenser in'al fibers.
  • a Waring Blendor at high speed for 30 minutes formed dispersions having a pH of 3.22 which was substantially identical to the pH of dispersions formed from the orig-
  • the absorbency of freeze dried and vacuum dried products formed from the slurries in different compositions was determined by the use of a mixture of 90'volumes of ethanol and 10 volumes of water.
  • the central portions (1 1% inch in diameter) of plastic screw tops of 4 oz. jars were removed leaving a sufficient annular flange to cover the top edge of the jars.
  • Samples of the various non-woven sheets in the form of circular discs 2 inches in diameter were placed on the top edges of the jars and the cut screw tops placed on the jars to secure the circular discs on the jar tops.
  • the liquid was allowed to drip through a distance of one-half inch on to the center of the sheet drop by drop allowing each drop to be absorbed by the sheet before the succeeding of the original dry sample and the weight of the wetted sample, the data, the average for two samples, being presented in Table 1.
  • the data are plotted in FIG. 2.
  • the tensile strength of the various sheets was mea- 'sured-by the use of a Thwing-Albert electrohydraulic tensile tester Model No. 37-4 at a 5.5 Kg and 3 I .8'Kg loading.
  • TAPPI Standard Test Table I and plotted in FIG. 5 are the average values for two samples.
  • the stiffness of the sheets was measured by maintaining samples wrapped on a glass cylinder for 24 hours at room temperature (73F) and a relative humidity of about 50 percent and then releasing the samples and allowing them to flatten under their own weight.
  • the samples were cut into 3 in. X 7 in. strips. wrapped around a glass tube 2.25 in. in diameter and held in place by scotch tape.
  • the tube was placed on a horizontal surface with the mid portion of the sample sheet in contact with the horizontal surface.
  • the tape was then cut and the free ends of the samples allowed to separate from the glass tube and unfold or uncurl under their own weight. 'The amount of uncurling was determined by measuring the angle between the horizontal surface and the uncurled ends of the samples. The angle in degrees is termed-the Stiffness Factor, which is the average for four sheets, both ends, and is reported in Table 1 and plotted in- FIG, 6.
  • the porosities of the sheets were determined by the use of a Gurley Densometer (Closed-Top Model) in ac cordancewith TAPPI Standard Test Method T460 os-68. This test measures the air resistance of the sheets and is reported in Table l as the average time in seconds required to displace 100 ml. of air through an area of 6.45 sq.cm. ofthe paper. The reported values are averages for two to six tests. These data are plotted Method T220 m-60, the test was applied to six strips 30 in FIG. 7 and reported in Table 1.
  • the fibrous collagen products prepared in the above examples were employed in surgical test procedures 5 designed to provide the efficacy of the material both as a hemostat and adhesive for severed biological surfaces in a warm blooded animal when wet with blood.
  • Severed biological surfaces for the purposes of this invention includes cut, sliced, ripped, abraded, torn, punctured, burned, and tissue severed by any means or method whereby a fresh biological surface is present.
  • Biological surfaces will include tissue, cartrilage, vessels, bone or other normal organic parts of the warm blooded animal which may require mending or joining.
  • the investigators ratings of the samples based upon the evaluations and based upon the foregoing considerations are set forth in Table 2. in addition, the investigators also observed the handling characteristics of the samples. These characteristics included a consideration of the physical properties such as. cohesiveness and flakiness of the sheet, the friability, the stiffness and the ability to cut swatches of the required size from the sheet with scissors to form a clean cut. The investigators comments with respect to these characteristics are set forth in the Table 2.
  • hemostasis was effected within this time period. After 5 to minutes, removal of the excess outer marginal portions of the swatch was attempted by pulling off such portions. Subsequent to rating the swatch, it was forcibly removed and a uniformly bleeding lesion reestablished and another swatch placed over the lesion as described and the swatch rated.
  • the sample exhibited no hemostatic property, no adhesiveness to the wound surface and that the sample could not be delaminated; that is, excess marginal portions could not be removed without overcoming the adhesiveness and thereby permitting resumption of bleeding.
  • the delamination is highly desirable so that in an internal surgical procedure, no more of the material be allowed to remain than is necessary to effect hemostasis and seal the wound and excess material be removed.
  • a surgical cotton gauze pad Not tested, too harsh and board-unsetisfactory static efficacy, adhesiveness and delamination, the sheets are not deemed satisfactory from a handling viewpoint. Because of the loose, crumbly and friable characteristics of these sheets, the products may be said to be delicate and can not withstand normal shipping and handling. Upon handling, the sheets exhibit excessive flaking and loss of fibers. Such sheets can not withstand slight abrasion.
  • the sheets are too stiff and are too harsh and boardy, they have a low hemostatic efficacy, low adhesive quality and cannot be delaminated without opening the wound. Furthermore, such sheets do not readily conform to irregular surfaces encountered in a wound and, hence, are unsatisfactory.
  • Tensile strength in Kg. per 15 mm. strip from about 1 to about 4;
  • Burst Factor from about 1.2 to about 6;
  • a hemostatic adhesive dressing for severed biological surfaces comprising a liquid-laid, non-woven web having hemostatic-adhesive properties comprising hemostatic-adhesive fibers of ionizable, waterinsoluble, partial acid salts of collagen, the web having an absorbency of a mixture of 90 volumes of ethanol and 10 volumes of water of between about 100 percent and about 300 percent by weight and a porosity of from about 4 to about seconds per 6.45 sq. cm based upon a web having a basis weight of about l75.5 lbs. per 3,000 sq.ft., the fibers of the partial acid salt of collagen containing fromabout 50% to about 90% of the theoretical stoichiometric amount of ionizable acid.
  • the fibers are partial hydrogen chloride salts of collagen 4.
  • a dressing asdefined in claim 2 wherein the fibers are. partial hydrogen chloride salts of collagen containing from 60 percent to 85 percent of the theoretical stoichiometric amount of hydrogen chloride.
  • a dressing as defined in claim 1 wherein the fibers have a fiber length distribution by the McNett Classifier such that about 45 to 55% are retained on a mesh screen, 20 to are retained on a 35 mesh screen, 3 to 6% are retained on a 65 mesh screen, 0.5 to 1.5% are retained on a 150 mesh screen, and not more than pass a 150 mesh screen.
  • the method of forming a hemostatic adhesive liquid-laid, non-woven web dressing for severed biological surfaces from hemostatic-adhesive fibers of ionizable, water-insoluble, partial acid salts of collagen including the steps of slurrying the fibers in a mixture of a watermiscible organic liquid and water, sheeting the fibers :6 form a web and drying the web, the fibers of the partial acid salt of collagen containing from about 50% to about 90% of the theoretical stoichiometric amount of ionizable acid, the mixture of organic liquid and water consisting of from about 95 -volumes of organic liquid' and about 5 volumes of water to about 80 volumes of organic liquid and 20 volumes of water.
  • the fibers of the partial acid salt of collagen contain from 60% to 85% of the theoretical stoichiometric amount of hydrogen chloride, the mixture consists of volumes of ethanol and 10 volumes of water, the fibers have a fiber length distribution by the McNett Classifier such that about 48% are retained on a 20 mesh screen, about 22% are retained on a 35 mesh screen, about 3.6% are retained on a 65 mesh screen, about 0.7% are retained on a mesh screen and the balance passes a 150 mesh screen and the web is freeze dried.
  • the method of joining severed biological surfaces in a living warm blooded animal which comprises placing between and in contact with the severed surfaces a liquid-laid, non-woven fibrous web of hemostatic.
  • adhesive fibers of ionizable, water'insoluble, partial acid salts of collagen allowing the web to become wetted with blood, pressing the web into contact with the severed surfaces until hemostasis has been effected and then releasing the pressure, the web having the property of combining with blood to effect hemostasis and to form a mass with the blood that is self-adherent to the severed surfaces and thereby seal the wound, the
US00312210A 1972-12-04 1972-12-04 Liquid-laid, non-woven, fibrous collagen derived surgical web having hemostatic and wound sealing properties Expired - Lifetime US3810473A (en)

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US00312210A US3810473A (en) 1972-12-04 1972-12-04 Liquid-laid, non-woven, fibrous collagen derived surgical web having hemostatic and wound sealing properties
GB5528273A GB1426198A (en) 1972-12-04 1973-11-28 Liquid-laid non-woven fibrous collagen derived web having hemostatic and wound sealing properties
CA186,862A CA1020462A (en) 1972-12-04 1973-11-28 Liquid-laid, non-woven, fibrous collagen derived web having hemostatic and wound sealing properties
DE2359949A DE2359949C3 (de) 1972-12-04 1973-12-01 Verfahren zur Herstellung von naßverlegten Bahnen aus Fasern von partiellen Kollagensalzen
FR7343057A FR2281745A1 (fr) 1972-12-04 1973-12-03 Feuilles non tissees pour usages medicaux et chirurgicaux
JP13598973A JPS5436641B2 (de) 1972-12-04 1973-12-04
IT54111/73A IT1016029B (it) 1972-12-04 1973-12-05 Velo derivato da collagene fibro so non tessuto stratificato allo stato liquido avente proprieta emostatiche e cicatrizzanti

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JPS4986676A (de) 1974-08-20
DE2359949C3 (de) 1982-05-13
JPS5436641B2 (de) 1979-11-10
GB1426198A (en) 1976-02-25
IT1016029B (it) 1977-05-30
FR2281745A1 (fr) 1976-03-12
DE2359949B2 (de) 1981-08-06
DE2359949A1 (de) 1974-06-06
FR2281745B1 (de) 1978-07-21
CA1020462A (en) 1977-11-08

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