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WO1993002571A1 - Glucomannan de konjac clarifie et a fusion a froid - Google Patents

Glucomannan de konjac clarifie et a fusion a froid Download PDF

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Publication number
WO1993002571A1
WO1993002571A1 PCT/US1992/006591 US9206591W WO9302571A1 WO 1993002571 A1 WO1993002571 A1 WO 1993002571A1 US 9206591 W US9206591 W US 9206591W WO 9302571 A1 WO9302571 A1 WO 9302571A1
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WIPO (PCT)
Prior art keywords
konjac
clarified
gel
sol
turbidity
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.)
Ceased
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PCT/US1992/006591
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English (en)
Inventor
William C. Snow
Donald W. Renn
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FMC Corp
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FMC Corp
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Filing date
Publication date
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Priority to AU24494/92A priority Critical patent/AU663333B2/en
Priority to EP92914652A priority patent/EP0646133A1/fr
Publication of WO1993002571A1 publication Critical patent/WO1993002571A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
    • C08B37/0087—Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof
    • C08B37/009—Konjac gum or konjac mannan, i.e. beta-D-glucose and beta-D-mannose units linked by 1,4 bonds, e.g. from Amorphophallus species; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/244—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from corms, tubers or roots, e.g. glucomannan
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/256—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seaweeds, e.g. alginates, agar or carrageenan
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/269—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of microbial origin, e.g. xanthan or dextran
    • A23L29/27—Xanthan not combined with other microbial gums

Definitions

  • This invention relates to clarified konjac (that is, purified glucomannan derived from konjac) and methods for preparing the same. It includes clarified konjac powders as well as sols and gels prepared therefrom.
  • the clarified konjac glucomannan has enhanced purity and a low nitrogen content, and aqueous sols and gels thereof have low turbidity.
  • invention also relates to aspects of the clarified konjac including a cold-melt product and to methods for making the above products as well as varying the clarified konjac viscosity.
  • Konjac (Amorphophallus konjac) is a plant, the tuber of which is the source of a well-known foodstuff in China and Japan, namely konjac flour. This flour, which contains a variety of insoluble materials
  • glucomannan a polysaccharide comprised of D-glucose and D-mannose, which is useful as an ingredient in various foodstuffs, as well as in
  • U.S. Patent 3,928,322 to Sugiyama et al. disclose a method for producing konjac mannan polysaccharide, i.e. glucomannan, which comprises the principal ingredient of konjac flour, from raw konjac flour by first
  • Japanese Patent Disclosure 01-49657 filed March 1, 1989, discloses a konjac mannan product which has a nitrogenous component of not more than 0.2%. However, the method of achieving this reduced nitrogen content is not disclosed but appears to be by simple dilution.
  • decolorizing and clarifying galactomannan gum sols such as locust bean gum which comprises contacting the gum sol with activated carbon in the presence of aluminum sulfate, the latter being added in amounts sufficient to form a double Al-Na salt with sodium sulfate which is intrinsically present in the activated carbon
  • organic oxygen-containing hydrophilic stabilizers such as alcohols, glycols, ketones or the like. Incidental to this process there is disclosed in one example
  • Example 5 a means for clarifying locust bean gum by the conventional use of a filter aid such as
  • Japanese Patent Disclosures 59-227,267 (Dec. 20, 1984), and 58-165,758 (Sept. 30, 1983) disclose methods for treating aqueous sols of crude konjac flour with certain salts at pH , s of 10 or below to obtain an insoluble form of konjac, principally for use as insoluble food products.
  • Japanese Patent Disclosure 63-68054 discloses a reversibly soluble konjac gel product, but not the removal of insolubles which remain present in the product.
  • Gels formed from combinations of glucomannan derived from crude konjac with other hydrocolloids, particularly polysaccharides such as carrageenan or xanthan gums, are already known in the art. See, for example U.S. Patent 4,427,704.
  • This invention provides dry clarified konjac glucomannan of low nitrogen content; aqueous sols and gels thereof; and methods for preparing each of the above products.
  • the invention further provides:
  • hydrocolloid gums a cold-melt clarified konjac gel
  • further method and product variations hydrocolloid gums; a cold-melt clarified konjac gel; and further method and product variations.
  • the term "clarified” konjac refers to a konjac glucomannnan which is substantially free of insoluble impurities, which has a lower nitrogen content than unclarified konjac, and which exhibits a lower turbidity than unclarified konjac when in the form of an aqueous sol or gel.
  • the term "crude” konjac refers to an unclarified or native konjac flour in which the glucomannan is still contained in the sacs in which it occurs in nature, and various other impurities may be present.
  • this invention encompasses clarified konjac characterized in that it comprises glucomannan derived from konjac which is substantially free of insoluble impurities, and has a nitrogen content of 0 to 0.60 wt % accompanied by an aqueous sol turbidity potential of 20 to 70 Turbidity Units as well as a continuum of a nitrogen content of 0 to 0.25 %
  • this invention provides clarified konjac characterized in that it comprises glucomannan derived from konjac which is substantially free of insoluble impurities; and [A] has a nitrogen content of from more than 0.25 up to about 0.60 wt % and an aqueous sol turbidity potential of from 20 to 70 turbidity units as measured at 1.0 w/v % concentration using the Formazin Turbidity Standard; as well as the continuum of [B] a nitrogen content of 0.25 wt % or less, and an aqueous sol turbidity potential of 20 to 100 turbidity units as measured at 1.0 w/v % concentration using the Formazin Turbidity Standard, of which [B] is preferred. More preferably, the clarified konjac is characterized by a nitrogen content of 0.175 wt % or less and an aqueous sol turbidity potential of 20 to 70 turbidity units. Most preferably, the
  • clarified konjac is characterized by a nitrogen content of 0.15 wt % or less and an aqueous sol turbidity potential of 20 to 60 turbidity units.
  • This first group of embodiments also provides sols and gels of clarified konjac, cold-melt and spongy products, and methods for manufacturing the same.
  • substantially free of insoluble impurities has a nitrogen content of about 0.60 wt % or less, and has an aqueous sol turbidity potential of less than 20
  • the clarified konjac is characterized by a nitrogen content of no greater than about 0.25%. More preferably the clarified konjac is characterized by a nitrogen content of no greater than about 0.175%.
  • This second group of embodiments also provides sols and gels of this
  • the clarified konjac of this invention also is characterized by an aqueous sol viscosity potential of about 50 to 25,000 cps at a 1 w/v % concentration as measured using a Brookfield Viscometer Model LVTDV-II at 25°C and 20 rpm, preferably a viscosity of about 1,000 to 25,000 cps.
  • clarified konjac of this invention is characterized by the consecutive steps of: [a] preparing an aqueous sol of crude konjac comprising insoluble impurities and glucomannan; [b] contacting the crude konjac sol with an extraction-effective amount of an agent capable of extracting the insoluble impurities; [c] precipitating and removing the insoluble impurities; [d] forming a glucomannan coagulate by treating the remaining aqueous sol with a coagulant present in an amount sufficient to coagulate substantially all glucomannan therein; and [e] removing and drying the glucomannan coagulate to recover the dry, clarified glucomannan.
  • the clarified konjac of this invention may be prepared by dispersing the konjac flour in water, and treating the resulting glucomannan dispersion with one or more reagents together or sequentially, to extract by aggregation, precipitation, or absorption of the impurities present.
  • impurities are principally naturally-occurring in the konjac tuber and comprise nitrogenous materials such as proteins, insoluble fibers, and starches.
  • the method for production of the clarified konjac is characterized by the steps of:
  • extraction salt selected from one or more of dicalcium phosphate, calcium phosphate, magnesium phosphate, and aluminum sulfate (preferably calcium sulfate and aluminum sulfate, more preferably aluminum sulfate) in an amount effective to extract the insoluble impurities by precipitation;
  • clarified konjac sols alone or with other components, may be further converted into
  • correspondingly pure gels by known methods, such as by addition of an alkali.
  • the resulting gels may then be used in or as foodstuffs or in industrial compositions such as paints and other coatings.
  • the clarified konjac gels have the unusual property of liquifying within specific low temperature ranges. This is quite the reverse of the normal behavior of most hydrocolloid gels. Moreover, when cooled still further and then brought back to ambient temperature, the clarified konjac forms fibrous, porous, spongy, yet gel-like structures which, when compressed, rebound to their original form, and thus can serve as sponges to take up liquids and transport them to desired sites, such as to cells, seeds, calli, or plantlets placed within them.
  • inventive methods afford additional advantages over unclarified (crude) konjac flour, namely improved odor, color, solubility, and grindability.
  • Crude konjac has a known distinct odor, and a tan to dark brown color (as a dry powder).
  • crude konjac particles are not uniform in size and cannot be ground at normal milling temperatures. Milling or other such grinding of crude konjac produces high temperatures which destroy its viscosity potential in much the same way as dry heat degradation, and which contribute to its dark color.
  • clarified konjac of this invention is a white powder which forms a clear sol, is odor-free and can readily be ground to a uniform size. Additionally, clarified konjac is more uniform in glucomannan content, and thus avoids the wide, uncontrolled variations in viscosity or gel strength which occur with crude konjac.
  • clarified konjac powder of this invention Another desireable property of the clarified konjac powder of this invention is that, unlike crude konjac powder, clarified konjac hydrates rapidly in room temperature water with little effort, thereby
  • Figure 1 compares the nitrogen and turbidity values of the clarified konjac of this invention obtained using various extraction agents, with those of prior art products, including crude konjac.
  • Figure 2 compares the UV absorbance properties of clarified konjac with crude konjac.
  • amylopectin starches and carrageenan.
  • Gel forming hydrocolloids such as agarose are merely additive and not synergistic. It is notable that crude xanthan and AMF (seaweed flour, sometimes sold as carrageenan) are not adequate for this purpose, because the combinations do not produced the desired clear gel. Clarified konjac gel alone is somewhat cloudy, although less cloudy than crude konjac gel.
  • clarified konjac is more stable as a dry powder.
  • crude konjac stored for 4 weeks at above room temperature (50°C) loses 80% of its aqueous sol viscosity potential.
  • clarified konjac stored for the same time and at the same temperature loses only about 20% of its viscosity potential. It is believed that the increased storage stability is the result of the denaturing of enzymes present in the crude material, both by the initial heating of the sol and by the subsequent alcohol wash during the
  • Crude konjac flour starting material is a
  • the process involves slicing, drying and then wet- or dry-milling the Amorphophallus tuber, followed by pulverization of the resulting konjac to a powder ("flour”) which is sifted and air classified.
  • the resulting flour as described in the above publication, consists of fine, oval, whitish granules containing "flour sacs", that is, the glucomannan is encapsulated in a protein/fiber coating.
  • This flour when hydrated for some time with agitation releases the encapsulated glucomannan to form a sol which is characterized principally by its high viscosity, even at 1% concentrations, substantial turbidity, and high nitrogen content.
  • Viscosities in the range of 8,000 cps at a 1% by weight sol up to 130,000 cps at 3% are typically obtained after a heat (85°C) and cool cycle, as measured on a Brookfield ® RVT Viscometer, and an appropriate spindle, at 20 rpm and 25°C [the viscometer is a product of Brookfield
  • centipoise (cps) readings into viscosity functions are discussed by Mitschka, P. in Rheologica Acta, 21:207-209 (1982). As used herein, centipoise (cps) is equivalent to milli- Pascals ⁇ second (mP ⁇ s).
  • the crude konjac turbidity may vary considerably, depending upon the concentration of the sol, but in the above viscosity range of from 8,000 cps up to 130,000 cps and concentrations of 1% to 3%, turbidities of 100 to 300 turbidity units are conventionally obtained at 0.5 wt. % concentration, based on the Formazin
  • the high nitrogen content of the initial crude konjac flour is essentially a function of the amount of impurities present, principally the tuber's naturally- occurring protein and the sac fiber coating which encapsulates the glucomannan.
  • the nitrogen content of the dry crude flour is typically in the range of 0.3 to 1.3 wt. % of nitrogen, although higher percentages are possible depending upon the variety of tuber used.
  • the clarified products of this invention are characterized principally by their low nitrogen content and low turbidity as an aqueous sol or gel.
  • the corresponding viscosity of the product, in sol form, is also characteristically at a high level, and it is not adversely affected by the majority of agents that may be employed in the extraction process.
  • the clarified konjac is substantially free of insoluble impurities, having a nitrogen content and turbidity as low as possible.
  • a 1.0% aqueous sol according to this invention should have no greater than 100 (preferably 70, more preferably 60), turbidity units, as measured by a MacBeth Coloreye Computer, model 1500, (Kollmorgen Corp., Newburgh, N.Y.), and a Formazin Standard; and has a nitrogen content, (based on the weight of the dry product used to prepare the sol), of generally no greater than 0.25 (preferably
  • the clarified konjac sol is substantially transparent in appearance and may be used in a number of
  • the product of this invention may further be described as having a very wide, non-critical range at 1.0 wt % aqueous sol of viscosities of from 50 to
  • the clarified product inherently has high viscosities, i.e. from 1,000 to 25,000 cps, which are particularly useful for food formulations, but this viscosity can be reduced to as little as 50 cps by methods disclosed herein.
  • UV light may also be employed to characterize the clarified product and gauge the effectiveness of clarification procedures. This may be achieved by preparing 0.5% sols of product, placing them in cuvettes and measuring their UV absorbance between 200 and 320 nanometers (nm). Impurities, including DNA and protein, absorb UV light in the 260- 280 nm region and peaks in this area indicate their presence and relative amounts. As can be seen in
  • crude konjac samples contain a broad peak in this region and, overall, have a higher baseline of absorbance than clarified konjac samples, which lack the 260-280 peak. This is especially important for a biotechnology separation medium where the presence of DNA or protein might interfere with performance.
  • extraction agents The heating of the sol acts to break the natural sacs surrounding the glucomannan present in the crude konjac, and the extraction agent assists in removing protein impurities as well as the sacs themselves.
  • extracting or “extraction”, as used herein, means the separation of insoluble impurities from the konjac by aggregation, adsorption,
  • the sol is filtered to remove the insoluble impurities, and the filtrate coagulated with a water-miscible coagulating agent such as isopropyl alcohol to recover the glucomannan
  • the coagulate is then dried and ground to particulate form, to produce a clarified konjac flour according to this invention.
  • the extraction step may be varied somewhat
  • the agent may be blended with the crude konjac flour starting material, optionally with a filter aid, and the dry mixture dispersed with agitation into a sufficient amount of water to obtain the desired concentration of the resulting clarified konjac glucomannan, 0.1 to 10 (preferably 0.5 to 3) wt % depending on the viscosity potential.
  • the extraction agent may be added to the water either before or after the aqueous dispersal of the flour, particularly if an acid is employed to adjust the viscosity of the resulting product. While this dispersion may be carried out in water at ambient temperatures, preferably the water should be heated to temperatures of from 70 to 100°C, (preferably 85 to
  • the sol is filtered to remove the insoluble impurities, with or without a filter aid present.
  • Filters such as glass wool, paper, cloth and fibrous mats may be used for this purpose, although any filter which will remove insoluble particles is generally satisfactory.
  • Filter aids which may be employed include perlite and diatomaceous earth. The amount of filter aid is not critical, but is desirably employed in amounts of 1 to 5 times the weight of the konjac flour.
  • the filter cake is preferably then washed with hot water until no further clarified konjac glucomannan is recovered.
  • the filtrate is next treated with a water-miscible coagulating agent for the glucomannan, and the
  • Useful coagulating agents include lower alcohols such as methanol,
  • coagulating agent is not critical, but it should be added in amounts sufficient to recover the glucomannan from the sol generally in a weight ratio of 1-4:1, or a volume ratio of 2-3:1, coagulant:glucomannan.
  • the dry product may be recovered directly from sol by such methods as freeze drying or spray drying.
  • the coagulate should be dried until it is capable of being ground to a fine powder. This may be
  • the clarified, low-nitrogen product may be used in its dry, particulate form, for example in absorbent or texturizing applications, preferably it is used in sol form by redispersing the particles in water.
  • the resulting clear sol may then be gelled in known manner and/or as described herein.
  • the desired percent concentration of the dry composition in a sol or gel will depend largely on its intended use and its viscosity. Generally, 0.1 to 10 (preferably 0.5 to 3.0) wt %, based on the total weight of the sol may be employed, although these amounts are not critical.
  • the process includes deliberate steps to reduce the viscosity of the product, it will
  • this clarified konjac sol normally develops a high
  • the viscosity may be reduced to as low as about 50 cps at 1 w/v % and at 25°C.
  • the resulting sol may then readily be converted to a gel by known means, for example by addition of an alkali such as K 2 CO 3 followed by heating. Unless the degree of polymerization has been deliberately modified during the processing, as described below, these gels generally possess a 1% gel strength at 85°C of from 100 to 310g/cm 2 , when measured by a Marine Colloids Gel Tester GT-2. (FMC Corporation, Marine Colloids
  • useful extracting agents are: one or more salts selected from the group comprising dicalcium phosphate, calcium phosphate, magnesioum phosphate, or aluminum sulfate (which is preferred), used together or sequentially.
  • suitable extraction agents are those useful for changing the pH of the crude sol in order to refine the konjac, for example organic or inorganic acids such as HCl and bases such as NaOH.
  • the amount of such agent employed should be extractive-effective, that is, sufficient to vary the pH from 1 to 8.5, preferably 3 to S.5, within which ranges the benefits described in the product are obtained.
  • the glucomannan in addition to being extracted, may also begin to gel prematurely, while at highly acidic pH's the viscosity of the resulting product may be reduced. However, if this latter viscosity reduction is desired, then beneficially both extraction and viscosity
  • Aqueous extraction of the crude konjac may also be achieved by the use of chelating agents such as alkali metal hexametaphosphates, ethylenediamine tetraacetic acid (EDTA), and nitrilotriacetic acid (NTA).
  • chelating agents such as alkali metal hexametaphosphates, ethylenediamine tetraacetic acid (EDTA), and nitrilotriacetic acid (NTA).
  • the amount of chelating agent which should be used should be that which is chelating-effective, preferably 1 to 50 wt % based on the weight of the crude konjac.
  • CMC carboxymethyl cellulose
  • Soluble salts which may also be used as extraction agents include neutral salts such as sodium chloride; basic salts such as sodium acetate; or acidic salts such as calcium chloride, or combinations thereof.
  • a phosphate buffer for example a 0.005 M buffer, pH 7.3, prepared by mixing monobasic sodium phosphate with dibasic sodium phosphate in suitable amounts.
  • the soluble salt or buffer should be present in an extraction-effective amount, preferably 5 to 50 wt % based on the weight of the crude konjac.
  • insoluble salts may be employed as extraction agents, for example dicalcium phosphate, aluminum sulfate, calcium phosphate,
  • magnesium phosphate of which aluminum sulfate (alum) is preferred.
  • these salts may be formed in situ during the extraction steps by known means.
  • the insoluble salts should be present in an extraction-effective amount, preferably 1 to 25 (more preferably 5 to 15) wt % based on the weight of the crude konjac.
  • organic solvents including lower alcohols such as isopropyl alcohol may be used for this purpose, as demonstrated in Example 15. When utilized, the organic solvents should be present in an extraction-effective amount.
  • Hot water alone i.e. at 65 to 100°C
  • Hot water alone i.e. at 65 to 100°C
  • the amount of clarified konjac employed when incorporated in foodstuffs or industrial compositions will necessarily be varied, and can be determined without undue experimentation by those skilled in the art based on the known usage of crude konjac.
  • amounts of 0.1 wt % may be used in cake mix, while in industrial applications such as films, oil drilling fluids, and paints, amounts ranging from 1 to 2% and upward may be employed.
  • clarified glucomannan of this invention in foodstuffs such as baked goods, dessert gels, and meats, results in improved food properties.
  • addition of the refined material to cake dough results in improved texture, moistness, and rise of the final product.
  • the product In its gel form the product is useful as a food or food component, film former, and in various
  • the viscosity of the konjac sol which is normally high, may be reduced before, during, or after the extraction step by treatment of the glucomannan with a variety of reagents or other means to obtain viscosities of whatever reduced values are desired.
  • sols of reduced viscosity are particularly useful in biotechnology for preparing gels of high
  • Such means include: exposure to gamma radiation; exposure to radiation other than gamma such as actinic; acid hydrolysis, including "Smith
  • Reduction of viscosity by irradiation can be achieved by contacting the crude or clarified konjac with gamma rays, such as generated from cobalt 60 , at dosages ranging from 50 to 1200 Krad or above, in which case a direct correlation between dosage and viscosity is obtained, as shown in the examples below.
  • gamma rays such as generated from cobalt 60
  • heat degradation of the crude or clarified glucomannan may be employed. For example, heating the glucomannan for a requisite number of hours, or even days, at temperatures of from 50 to 200°C, depending upon the reduced level of viscosity desired, will produce satisfactory results.
  • clarified konjac When clarified konjac is cooled to freezing or slightly below and then brought back to room temperature, it forms a clear, water- insoluble, spongy, dimensionally stable mass. It is known that this phenomenon occurs with crude konjac, however the spongy mass formed with clarified konjac is noticeably lighter in color and contains none of the protein or other impurities found in crude konjac itself, and does not have the characteristic odor of crude konjac. Because of this, it is contemplated that the spongy mass prepared from clarified konjac is suitable for various medical applications such as implants and carriers for medications and for
  • the clarified konjac gel possesses this "cold-melt" property, it is important that it be formed under certain controlled conditions, primarily with respect to pH, as well as to the time the gel takes to form at any given temperature. Other factors which may also affect the ability of the gel to melt at low temperatures, include ion content and type. For example, it has been found that as the glucomannan concentration increases, the gel melts more slowly.
  • the concentration of clarified glucomannan in the gel is not critical, and may vary from .01 to 10 (preferably 1 to 5) wt %.
  • glucomannan first must be adjusted, desirably by heating it with an alkali at a temperature of from 65 to 130°C until the gel is formed.
  • the pH should desirably be 9.6 to 12.3, preferably 10 to 11.5, employing such bases as NH 4 OH, NaOH, K 2 CO 3 , or mixtures thereof, of which NH 4 OH is preferred. It has been found, moreover, that gels formed at the lower pH values within this alkaline range subsequently melt to a sol more rapidly.
  • the pH of already- formed gels which were prepared at high pH values, can be lowered by treatment with a buffer solution, to a pH of 8-9 or lower without adversely affecting the cold-melt property of the gel. It has also been found that the cold-melt property is
  • gels may be prepared at an acid pH (instead of alkaline pH) if the preparation is carried out under retort conditions, that is, at high temperatures while under pressure.
  • gels may be formed from clarified konjac sols at a pH of 6.7, a temperature of 130°C, and a pressure of 30 psi (about 2 atmospheres or 2.11
  • One convenient method for gelation is by adding NH 4 OH to a 1% sol of clarified glucomannan until the desired pH is achieved, e.g. 11.2; heating the alkaline sol for about 5 to 60 minutes, depending upon the amount employed, (preferably 20 to 30 minutes at a temperatures of from 50 to 120°C, more preferably 80 to 90°C), until a gel forms; and thereafter cooling the gel in an ice bath, until it liquefies.
  • the melted material can then be reformed to a gel by heating it until the gel starts to redevelop, generally starting at temperatures of 6°C and above.
  • the gels formed from the clarified konjac of this invention consistently exhibit cold-melt properties, that is, the gels liquefy when exposed to temperatures below 5°C, down to 0°C, at ambient pressure. If it is desired to keep the clarified konjac gel at low temperature without liquefying, this cold-melt property can be avoided by the admixture of non-cold-melt
  • hydrocolloids principally such gums as xanthan, carrageenans, and agaroids (especially agarose) or mixtures thereof.
  • the clarified konjac will cogel with the hydrocolloid without the addition of alkali.
  • Other hydrocolloids may require added alkali, heat, specific ions, or similar means to form the gel, as is known in the art.
  • hydrocolloids In addition to the hydrocolloids, it has been found that certain ionic compounds at or above certain concentrations, for example salts such as NaCl, may also be used for the purpose of preventing cold melting of gels. In either case it will be seen that variant cold-melt properties can be achieved on a selective basis by the addition of these materials.
  • salts such as NaCl
  • hydrocolloid or ionic compounds necessary for preventing cold-melting of gels may be varied considerably. For example, the addition of 10% NaCl, i.e. ionic compound, by volume, will prevent cold melting. Alternatively, when a hydrocolloid is employed, the weight ratio of glucomannan to
  • hydrocolloid in the gel may vary from about 10:1 to 1:10.
  • the addition of 1 part by weight carrageenan or xanthan to 3 parts of glucomannan, based on the weight of the konjac in the gel will likewise prevent cold melting.
  • the amount of these additions employed can be increased accordingly.
  • the melted clarified konjac may be recovered in its liquid state and stored or handled that way, if
  • the sol is notably stable at those temperatures.
  • biotechnology as an electrophoresis medium, or in medical technology as a drug delivery medium, e.g. by incorporation of a drug into the liquefied sol which could then be hardened by warming it for storage or administration purposes.
  • Foodstuffs and beverages normally served cold could have their texture and consistency enhanced by making and/or storing a gel- containing food under cold conditions until ready to be served, e.g. frozen desserts or the like; or
  • the cold-melted sol may be used in cell encapsulation or to deliver drugs
  • this sol upon application to a cut or burn, dries to form a thin film that slowly releases effective amounts of the drug to the affected area.
  • Example 2 demonstrating the preparation of the clarified konjac product of this invention by means of the aqueous extraction of crude konjac flour with a variety of extraction agents.
  • Example 1 the procedures of Example 1 were followed, except for the use of different extraction agents, as indicated.
  • a sol of the dry, ground product was prepared after which a viscosity
  • Aqueous extractions alone or incorporating various salts both soluble and insoluble, different pH's, chelating agents, ion exchangers, etc. were used.
  • filtration time was 70 minutes and 430 ml filtrate was collected.
  • the filtrate was coagulated in 2x volume of 99% isopropyl alcohol (IPA), based on the volume of the filtrate, and allowed to stand for 60 minutes.
  • IPA isopropyl alcohol
  • the coagulate was collected by vacuum filtration, on polyester cloth, squeezed dry, and transferred to 2x volume of 60% IPA for 30 minutes.
  • the coagulate was again recovered, again treated with 99% IPA, and then dried at 55°C overnight (14 hours) in a forced hot-air oven.
  • the sample weighed 3.57 g; (59.5% yield) and was ground through a 40 mesh screen (U.S. Standard Sieve Series). This material was used to prepare 200 ml of a 1 wt % aqueous sol by suspending 2 g in 200 ml
  • the following experiment illustrates the combined viscosity reduction and extraction of crude konjac with acid at low pH. The effect was to reduce the viscosity before the extraction was completed.
  • Example 1 The procedure outlined in Example 1 was repeated with the following changes. The water was adjusted to pH 2 with 1.0M HCl before heating. Filtration was very quick, with 550 ml filtrate passing through the filter bomb in 8 minutes without the need to apply any
  • Examples 3 and 4 illustrate the aqueous extraction, as in Example 2, except that in Example 4 a base was used. It will be noted that while this procedure was fully effective at pH 7, at pH 10 the results were poorer because of the partial gelling of the product at the higher pH values, which interfered with the
  • Example 2 The procedure described in Example 2 was repeated using pH 7. The pH was controlled, as needed, with small amounts of 0.1N NaOH and 1.0N HCl. 250 ml of filtrate was collected in 95 minutes and then
  • the dried sample 1.81 g or 30.1%, had a viscosity of 14,200.
  • Example 2 In a like manner, as in Example 2, an aqueous extraction was carried out using pH 10 adjusted (1.0N NaOH) water. Filtration was slow and only 150 ml of filtrate was collected (see table below for filtration times and pressures). The small amount of filtrate was observed to be partially gelled and was discarded. Examples 5 and 6 illustrate the extraction process using two different chelating agents.
  • EXAMPLE 5 (Hexametaphosphate - HMP) Sodium hexametaphosphate (3 g, 0.5% w/v) was added to the hot water prior to the addition of the konjac.
  • 50 g Celatom diatomite (Eagle- Picher; Cincinnati, Ohio) filter aid was mixed into the sample before filtration. After 109 minutes, 400 ml filtrate was collected and processed (see details below). After drying, 3.62 g (60.3% yield) was ground and used to prepare a 1% sol. This material had a viscosity of 3,010 cps and a gel strength of 124 g/cm 2 . It also "cold-melted” and regelled upon warming.
  • EXAMPLE 6 (Ethylenediamine Tetraacetic Acid-EDTA)
  • Example 5 In a manner similar to Example 5, another 6 g crude konjac was extracted substituting 0.6 g (0.1% w/v) disodium EDTA for hexametaphosphate. Only 300 ml filtrate was collected after 120 minutes. This yielded 1.91 g or 31.9% after coagulation and drying. A 1% sol had a viscosity of 19,700 cps.
  • Examples 7-10 demonstrate the use of various soluble salts, or mixtures thereof, in the aqueous extraction of crude konjac, again using the general procedures of Example 1.
  • a 0.005 M phosphate buffer, pH 7.3 was prepared by mixing 39 ml 0.2M monobasic sodium phosphate with 61 ml 0.2M dibasic sodium phosphate. An aliquot of this, 25 ml, was diluted to 1 liter giving a final concentration of 0.005M. Six grams of crude konjac was extracted in this solution as previously described. The filtrate, 250 ml obtained after 68 minutes, was processed and dried. The sample (1.957 g; 32.9% yield) had a 1% viscosity of 1,380 cps.
  • Examples 12-14 were found not to cold melt. This may be the result of ion binding and/or aggregation
  • EXAMPLE 12 (Cation Exchanger-Carboxymethyl Cellulose) (A.) To 600 ml distilled water, 0.6 g of water- soluble carboxymethyl cellulose (CMC) (10% w/w with konjac) was added before the addition of konjac. No filter aid was used and 500 ml filtrate was collected in 10 minutes at 5 psi (.35 kg/cm 2 ). After processing and drying, 4.45 g or 74.1% was obtained. It had a 1% viscosity of 15,700 cps.
  • CMC water- soluble carboxymethyl cellulose
  • EXAMPLE 15 (20% Isopropyl Alcohol) Six grams of the crude konjac was extracted in a mixture of 148 ml 99% isopropanol in 452 ml distilled water (20% w/w) as previously described. After 90 minutes of filtration, 275 ml of filtrate was collected and then processed. A total of only 1.25 g (20.9% yield) was recovered. This material had a viscosity of 11,800 cps. In Examples 16-21 insoluble salts were used to adsorb impurities from the konjac in which the salts were formed in situ in Examples 18-21. It will be noted that when a filter aid was introduced by way of a modification to Example 18, as in Example 19, a clearer product was obtained. In a similar modification of Example 20, as in Example 21, but using a filter aid, much less filtrate was obtained.
  • Dicalcium phosphate was also used in an extraction by adding 0.6 g (10% w/w with konjac) to the water before the addition of the konjac. After the "cook", 15 g of filter aid was added and filtration was carried out for 10 minutes at 25 psi (1.75 kg/cm 2 ) and then 40 minutes at 40 psi (2.8 kg/cm 2 ). Only 50 ml of filtrate was collected during this time so the sample was removed from the filter bomb, pooled with the small amount of filtrate and an additional 85 g of filter aid mixed in. Filtration proceeded for 120 minutes during which time 250 ml of filtrate was collected and
  • This process yielded 1.65 g; (27.4% yield) .
  • This material had a 1% viscosity of 4 , 410 cps on a Brookfield Viscometer, Model LTVDV-II, No. 1 spindle.
  • EXAMPLE 19 (Aluminum Sulfate - In situ) The above extraction was repeated with a few changes. 0.526 g of the aluminum chloride (0.291 g anhydrous AICI 3 ) and 0.310 g monobasic sodium sulfate were used in this case. Additionally, 25 g of filter aid was added before filtration. Over 98 minutes, 450 ml of clear filtrate was collected and then processed. After drying, 3.65 g (60.9% yield) of material was ground and used to prepare a 1% sol. The sol, which was very clear, had a viscosity of 1150 cps.
  • the sol was heated in a hot water bath for 60 minutes at a temperature of 85°C during which time a gel formed. The gel was immediately tested for gel
  • the coagulate was dried in a forced-draft oven overnight at 60°C to produce a hardened cake which was ground up through a No. 40 screen (U.S. Standard Sieve Series) (420 microus).
  • the dry particulate product was then reconstituted as a 1 wt % aqueous sol.
  • the viscosity and turbidity of this sol were then measured, the results of which are also reported in Table III.
  • comparative Example 46 the viscosity and turbidity of a sample of commercial konjac flour dissolved in water to which no reagents had been added, was measured.
  • comparative Example 47 the dissolved konjac flour was processed in accordance with the method of this invention except that no aluminum sulfate or NaOH was added.
  • Spectrophotometer II using a Fuller's Earth Standard. They were then converted to the Formazin Standard by correlation studies which compared samples of the two standards, using the Fisher unit. A final conversion to the MacBeth/ Formazin standard of this table was then obtained via a correlation coefficient, as described below in Table VI, footnote (b) . d. Unprocessed, untreated konjac flour.
  • Example 44 Processed with hot water (15 min. at 85°C) , but not with aluminum sulfate or NaOH. From the foregoing it will be seen, as shown in Example 44, that the viscosity of the clarified konjac may be maintained at very high levels, particularly for food use, by optimizing the amount of aluminum sulfate used. Also, the turbidity of the reconstituted, clarified konjac of this invention is significantly lower in Examples 43-45 of this invention as compared to the crude konjac sol of comparative Example 46. The processing (heating, etc.) of konjac with hot water in the absence of aluminum sulfate (Example 47) somewhat increased the turbidity of the reconstituted sol.
  • the following example illustrates a scaled-up version of the preceding aluminum sulfate clarification procedure.
  • the filtrate was coagulated in 300 gallons (1,136 liters) 85% isopropyl alcohol IPA.
  • the coagulate was recovered by screening and by pumping it through bags which were subsequently squeezed in a small press. The coagulate was then washed/hardened in 75 gallons of 85% IPA for 2 hours with air agitation. The coagulate was recovered by screening and then squeezed by hand to remove excess liquid and subsequently dried at 55°C overnight.
  • the sample 6.4 lbs. (2.9 kg) or 64% yield, was ground through a 0.039 inch (2.4mm) screen. It had a nitrogen content of 0.15% and a 1% turbidity of 11 NTUs
  • Example 48 In a further series of runs, and in accordance with the general procedures of Example 22, the product of Example 48 was tested for gelation and cold- meltability, using various bases and reaction
  • clarified konjac were prepared in accordance with the procedures of Example 48. Using 1.0N NaOH and 0.1N HCl (to back titrate), each beaker was adjusted to one of the following pH values: 8.5, 9.0, 9.5, 10.0, 10.5 and 11.0. These were all placed in a boiling water bath for 20 minutes. Those samples with initial pH values 10, 10.5 and 11 gelled and were removed after 20 minutes to cool at room temperature. Those samples at lower pH did not gel after 1 hour in the water bath.
  • the 3 gels were placed in an ice bath.
  • the gel made at pH 10 melted fully and quickly.
  • the gel made at pH 10.5 melted slowly and only partially.
  • the last gel (pH 11.0) did not melt but softened considerably.
  • a series of 50-g aliquots of 1 wt % of aqueous clarified konjac was prepared as in Example 49. To the first four aliquots, all contained in beakers, 25, 50, 75 and 100 microliters, respectively, of 5M NH 4 OH was added. The remaining aliquots received increments of 100 microliters (maximum 2.1 ml). The pH was checked by pH meter and visually, by universal indicator. The gels were then heat set for 20 minutes, cooled to room temperature, covered, and allowed to stand at room temperature overnight (16 hours). The beakers were all placed in an ice bath and monitored. The pH of those that melted was rechecked. Selected results are listed in the following table.
  • the following example illustrates the preparation of a gel at retort conditions and at a low pH.
  • 800 mis of a 2% sol of clarified konjac from Example 48 was prepared by dispersing and dissolving it in a pH 6.6 phosphate buffer. This material was used to fill an aluminum can to capacity which was subsequently sealed. The can was placed in a pressure cooker and heated at 130°C at 30 psi (2.1 kg/cm 2 ) for 60 minutes. After cooling, the can was opened. A soft gel was revealed. Several pieces were removed, placed in a separate small beaker and then iced. The gel melted fully and when heated in a hot water bath ( ⁇ 90°C) for 25 minutes, a much firmer gel reformed.
  • the gels stored at room temperature were placed in an ice bath to check for meltability.
  • the two lower pH gels melted completely.
  • Sols 200 ml, 1% w/v of each sample, as well as samples of the original nondegraded materials, were prepared by heating the sample in a water bath and stirring with an overhead mixer for 60 minutes. The samples were poured into 250 ml tall-form beakers and allowed to cool to room temperature. The viscosities were determined with a Brookfield digital viscometer as described above. An aliquot (50 ml) of each sample was mixed with 2 ml of 5M NH 4 OH and placed in a boiling water bath for 20 minutes to check for gelling ability. Following gelation, the gels were placed on ice to check for cold-meltability. The results of each of these tests are shown below in Table V.
  • the sol was passed through a 115 mesh (125 micron) and then a 270 mesh (53 micron) metal screen to remove gross insolubles.
  • the sol would not filter through a medium porosity glass filter (Pyrex 150 ml, ASTM 10-15) or a 0.2 micron filter so instead was heated to 90°C and twice passed through a 14 inch - 1 inch diameter (35.6 cm - 3.54 in diameter) bed of tightly packed glass wool.
  • the yield was 1.137 or 45.5%. Due to excessive static, the sample could not be ground and was wetted with a small amount of 20% isopropyl alcohol and then dried at 55°C for 3 hours. The sample was then ground through a 40 mesh screen.
  • the sample had a nitrogen content of 0.07% and a 1.0% turbidity of 128 Turbidity Units.
  • the sample was removed from the dialysis tubing and centrifuged at 7500 rpm for 10 minutes.
  • This material was frozen at -75°C for 45 minutes and then lyophilized at 0.1 Torr and 100°F (37.8°C) for 3 days.
  • Xanthan 100 g of a hot 1% clarified konjac sol was mixed with 33 g of a 1% w/v sol of xanthan (Keltrol T, Kelco Co., San Diego, Ca.). The mixture, which began gelling almost immediately, was heated in a hot water bath to melt the gel. Once melted, two 50 g aliquots were poured into beakers. Two ml of 5M NH 4 OH was stirred into each hot liquid sample. One was placed in a boiling water bath for 20 minutes while the other was allowed to cool to room temperature. Both samples formed gels although they differed in
  • the heat set gel was opaque and somewhat spongy while the second aliquot (not heat set) was clear and very elastic.
  • the heat set gel when placed in an ice bath, became clear and elastic but did not liquefy. When this transformed gel was reheated, it took on its original properties, that is, opaque and spongy. When placed in an ice bath, it again reverted to the clear elastic gel.
  • Carrageenan 33 g of a 1% w/v CIC carrageenan sol (sodium, reduced-viscosity kappa-form, a product of FMC Corporation, Marine Colloids Division, Philadelphia, Pennsylvania) was mixed with 100 g of a 1% clarified konjac sol. Five ml of 5M NH 4 OH was added with

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Abstract

Compositions de glucomannan de konjac clarifié exemptes d'impuretés insolubles, ayant une teneur en azote non supérieure à environ 0,60 % en poids, et présentant un potentiel de turbidité sous forme de sol aqueux à 1,0 % non supérieur à environ 100 unités de turbidité mesurées selon la norme de turbidité de Formazin, gels et sols aqueux, gels à fusion à froid ainsi que leurs formes spongieuses. Les sols et gels obtenus peuvent être utilisés dans des aliments, des applications industrielles biotechniques.
PCT/US1992/006591 1991-08-08 1992-08-07 Glucomannan de konjac clarifie et a fusion a froid Ceased WO1993002571A1 (fr)

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AU24494/92A AU663333B2 (en) 1991-08-08 1992-08-07 Clarified and cold-melt konjac glucomannan
EP92914652A EP0646133A1 (fr) 1991-08-08 1992-08-07 Glucomannan de konjac clarifie et a fusion a froid

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5455344A (en) * 1993-09-03 1995-10-03 Fmc Corporation Agarose compositions for nucleic acid sequencing
US5624612A (en) * 1993-08-25 1997-04-29 Fmc Corporation Nonaggregating hydrocolloid microparticulates, intermediates therefor, and processes for their preparation
US6586590B1 (en) 2000-07-03 2003-07-01 Marine Bioproducts International Clarified hydrocolloids of undiminished properties and method of producing same
WO2002072687A3 (fr) * 2001-03-13 2003-10-23 Marine Bioproducts Internat Formes physiques d'hydrocolloides clarifies possedant des proprietes inchangees et leur procede de production
US6831107B2 (en) * 1998-12-05 2004-12-14 Christian Joseph Dederen Emulsification systems and emulsions
US20160331000A1 (en) * 2015-05-12 2016-11-17 Takashi Sawamura Denatured glucomannan
CN107141505A (zh) * 2017-05-15 2017-09-08 陕西科技大学 一种魔芋葡甘聚糖抗菌海绵的制备方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6162906A (en) * 1991-08-08 2000-12-19 Fmc Corporation Clarified konjac glucomannan

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US2508726A (en) * 1946-06-27 1950-05-23 Gen Mills Inc Precipitation of mannogalactans and glucomannans from aqueous sols
US2599771A (en) * 1950-07-19 1952-06-10 Gen Mills Inc Gels of carboxyalkyl ethers of carbohydrate gums
US2767167A (en) * 1953-07-06 1956-10-16 Gen Mills Inc Process of reducing the viscosity of gums
US4427704A (en) * 1979-04-11 1984-01-24 Mars Limited Food product thickened or gelled with carrageenan and glucomannan
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US4746528A (en) * 1984-12-14 1988-05-24 Mars G.B. Limited Gel system
JPH02231044A (ja) * 1989-03-01 1990-09-13 Toki Bussan Kk 食物繊維加工食品

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US2508726A (en) * 1946-06-27 1950-05-23 Gen Mills Inc Precipitation of mannogalactans and glucomannans from aqueous sols
US2599771A (en) * 1950-07-19 1952-06-10 Gen Mills Inc Gels of carboxyalkyl ethers of carbohydrate gums
US2767167A (en) * 1953-07-06 1956-10-16 Gen Mills Inc Process of reducing the viscosity of gums
US4427704A (en) * 1979-04-11 1984-01-24 Mars Limited Food product thickened or gelled with carrageenan and glucomannan
JPS59227267A (ja) * 1983-06-07 1984-12-20 Kazuo Hara コンニヤクの利用方法
US4746528A (en) * 1984-12-14 1988-05-24 Mars G.B. Limited Gel system
JPH02231044A (ja) * 1989-03-01 1990-09-13 Toki Bussan Kk 食物繊維加工食品

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DERWENT ABSTRACT, Accession Number 84-021155/04; & JP,A,58 213 001, 10 December 1983, 1-8 and 19-26. *
Nutricol Konjac Flour, (1989) FMC Corporation, Marine Colloids Division, Philadelphia, PA 19103, USA. *
See also references of EP0646133A4 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5624612A (en) * 1993-08-25 1997-04-29 Fmc Corporation Nonaggregating hydrocolloid microparticulates, intermediates therefor, and processes for their preparation
US5718969A (en) * 1993-08-25 1998-02-17 Fmc Corporation Nonaggregating hydrocolloid microparticulates, intermediates therefor, and processes for their preparation
US5455344A (en) * 1993-09-03 1995-10-03 Fmc Corporation Agarose compositions for nucleic acid sequencing
US6831107B2 (en) * 1998-12-05 2004-12-14 Christian Joseph Dederen Emulsification systems and emulsions
US6586590B1 (en) 2000-07-03 2003-07-01 Marine Bioproducts International Clarified hydrocolloids of undiminished properties and method of producing same
WO2002072687A3 (fr) * 2001-03-13 2003-10-23 Marine Bioproducts Internat Formes physiques d'hydrocolloides clarifies possedant des proprietes inchangees et leur procede de production
US20160331000A1 (en) * 2015-05-12 2016-11-17 Takashi Sawamura Denatured glucomannan
CN106136213A (zh) * 2015-05-12 2016-11-23 张晓华 变性甘露聚糖
CN106136213B (zh) * 2015-05-12 2021-07-06 张晓华 变性甘露聚糖
CN107141505A (zh) * 2017-05-15 2017-09-08 陕西科技大学 一种魔芋葡甘聚糖抗菌海绵的制备方法

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CA2115141A1 (fr) 1993-02-18
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EP0646133A4 (fr) 1994-05-25
JP2687046B2 (ja) 1997-12-08
AU663333B2 (en) 1995-10-05
HU9400345D0 (en) 1994-05-30
AU2449492A (en) 1993-03-02
EP0646133A1 (fr) 1995-04-05

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