Manufacture of and uses for low molecular weight agars and agaroids

• US 6,322,814 B1
• Filed: 11/29/1999
• Issued: 11/27/2001
• Est. Priority Date: 03/04/1994
• Status: Expired due to Term

• Current Assignee: Ian James Miller
• Original Assignee: Ian James Miller
• Inventors: Miller, Ian James
• Primary Examiner(s): Levy, Neil S.
• Application Number:
  US09/456,017
• Time in Patent Office: 729 Days
• Field of Search: 536/114, 523/105, 523/122, 426/72, 426/311, 424/405, 424/406, 424/484, 424/485, 424/488, 424/442, 424/439, 424/400, 424/401, 424/78-2-, 424/409, 424/195.17, 514/24, 514/64, 514/54
• US Class Current: 424/484
• CPC Class Codes: A23G 2200/06 containing beet sugar or cane sugar if specifically mentioned or containing other carbohydrates, e.g. starches, gums, alcohol sugar, polysaccharides, dextrin or containing high or low amount of carbohydrate
• CPC Class Codes: A23G 3/346 Finished or semi-finished products in the form of powders, paste or liquids A23G3/343 takes precedence
• CPC Class Codes: A23L 29/256 from seaweeds, e.g. alginates, agar or carrageenan
• CPC Class Codes: A61K 8/042 Gels
• CPC Class Codes: A61K 8/73 Polysaccharides
• CPC Class Codes: A61Q 17/02 containing insect repellants
• CPC Class Codes: A61Q 19/00 Preparations for care of the skin
• CPC Class Codes: C08B 37/0039 Agar; Agarose, i.e. D-galactose, 3,6-anhydro-D-galactose, methylated, sulfated, e.g. from the red algae Gelidium and Gracilaria; Agaropectin; Derivatives thereof, e.g. Sepharose, i.e. crosslinked agarose

Abstract

A process is claimed whereby an aqueous solution of agar, in which most (ideally all) 4-linked residues consist of 3,6-anhydro-L-galactose, is subjected to partial acid hydolysis and upon neutralization following the time appropriate for the chosen conditions, a low strength gel is obtained, from which, contrary to expectations, a polyagarobiose can be obtained by freeze-thawing and straining, thereby eliminating undesirable agaroid materials without the appropriate 3,6-anhydrogalactosyl content. The appropriate time of hydrolysis depends on initial gel strength, pH, counterion concentration and temperature. As an example, agar (gel strength 700 g/cm², made to 1.86% solution) pH 3.25, counterion citrate (360 mg/L) at 96° C. requires 25 minutes to yield a material with an eventual gel stregth (1.5% solution) of 40 g/cm². A stabilized product can be prepared by reducing terminal anhydrogalactosyl residues with sodium borohydride. The resultant products are useful for preparing gels for application to the skin, such as massage gels, as skin moisturizers, or as carriers of other active ingredients, such as pharmaceuticals able to be applied through the skin.

Claims

1. A process to manufacture a material able to form an aqueous gel which, at a concentration of 15% of solids by weight has a dynamic gel strength of 0-100 g/cm², that comprises the sequence of steps of taking an agar or agarose with 0-2 methyl groups per agarobiose unit and which has had the agarobiose content maximised by rigorous alkali treatment such that no increase in gel strength can be achieved by repeated alkali treatment, and dissolving this agar or agarose in water, then partially depolymerizing it by making the pH less than 7 and maintaining temperature between 35-140°

C. for a period of time chosen to give the appropriate degree of depolymerization for the required final gel strength, then neutralizing the mixture and cooling it so a gel forms, then freezing then thawing the mixture to provide a particulate solid dispersed in the water, then straining the liquid to obtain the said material.

4. A gel for application to skin prepared by redissolving the material produced by the process of claim 1 in hot water and allowing to cool to form said gel.

6. A gel for application to the skin prepared by redissolving the material produced by the process of claim 1 or claim 2 in hot water together with lambda carrageenan and allowing to cool to form said gel.

7. A gel for application to the skin prepared by redissolving the material produced by the process of claim 1 or claim 2 in hot water together with carrageenans and allowing to cool to form said gel.

8. A gel for application to the skin prepared by redissolving the material produced by the process of claim 1 or claim 2 in hot water together with fucoidan and allowing to cool to form said gel.

9. A gel for application to the skin prepared by redissolving the material produced by the process of claims 1 or claim 2 in hot water together with sulphated polysaccharides from red seaweeds selected from the group consisting of the Lomentariaceae, Cryptonemiaceae, or Kallymeniaceae families and allowing to cool to form said gel.

10. Skin nutritive, emmollient or moisturizing gels prepared by redissolving the material produced by the process of claim 1 or claim 2 in hot water together with nutrient agents and/or agents which maintain moisture levels and allowing to cool to form said gel.

11. Gels for applying insect repellents to the skin prepared by redissolving the material produced by the process of claim 1 or claim 2 in hot water together with insect repellents and allowing to cool to form said gel.

12. Gels for applying pharmaceutical products to the skin prepared by redissolving the material produced by the process of claim 1 or claim 2 in hot water together with pharmaceutical products and allowing to cool to form said gel.

2. A process to manufacture a material able to form an aqueous gel which, at a concentration of 15% of solids by weight has a dynamic gel strength of 0-100 g/cm², that comprises the sequence of steps of taking an agar or agarose with 0-2 methyl groups per agarobiose unit and which has had the agarobiose content maximised by rigorous alkali treatment such that no increase in gel strength can be achieved by repeated alkali treatment, and dissolving this agar or agarose in water, then partially depolymerizing it by making the pH less than 7 and maintaining temperature between 35-140°

C. for a period of time chosen to give the appropriate degree of depolymerization for the required final gel strength, then neutralizing the mixture and adding sodium borohydride, neutralizing to pH 7, and cooling the mixture so a gel forms, then freezing then thawing the mixture to provide a particulate solid dispersed in the water, then straining the liquid to obtain the said material.

3. The material which is produced by the process of claim 2.

5. A gel for application to skin prepared by redissolving the material produced by the process of claim 2 in hot water and allowing to cool to form said gel.