WO2008141507A1 - Gomme gellane organique sans solvant et son procédé de préparation - Google Patents

Gomme gellane organique sans solvant et son procédé de préparation Download PDF

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Publication number
WO2008141507A1
WO2008141507A1 PCT/CN2007/070027 CN2007070027W WO2008141507A1 WO 2008141507 A1 WO2008141507 A1 WO 2008141507A1 CN 2007070027 W CN2007070027 W CN 2007070027W WO 2008141507 A1 WO2008141507 A1 WO 2008141507A1
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WIPO (PCT)
Prior art keywords
gellan gum
filtration
products
ppm
gellan
Prior art date
Application number
PCT/CN2007/070027
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English (en)
Chinese (zh)
Inventor
Shichu Zhang
Delong Hu
Zhi Ding
Nana MA
Original Assignee
Shanghai Huiyuan Vegetal Capsule Co., Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shanghai Huiyuan Vegetal Capsule Co., Ltd filed Critical Shanghai Huiyuan Vegetal Capsule Co., Ltd
Priority to PCT/CN2007/070027 priority Critical patent/WO2008141507A1/fr
Publication of WO2008141507A1 publication Critical patent/WO2008141507A1/fr

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Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • 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
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00—Preparation of compounds containing saccharide radicals
    • C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds

Definitions

  • the present invention relates to the field of production of microbial polysaccharide gellan gum, and more particularly to a method for producing a low acyl cold gel in the absence of an organic solvent and a novel gellan gum prepared. Background technique
  • Gellan gum approved by the US FDA in 1992, is a high-quality gelling agent and suspending agent. It is of great value in food additives, pharmaceutical excipients, and microbial and plant tissue culture media.
  • Chinese patent application CN 00125858.3 (application date; October 26, 2000) discloses a microbial polysaccharide gellan gum production process.
  • gellan gum products are classified into two types depending on the composition of some components in the molecular structure.
  • gellan gum polysaccharide molecules in the D- glucose residues about 50% of C 6 substituted acetyl group has the effect of hindering intermolecular carrier web to form a gel, which has good viscoelasticity, termed It is a high acyl gellan gum. Since the gellan gum in the fermentation broth is of this type, it is also called natural gellan gum.
  • the extraction of high acyl gellan gum is generally carried out by using alcohol insoluble of high molecular polysaccharide and mixing with a large amount of alcohol solvent and fermentation liquid, and at the same time, dehydration, decolorization and desalting are achieved, and gellan gum precipitation is obtained. This method is simple in process, and the disadvantage is that the solvent recovery cost is high, resulting in high production cost of the entire process.
  • Another gellan gum is a low acyl or deacylated gellan gum which has been removed by extensive alkali treatment at elevated temperatures.
  • This type of gellan gum has excellent gel properties.
  • impurities such as cells and pigments brought by the fermentation liquid are removed to obtain a deacylated transparent gellan gum.
  • the difficulty in extracting and refining the deacylated transparent gellan gum lies in how to clarify the glue and how to obtain the product from the low concentration glue inexpensively.
  • the gel strength of the gellan gum is lowered.
  • the low acyl cold gel As a biomaterial, the low acyl cold gel has been widely welcomed due to its excellent unique performance. However, when it wants to scale into industries related to human life systems (especially food, medicine), it is often necessary to have a low residual organic solvent (such as ethanol, acetone) with low acyl gel.
  • a low residual organic solvent such as ethanol, acetone
  • a gellan gum having the following characteristics: (a) an ethanol residual amount of 200 ppm or less;
  • the gel strength is greater than 1000 g/cm 2 .
  • the gellan gum further has the following characteristics:
  • Transmittance is greater than or equal to 80%.
  • the gellan gum has an ethanol residual amount of 100 ppm, more preferably 50 ppm or less, such as 30-50 ppm.
  • the gellan gum has a light transmittance of greater than or equal to 85%.
  • the gellan gum has a gel strength of greater than or equal to 1050 g/cm 2 , more preferably from 1050 to 1800 g/cm 2 , most preferably from 1100 to 1500 g/cm 2 .
  • the gellan gum has an arsenic content of less than 3 ppm and a lead content of less than 2 ppm.
  • the gellan gum is prepared by the method comprising the following method of the invention.
  • a method of preparing gellan gum comprising the steps of:
  • (a) flocculation the gellan gum fermentation broth is stirred under acidic conditions, so that the gellan gum composition flocculate, forming a raw material liquid containing gellan gum floc, wherein the acidic condition is pH l. 5-4;
  • the method further includes the steps of:
  • the condition of the step (a) is pH 1. 5-4, and the flocculation time is 10-40 minutes.
  • the temperature is normal temperature, such as 4 to 30 ° C, more preferably 15 to 25 ° C.
  • the pH is adjusted to be acidic with hydrochloric acid, sulfuric acid or a combination thereof.
  • the amount of water is from 10 to 20 times the weight of the dehydrated gellan gum filter cake.
  • the step of boiling the glue comprises the following three substeps:
  • the pH adjusting agent comprises a basic adjusting agent and an acidic adjusting agent, wherein the basic adjusting agent is selected from the group consisting of sodium hydroxide, potassium hydroxide, calcium hydroxide, or a combination thereof.
  • a preferred alkaline regulator is sodium hydroxide.
  • the acidic modifier is selected from the group consisting of: hydrochloric acid, sulfuric acid, acetic acid or a combination thereof.
  • a preferred acid regulator is hydrochloric acid.
  • step (e) the temperature of the gutta-permixed mixture is maintained at 70-90 °C.
  • step (e) a filter aid is added to the gutta-permixture and then alkaline filtered.
  • a filter aid is added to the gutta ground mixture, followed by filtration.
  • the filtrate is cooled with a countercurrent coil condenser.
  • the article is selected from the group consisting of:
  • Food beverages, pastries, jams, jellies, synthetic foods, pet food, sugar coatings, icing, milk products, soy products, etc.;
  • FIG. 1 shows a counterflow coil condenser employed in a preferred embodiment of the invention.
  • the inventors have conducted intensive and extensive research to optimize the post-treatment process of the gellan gum fermentation broth, and for the first time, developed a low-cost, high-efficiency preparation of gellan gum under acidic conditions and without the use of organic solvents. New production process.
  • the gellan gum prepared by the novel process of the present invention not only has a very low residual amount of the organic solvent, but also has a markedly improved gel strength.
  • the gellan gum of the present invention means a low residual amount of the organic solvent (e.g., an ethanol residual amount of 200 ppm, preferably 100 ppm, more preferably 50 ppm, most preferably 30 ppm or less), and the gel strength is greater than or Equal to 1000 g/cm 2 (preferably, the gel strength is greater than or equal to 1050 g/cm 2 (such as 1050-1800 g/cm 2 ), and more preferably the gel strength is greater than or equal to 1 100 g/cm 2 (eg 1 Gellan gum of 100-1500 g/cm 2 )). Further, the term also includes gellan gum prepared by the method of the present invention having the above-described low organic solvent residual amount and high gel strength characteristics.
  • the present invention provides a method of producing gellan gum comprising the following steps:
  • (a) flocculation The gellan gum fermentation broth is stirred under acidic conditions to cause the gellan gum component to flocculate to form a raw material liquid containing gellan gum floc, wherein the acidic condition is pH 1.5-4.
  • the acid to be used in the present invention is not particularly limited and may be an organic acid or an inorganic acid, preferably a mineral acid, particularly hydrochloric acid, sulfuric acid or a combination thereof.
  • a preferred method is to add a concentration of 0.5% by weight of hydrochloric acid to the fermentation raw material during the stirring process, thereby flocculation of the gellan gum component to form a raw material liquid containing gellan gum floc.
  • the raw material liquid containing the gellan gum floc is dehydrated (and optionally decolored;) to obtain a dehydrated gellan gum filter cake.
  • the dehydration and/or decolorization can be carried out by a conventional method, for example, by a dewatering press.
  • the dehydrated gellan gum filter cake is mixed with a quantity of water to homogenize to form a homogenate mixture.
  • the amount of water to be added is not particularly limited, and usually 10 to 20 times the weight of the dehydrated gellan gum filter cake, a little more water may be added.
  • Homogenization can be carried out by methods and equipment conventional in the art.
  • the dehydrated gellan gum filter cake is mixed with water by a beater to form a paste-like homogenate mixture (also referred to as a paste liquid;).
  • the pH of the homogenate mixture is adjusted to near neutral (pH 6-8), and the glue is heated (eg 70-90)
  • the step of boiling the glue comprises the following three substeps:
  • This three-step cooking step helps to further increase the gel strength of the gellan gum.
  • the pH adjusting agent may be various pH adjusting agents conventional in the art.
  • alkaline regulators include, but are not limited to;: sodium hydroxide, potassium hydroxide, hydrogen peroxide Calcium, or a combination thereof.
  • a preferred alkaline regulator is sodium hydroxide.
  • acidic modifiers include, but are not limited to;: hydrochloric acid, sulfuric acid, acetic acid, or a combination thereof.
  • a preferred acid regulator is hydrochloric acid.
  • the boiled mixture is filtered while hot to obtain a filtrate containing gellan gum.
  • the filtration can be carried out by various conventional means and equipment in the art. As the temperature is low, the gellan gum will solidify, so the temperature of the boiling mixture should be kept high during filtration (usually 70-90)
  • filter aid may be added to the gutta-per blend mixture prior to filtration.
  • filter aids include, but are not limited to;: diatomaceous earth, perlite, or combinations thereof.
  • 0.8 to 3.0% by weight of a filter aid is added to the mash mixture, followed by filtration.
  • the temperature is lowered to 20-45 ° C, so that the gellan gum gels to form a liquid containing gelatinous gellan gum.
  • the temperature of the filtrate can be lowered by a conventional method to effect gelation.
  • a preferred way is to use a coil condenser, especially a counterflow coil condenser.
  • the liquid material i.e., the filtrate containing gellan gum
  • the liquid material enters the condenser from the liquid feed inlet 10 above the condenser, after cooling, from the condenser.
  • the lower liquid material outlet 20 flows out; and the cooling water enters from the lower cooling water inlet 30 and flows out from the upper cooling water outlet 40.
  • the liquid containing the gelatinous gellan gum is subjected to extrusion filtration to remove a part of moisture to obtain a gellan gum filter cake.
  • the gelatin cake in the filter cake has a solid content of 15-30%.
  • the method for determining the solid content is determined by a conventional method, such as a method of weight loss by drying (for example, according to the Chinese national standard GB5009.3).
  • pressure filtration can be carried out by a conventional squeezing filter device such as a filter press.
  • Post-treatment steps such as granulation and drying
  • the gellan gum cake can be granulated in a conventional manner to form a granulated material.
  • Granulation can be carried out by methods and apparatus conventional in the art, for example, using a commercially available granulator.
  • the particulate gellan gum material can be dried to obtain a dry gellan gum.
  • -15 ⁇ % ⁇ The moisture content of the dried gellan gum is less than 15wt%, more preferably 0. l-15wt%. Drying can be carried out by methods and apparatus conventional in the art, for example, using various commercially available dryers, especially vacuum dryers.
  • the dried material can also be pulverized to obtain a powdery gellan gum.
  • the pulverization can be carried out by a conventional method and apparatus in the art, for example, using various pulverizers commercially available.
  • the material is subjected to cryogenic jet milling. 01-99wt%, ⁇ 0. 0. 01-99wt%, more preferably 0. 01-99wt%, more preferably 0. 01-99wt%, more preferably 0. 01-99wt%, more preferably 0. 01-99wt%, more preferably 0. 01-99wt%, more preferably 0. 01-99wt%, more preferably 0. L-50wt%.
  • Representative gellan gum products include (but are not limited to;):
  • Food beverages, pastries, jams, jellies, synthetic foods, pet food, sugar coatings, icing, milk products, or soy products;
  • the low acyl cold gel which can be obtained by the method of the invention has the characteristics of high purity, high content, low bacterial quantity, and low process cost.
  • the main advantages of the invention include:
  • the organic solvent residue index is very low. Specifically, except for a trace amount or a small amount of ethanol contained in the fermentation liquid, the residue remains in the gellan gum product, and no exogenous organic solvent is added, so the organic solvent content is extremely low, for example, the residual amount of ethanol is less than 100 ppm. More preferably less than 50 ppm. This greatly improves the safety of the gellan gum of the present invention.
  • the flocculation step is carried out under acidic conditions, effectively avoiding the alkali substance being strong against the gellan gum gel
  • the negative effect of the degree effectively improves the gel strength of the gellan gum.
  • gellan gum is very sensitive to alkali.
  • the alkali-free treatment is used to transform the gellan gum under the condition of no damage, so that the product not only has a great improvement in purity and content, Moreover, there is a significant increase in gel strength.
  • the boiling step of the present invention helps to further increase the gel strength of the gellan gum.
  • the fermentation stock solution containing gellan gum was obtained in a conventional manner (e.g., the method described in Example 1 of Chinese Patent Application No. 00125858.
  • the gellan gum was prepared according to the following process:
  • the flocculated feed liquid is pumped into a continuous dewatering press to obtain a filter cake having a water content of about 15 to 30%.
  • Granulation The filter cake is transferred from the conveyor belt into the granulator to form a granular gellan gum gel.
  • Drying The granulated material is fed into a vacuum dryer to obtain a dried gellan gum with a moisture content of ⁇ 15%.
  • the gellan gum No. 1, prepared in Example 1, was measured for its performance by a conventional method.
  • Example 1 was repeated except that the conditions of the cooking step were as follows: The pH of the homogenate mixture was adjusted to pH 6-8, and heated to 70-85 ° C, and the gel was boiled for 5 to 15 minutes to obtain a gutta-percha.
  • the gellan gum No. 2 was tested in the same manner as in Example 2. The results showed that the characteristics were basically the same as those of the gellan gum No. 1, wherein the residual amount of ethanol was not detected (Oppm;), and the gel strength was 1070 g/ Cm 2 .
  • Example 4
  • the pH is 2.0, the pH is 3. 0, or the pH is 4.0.
  • the reaction is repeated as follows: 1.
  • the pH is 2.0, the pH is 3. 0, or the pH is 4.0.
  • the gellan gum No. 3-5 was tested in the same manner as in Example 2. The results showed that the characteristics were basically the same as those of the gellan gum No. 1, wherein the residual amount of ethanol was not detected (Oppm), and the gel strength was 1050- Between 1 100 g/cm 2 .
  • Example 5
  • Example 1 was repeated except that the filtration step conditions were as follows: No filter aid perlite was added, and 2% diatomaceous earth was added as a filter aid.
  • the gellan gum Nos. 6 and 7 were tested in the same manner as in Example 2. The results showed that although the filtration effect of adding the filter aid was better than that of the filter without the addition of the filter aid, the characteristics and knot of the gellan gum obtained were obtained.
  • Cold glue No. l is basically the same, in which the residual amount of ethanol is not detected (0 ppm), and the gel strength is between 1050 and 1 100 g/cm 2 .
  • Example 7 The gellan gum No. 1 obtained in Example 1 was added to the raw material in a usual manner to obtain a beverage product and a jelly product having a gellan gum content of from 1 to 20% by weight.
  • Example 7 The gellan gum No. 1 obtained in Example 1 was added to the raw material in a usual manner to obtain a beverage product and a jelly product having a gellan gum content of from 1 to 20% by weight.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
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  • Engineering & Computer Science (AREA)
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  • Biochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Wood Science & Technology (AREA)
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  • Pharmacology & Pharmacy (AREA)
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  • Inorganic Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Molecular Biology (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Engineering & Computer Science (AREA)
  • Genetics & Genomics (AREA)
  • Jellies, Jams, And Syrups (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

L'invention concerne une nouvelle gomme gellane, son procédé de préparation et son utilisation. La gomme gellane selon l'invention présente un niveau d'éthanol résiduel inférieur ou égal à 200 ppm et une résistance de gel supérieure à 1 000 g/cm2.
PCT/CN2007/070027 2007-05-18 2007-05-18 Gomme gellane organique sans solvant et son procédé de préparation WO2008141507A1 (fr)

Priority Applications (1)

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PCT/CN2007/070027 WO2008141507A1 (fr) 2007-05-18 2007-05-18 Gomme gellane organique sans solvant et son procédé de préparation

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PCT/CN2007/070027 WO2008141507A1 (fr) 2007-05-18 2007-05-18 Gomme gellane organique sans solvant et son procédé de préparation

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103146778A (zh) * 2013-03-02 2013-06-12 安徽龙津生物科技有限公司 一种结冷胶的制备方法
CN115975320A (zh) * 2023-01-10 2023-04-18 青岛振昌工贸有限公司 一种塑料包装袋及其制备工艺

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5580975A (en) * 1993-07-23 1996-12-03 Od Kikaku Co., Limited Agent for keeping cut flowers fresh
JPH11341955A (ja) * 1998-06-02 1999-12-14 Nisshin Oil Mills Ltd:The 改質ジェランガムおよびその製造方法
CN1351172A (zh) * 2000-10-26 2002-05-29 上海众伟生化有限公司 新的微生物多糖结冷胶生产工艺
CN1766120A (zh) * 2004-10-28 2006-05-03 上海和羲生物科技有限公司 一种低酰基透明结冷胶的生产方法
CN101062957A (zh) * 2006-04-24 2007-10-31 上海众伟生化有限公司 无有机溶剂结冷胶及其生产工艺

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5580975A (en) * 1993-07-23 1996-12-03 Od Kikaku Co., Limited Agent for keeping cut flowers fresh
JPH11341955A (ja) * 1998-06-02 1999-12-14 Nisshin Oil Mills Ltd:The 改質ジェランガムおよびその製造方法
CN1351172A (zh) * 2000-10-26 2002-05-29 上海众伟生化有限公司 新的微生物多糖结冷胶生产工艺
CN1766120A (zh) * 2004-10-28 2006-05-03 上海和羲生物科技有限公司 一种低酰基透明结冷胶的生产方法
CN101062957A (zh) * 2006-04-24 2007-10-31 上海众伟生化有限公司 无有机溶剂结冷胶及其生产工艺

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Title
LI H. ET AL.: "A review of research on gellan gum", FOOD AND DRUG, vol. 7, no. 12, December 2005 (2005-12-01), pages 3 - 7 *
LIU L. ET AL.: "The Property and Application of Novel Microbial Exocellular Polysaccharide Gellan Gum", SICHUAN FOOD AND FERMENTATION, no. 1, February 2006 (2006-02-01), pages 28 - 31 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103146778A (zh) * 2013-03-02 2013-06-12 安徽龙津生物科技有限公司 一种结冷胶的制备方法
CN115975320A (zh) * 2023-01-10 2023-04-18 青岛振昌工贸有限公司 一种塑料包装袋及其制备工艺
CN115975320B (zh) * 2023-01-10 2024-05-24 青岛振昌工贸有限公司 一种塑料包装袋及其制备工艺

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