An improved method for extracting high-acyl tri-gluconate and tri-gluconate products

Abstract

The invention belongs to the technical field of extraction after microbial fermentation, and particularly relates to an improved high-acyl tri-gluconate extraction method and a tri-gluconate product. The extraction method comprises the following steps: firstly adjusting the pH value of the fermentation liquid to 1.5-2.0 with an acidic regulator, collecting precipitates, soaking the obtained precipitates with anhydrous ethanol, adjusting the pH value of the material system to 7.0-8.0 with a NaOH solution, and the product begins to precipitate, and the obtained precipitates are washed again with an ethanol system with a purity of 95%, and plate-frame separation is performed again, and the obtained wet materials are wet-crushed, and the wet materials are dried at 55-75° C. to a water content of 8-15%, and the dried product is crushed, and the tri-gluconate product is obtained by sieving. The tri-gluconate product obtained by the invention has the advantages of high yield, high acyl content, high gel strength, good suspension performance, low total bacterial count, low impurity ash content, high product qualification rate, and the like.

Description

Technical Field

[0001] The invention belongs to the technical field of extraction after microbial fermentation, and in particular relates to an improved high-acyl tri-gluconate extraction method and a tri-gluconate product. Background Art

[0002] With the rapid development of modern industry and scientific research, microbial polysaccharides have become the focus of attention of many industries due to their unique physical and chemical properties and wide application potential. Sphingosine gum is a type of polysaccharide synthesized by Sphingomonas as the main producing bacteria. Typical sphingosine gums include gellan gum, welan gum and diutan gum. Similar main chain structures and different side chain groups give sphingosine gums similar excellent properties and each has unique physical properties. Sanzan gum is the first new variety of sphingosine gum independently developed in China. Its main chain structure is different from other sphingosine gums and is composed of glucose, glucuronic acid, mannose and rhamnose. Sanzan gum has excellent properties and can be used as a thickener, suspending agent and emulsifier in petroleum, food and daily chemicals. However, there are many problems to be solved in the existing method of extracting Sanzan gum from fermentation broth.

[0003] The invention patent with application number CN201911131488.0 discloses an improved method for extracting tri-gluconate. In the invention, the fermentation liquid is added with one of hydrogen peroxide, sodium hypochlorite, peracetic acid or a combination thereof for temperature treatment, and an ethanol solution is added during drying. Before the extraction, the pipes and equipment in contact with the material are disinfected. The above technical means are adopted to control the total colony count of the prepared tri-gluconate product to below 5000 CFU / g; after the settled material is neutralized to pH=6.5-7.5, sodium chloride and potassium chloride are added to the material, and the metallic sodium or potassium ions are combined with the molecules to greatly improve the viscosity of the 1% aqueous solution of the tri-gluconate product to above 900 mPa·s.

[0004] The invention patent with application number CN202110530286.4 discloses a method for extracting Sanzan gum from fermentation broth. The invention utilizes the comprehensive effects of mother liquor, ethanol, acid, alkali, salt and other specific means to prepare Sanzan gum products with the advantages of high gel strength, high product viscosity, high product qualification rate, low total colony count, stable whiteness and low production cost.

[0005] However, Sanzuan gum has the characteristic of high viscosity at low concentrations. The viscosity of the fermentation broth containing Sanzuan gum often reaches more than 3000cp. The bacteria are tightly wrapped in the Sanzuan gum. In addition, there are still unconsumed components in the culture medium (including reducing sugars, inorganic salt ions, organic extracts, etc.) remaining in the fermentation broth, as well as various metabolites produced by the growth of bacteria during the fermentation process. It is difficult to remove the bacteria in Sanzuan gum and obtain a Sanzuan gum product with a higher acyl retention degree.

[0006] The extraction process of the above invention patents is also relatively extensive, and lacks precise control in the impurity removal link, resulting in a high impurity content in the final product, which not only affects the performance of Sanzan gum itself, but may also cause adverse consequences such as food spoilage and reduced drug stability during the application process; moreover, the acyl content is an important indicator that determines the gel strength of Sanzan gum. The traditional method fails to fully consider the stability of the acyl group when adjusting the pH of the system, and acyl group loss occurs frequently, which greatly reduces the gel strength of Sanzan gum and cannot meet the strict standards of high-end applications; furthermore, the yield problem has always been a bottleneck restricting the large-scale industrial production of Sanzan gum. Due to the imprecise control of the conditions in the precipitation step, the precipitation of Sanzan gum is often incomplete, a large amount of effective ingredients are lost, and the production cost rises accordingly, which seriously weakens the market competitiveness of the product; in addition, microbial contamination is also a major hidden danger. The residual bacteria in the crude product not only threaten the quality and safety of the product, but may also cause problems such as excessive microorganisms during subsequent storage and use. Summary of the invention

[0007] The main technical problem to be solved by the present invention is to provide an improved method for extracting high-acyl trisammonium gum, which can obtain trisammonium gum products simply, quickly, safely and efficiently, greatly improve the yield, well maintain the acyl content, significantly enhance the gel strength, have excellent suspension performance, significantly reduce the total number of colonies, have very little impurity ash, and have a high product qualification rate.

[0008] In order to solve the above technical problems, the present invention provides the following technical solutions: An improved method for extracting high acyl trisammonium gum comprises the following steps: A: adjusting the pH value of the Sphingomonas T-3 fermentation broth to 1.5-2.0 using an acidic regulator to obtain a mixed solution; In this step, the acyl structure of trisammonium gum can be protected because when the pH value is greater than 2, incomplete precipitation will seriously affect the yield of trisammonium gum.

[0009] B: After adjusting the pH value, the mixed solution is filtered through a plate and frame filter press to collect the precipitate, which is a fibrous material mass; C: Soaking the obtained fibrous material mass in anhydrous ethanol, the volume of the ethanol used being 75% of the volume of the initial extraction fermentation liquid, to obtain a material system; In this step, the water-soluble impurities and alcohol-soluble impurities in the system are fully dissolved, aiming to remove salt and impurities, while killing bacteria and ensuring product purity.

[0010] D: Use NaOH solution to adjust the pH value of the material system to 7.0-8.0, at which time the product begins to precipitate, and the precipitate is taken out through a plate and frame filter press; In this step, plate and frame filtration allows some impurities and bacteria to be removed along with the ethanol solution, which preliminarily improves the purity of Sanzan gum. The pH value of the material system is adjusted to the range of 7.0-8.0, avoiding the deacylation phenomenon caused by the pH value being greater than 8, which would damage the product performance.

[0011] E: Soak the obtained precipitate in 95% ethanol, the volume of ethanol used is 25% of the volume of the initial extraction fermentation liquid, to obtain a mixed solution; In this step, salt, impurities, and residual bacteria are further removed thoroughly, which can not only perform secondary sterilization, but also further effectively remove residual impurities and bacteria.

[0012] F: After the mixed liquid is separated through a plate frame, the obtained wet material is wet crushed; G: The obtained wet material is dried at 55-75°C to a moisture content of 8-15% to obtain a dried product; In this step, the control of temperature range is very important. Once the temperature is too high, the solubility of Sanzan glue will be affected.

[0013] H: The obtained dried product is crushed and then sieved to obtain the Sanzan gum product.

[0014] The following is a further optimization of the above technical solution by the present invention: In step A, the acidic regulator is a solution of hydrochloric acid and acetic anhydride mixed in a volume ratio of 70-90:30-10.

[0015] Further optimization: In step A, use a PTFE-lined stirring device to stir continuously for 30 minutes to ensure uniform mixing.

[0016] In this step, the use of PTFE-lined stirring equipment can effectively remove heavy metals and avoid heavy metal contamination of the product.

[0017] Further optimization: In step C, the ethanol concentration in the material system was adjusted to 85-91.6% (v / v).

[0018] Further optimization: In step D, the concentration of the NaOH solution is 2 mol / L.

[0019] Further optimization: In step E, the mixture was stirred for 30 min, and the ethanol concentration in the mixture was adjusted to 80-87.6% (v / v).

[0020] Further optimization: In step H, the crushed dried product is sieved using an 80-mesh sieve.

[0021] The present invention also provides a Sanzan gum product, which is prepared by the above method; the Sanzan gum product has the following parameter indicators: acetyl content: 7.56-8.53%, glycerol acyl content: 12.67-14.97%, gel strength: 143.56-187.21g / cm 2 , total colony count: 679-891 CFU / g, ash content: 9.76-10.21%.

[0022] The present invention adopts the above-mentioned technical scheme, and the prepared Sanzan gum product has significant advantages over the traditional method, the yield is greatly improved, the acyl content is relatively high, the purity is high, the suspension and viscosity are high, the gel strength is significantly enhanced, the total colony count is significantly reduced, the impurity ash content is extremely small, the product qualification rate is high, and the final product is a Sanzan gum powder finished product that meets the standard specifications, which can meet the strict requirements of various high-end application fields on the quality of Sanzan gum, can be put into use directly or be compounded with other materials and applied to dairy products, beverages, meat products and other food fields, and has immeasurable value in production practice and actual application.

[0023] The present invention is further described below in conjunction with the accompanying drawings and embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 The following is a comparison chart of parameters of products extracted from the embodiments of the present invention and the comparative examples. DETAILED DESCRIPTION

[0025] The extraction method of the present invention is further described in detail below through specific examples, but the present invention is not limited to these examples.

[0026] Unless otherwise specified, the experimental methods used in the following examples are all conventional methods, and the materials, reagents, etc. used in the following examples are all commercially available unless otherwise specified.

[0027] Example 1 This embodiment provides a method for extracting a Sanzan gum product of the present invention, comprising the following steps: (1) Using a PTFE-lined stirring device to stir the Sphingomonas T-3 fermentation liquid and slowly adding an acidic regulator thereto to adjust the pH value of the fermentation liquid, during the stirring process, continuously monitoring the pH value until it reaches 1.8, and using a PTFE-lined stirring device to stir for 30 minutes to ensure that the mixed liquid is evenly mixed.

[0028] In step (1), the acidic regulator is prepared by mixing hydrochloric acid and acetic anhydride in a volume ratio of 80:20 (v / v).

[0029] (2) The mixed solution of step (1) is separated by a plate and frame filter press, and the precipitate is collected, wherein the precipitate is a fibrous material agglomerate.

[0030] (3) The fibrous material mass obtained in step (2) is transferred to a container containing anhydrous ethanol, wherein the volume of the anhydrous ethanol is 75% of the volume of the initial extracted fermentation liquid, and the whole system is stirred to be evenly dispersed, and the ethanol concentration in the material system is adjusted to 91.6% (v / v).

[0031] (4) Add a 2 mol / L NaOH solution to the system of step (3) while stirring until the pH value of the system stabilizes at 7.5.

[0032] (5) After the precipitation in step (4) is complete, the mixture is filtered again through a plate and frame filter press to collect the precipitate, which is a fibrous material mass.

[0033] (6) Soak the fibrous material mass obtained in step (5) in 95% ethanol, the volume of ethanol being 25% of the volume of the initial extraction fermentation liquid, stirring the mixed liquid for 30 minutes, and adjusting the ethanol concentration in the mixed liquid to 87.6% (v / v).

[0034] (7) After the mixed liquid in step (6) is separated by a plate frame, the obtained wet material is wet-crushed.

[0035] (8) The wet material obtained in step (7) is placed in an oven at 65° C. and dried to a moisture content of 12% to obtain a dried product.

[0036] (9) The dried product obtained in step (8) is crushed and then passed through an 80-mesh sieve to obtain a Sanzan glue product.

[0037] The initial extraction fermentation broth in step (3) and step (6) refers to the Sphingomonas T-3 fermentation broth in step (1).

[0038] Example 2 This embodiment provides a method for extracting the tri-zan gum product of the present invention, which is as follows: (1) Using a PTFE-lined stirring device to stir the Sphingomonas T-3 fermentation liquid and slowly adding an acidic regulator thereto to adjust the pH value of the fermentation liquid, during the stirring process, continuously monitoring the pH value until it reaches 1.5, and using a PTFE-lined stirring device to stir for 30 minutes to ensure that the mixed liquid is evenly mixed.

[0039] In step (1), the acidity regulator is prepared by mixing hydrochloric acid and acetic anhydride in a volume ratio of 90:10 (v / v).

[0040] (2) The mixed solution of step (1) is separated by a plate and frame filter press, and the precipitate is collected, wherein the precipitate is a fibrous material agglomerate.

[0041] (3) The fibrous material mass obtained in step (2) is transferred to a container containing anhydrous ethanol, wherein the volume of the anhydrous ethanol is 75% of the volume of the initial extracted fermentation liquid, and the whole system is stirred to be evenly dispersed, and the ethanol concentration in the material system is adjusted to 90.4% (v / v).

[0042] (4) Add a 2 mol / L NaOH solution to the system of step (3) while stirring until the pH value of the system stabilizes at 7.2.

[0043] (5) After the precipitation in step (4) is complete, the mixture is filtered again through a plate and frame filter press to collect the precipitate, which is a fibrous material mass.

[0044] (6) Soak the fibrous material mass obtained in step (5) in 95% ethanol, the volume of ethanol being 25% of the volume of the initial extracted fermentation liquid, stirring the mixed liquid for 30 minutes, and adjusting the ethanol concentration in the mixed liquid to 85.8% (v / v).

[0045] (7) After the mixed liquid in step (6) is separated by a plate frame, the obtained wet material is wet-crushed.

[0046] (8) The wet material obtained in step (7) is placed in an oven at 65° C. and dried to a moisture content of 10% to obtain a dried product.

[0047] (9) The dried product obtained in step (8) is crushed and then passed through an 80-mesh sieve to obtain a Sanzan glue product.

[0048] The initial extraction fermentation broth in step (3) and step (6) refers to the Sphingomonas T-3 fermentation broth in step (1).

[0049] Example 3 (1) Using a PTFE-lined stirring device to stir the Sphingomonas T-3 fermentation liquid and slowly adding an acidic regulator thereto to adjust the pH value of the fermentation liquid, during the stirring process, continuously monitoring the pH value until it reaches 2, and using a PTFE-lined stirring device to stir for 30 minutes to ensure that the mixed liquid is evenly mixed.

[0050] In step (1), the acidity regulator is prepared by mixing hydrochloric acid and acetic anhydride in a volume ratio of 70:30 (v / v).

[0051] (2) The mixed solution of step (1) is separated by a plate and frame filter press, and the precipitate is collected, wherein the precipitate is a fibrous material agglomerate.

[0052] (3) The fibrous material mass obtained in step (2) is transferred to a container containing anhydrous ethanol, wherein the volume of the anhydrous ethanol is 75% of the volume of the initial extracted fermentation liquid, and the whole system is stirred to be evenly dispersed, and the ethanol concentration in the material system is adjusted to 85% (v / v).

[0053] (4) Add a 2 mol / L NaOH solution to the system of step (3) while stirring until the pH value of the system stabilizes at 7.8.

[0054] (5) After the precipitation in step (4) is complete, the mixture is filtered again through a plate and frame filter press to collect the precipitate, which is a fibrous material mass.

[0055] (6) Soak the fibrous material mass obtained in step (5) in 95% ethanol, the volume of ethanol being 25% of the volume of the initial extraction fermentation liquid, stirring the mixed liquid for 30 minutes, and adjusting the ethanol concentration in the mixed liquid to 80% (v / v).

[0056] (7) After the mixed liquid in step (6) is separated by a plate frame, the obtained wet material is wet-crushed.

[0057] (8) The wet material obtained in step (7) is placed in an oven at 65° C. and dried to a moisture content of 14% to obtain a dried product.

[0058] (9) The dried product obtained in step (8) is crushed and then passed through an 80-mesh sieve to obtain a Sanzan glue product.

[0059] The initial extraction fermentation broth in step (3) and step (6) refers to the Sphingomonas T-3 fermentation broth in step (1).

[0060] Comparative Example 1 This comparative example provides a method for extracting trisammonia gum (refer to CN110760015B), which is as follows: (1) Add 30% hydrogen peroxide solution to the fermentation broth in an amount of 0.02% (m / m) of the fermentation broth, stir evenly, and then heat the fermentation broth in a water bath to a material temperature of 70°C.

[0061] (2) Adjust the pH to 2.05 with 6 mol / L hydrochloric acid.

[0062] (3) Separating the sedimentation liquid to obtain fibrous material agglomerates.

[0063] (4) Slowly add sodium carbonate powder to the agglomerate auxiliary material obtained in step 3 and continuously stir to form a uniform paste material until the pH value of the material reaches 7.18, and then add 0.5% (m / m) sodium chloride to the paste material.

[0064] (5) Add 75% ethanol solution to the material in step 4 above, with the added amount being 0.5% (m / m) of the above material. During the entire experiment, all experimental tools and instruments were wiped clean with 75% ethanol disinfectant alcohol cotton.

[0065] (6) 105°C, drying time 6 h until the material is dry and there is no sticky part.

[0066] The product was crushed and sieved to obtain the product under 80 mesh.

[0067] Comparative Example 2 This comparative example provides a method for extracting triazole gum (refer to CN113248629B), which is as follows: (1) Add potassium chloride (in the form of an aqueous solution) equivalent to 0.7% (m / m) of the fermentation broth, stir evenly, and let stand for 20 minutes.

[0068] (2) Add 85.2% (v / v) ethanol solution to the solution obtained in step (1) until the alcohol content in the raw material solution reaches 35±5% (v / v).

[0069] (3) Add 6 mol / L hydrochloric acid solution to the solution obtained in step (2), stir and measure the pH value of the material to 1.58, and obtain a sedimentation liquid containing fibrous material.

[0070] (4) Separating the sedimentation liquid to obtain fibrous material agglomerates and mother liquor.

[0071] (5) Add 900 mL of 85.2% (v / v) ethanol solution to the 200 g material mass obtained in step (4), stir to adjust the ethanol concentration in the material to 75.2% (v / v), and soak for 30 minutes.

[0072] (6) Add 40% (m / v) KOH solution to the material obtained in step (5) above, adjust the pH value of the material to 7.79, and the ethanol concentration to 74.8% (v / v).

[0073] (7) Separating the above materials to obtain a fibrous wet product and a mother liquor.

[0074] (8) 105°C, drying time 4h.

[0075] (9) The mother liquor obtained from the above two separations was distilled by a rotary evaporator at a distillation temperature of 45° C. and a vacuum degree of -0.08 to -0.10 MPa. The ethanol content of the distillate after cooling was determined to be 85.2% (v / v). The mother liquor can be recycled and reused in the extraction of trisammonia gum.

[0076] (10) The product after crushing and drying is sieved to obtain the finished product of 80 mesh sieve.

[0077] Comparative Example 3 This comparative example provides a method for extracting trisammonia gum (refer to CN110760015B), which is as follows: A, after the fermentation is completed, a 30% concentration of hydrogen peroxide solution is added to the fermentation broth, the amount of the above materials added is 0.02% of the mass of the fermentation broth, and then the temperature is raised to 70 ℃; B. After the fermentation liquid is heated in step A, the isoelectric point is adjusted, and a fibrous material is obtained by sedimentation extraction. The pH value of the fibrous material is adjusted to 6.5-7.5, and 0.5% by weight of sodium chloride is added to the above material; C. Add 0.5% of ethanol solution by weight to the material prepared in step B, dry and crush to prepare Sanzan glue, wherein the volume percentage concentration of the ethanol solution is 70%-75%.

[0078] In order to ensure the cleanliness of the equipment and avoid the invasion of miscellaneous bacteria during the extraction process to reduce product quality, the preferred technical solution is to disinfect the pipe wall and equipment for conveying materials before the extraction begins.

[0079] The preferred technical solution is that the conditions for disinfecting the pipe wall for conveying materials are: steam temperature 121°C-123°C, time 15-20 minutes.

[0080] A more preferred technical solution is to sterilize the equipment for conveying materials with an ethanol solution having a volume percentage concentration of 70%-75%.

[0081] Experimental example This experimental example uses the following method to measure the finished products (products) obtained in the above embodiments and comparative examples: 1. Determination of product acyl content 1. Instruments and equipment a) Analytical balance: accurate to 0.001g; b) 50 mL centrifuge tube; c) 4°C refrigerator; d) Large table centrifuge; e) oven; e) High performance liquid chromatograph, Agilent, USA.

[0082] 2. Detection methods and steps (1) Weigh 0.05 g of pure polysaccharide into a 50 mL centrifuge tube and add 10 mL of 0.02 M NaOH alkaline solution to prepare a 0.5% sample alkaline solution; (2) Place the dissolved sample in a constant temperature shaker at 65°C, 200 rpm, and alkalize for 2 h, shaking repeatedly during the process; (3) After alkalization, add 3 volumes of anhydrous ethanol to the system and place it in a refrigerator at 4°C for 1 h; (4) After standing, balance the mixture and centrifuge at 9000 g for 30 min at 4°C. Collect the supernatant in a disposable dish. (5) Place the plate in an oven at 65°C until a white solid is obtained; (6) Add 0.3 mol / L HCl solution to adjust the pH value of the sample to acidic, and mix by inversion; (7) Add deionized water to make the volume 1 mL, add 1 mL of propionic acid solution (0.7 g / L) as the internal standard, mix well, filter the sample with a 0.22 μm filter, inject 20 μL of the sample into the sampler, and analyze the sample on an Agilent HPLC instrument.

[0083] 2. Determination of product gel strength 1. Instruments and equipment a) Analytical balance: accurate to 0.001g; b) high-speed agitator; c) 500 mL glass beaker; d) Constant temperature box (temperature range: 5℃~50℃); e) TA.XTC-18 texture analyzer, China Baosheng Technology; f) Water bath (temperature control range: room temperature ~ 100°C).

[0084] 2. Test conditions a) Probe shape and size: P / 0.5 cylindrical probe, contact area 126.68mm 2 ; b) Probe test moving speed: 0.1mm / s.

[0085] 3. Detection methods and steps a) Weigh 2g of sample (accurate to 0.001g), slowly add it into a liquid cup containing 200mL of distilled water under stirring at a speed of 600r / min, and stir for 1h. Pour the sample solution into a beaker, place it in a water bath at 85℃, stir it intermittently with a glass rod for 3 times, take out the beaker after heating for 30min, remove the upper foam, pour the gel solution into a flat-bottomed container while it is hot, with the liquid level at 4cm, let it stand, cool it naturally to gel, put it in a constant temperature box at 25℃ and let it stand for 12h before testing; b) Measure three parallel samples using a texture analyzer and take the arithmetic mean.

[0086] 3. Determination of product suspension performance 1. Instruments and equipment a) Analytical balance: accurate to 0.001g; b) Glass beaker 500 mL; c) high speed stirrer; d) 250mL measuring cylinder; e) Plastic pellets.

[0087] 2. Detection methods and steps (1) Weigh 0.2 g of sample powder and add 199.8 g of distilled water to obtain a 0.1% glue solution; (2) 65°C water bath, stirring at 500 rpm for 30 min; (3) Cool to room temperature and add distilled water until the system weight is 200 g; (4) Adjust the pH to 3.5 with 10% citric acid while stirring; (5) Transfer to a 250 mL measuring cylinder and let stand for at least 4 h; (6) Add a small plastic ball into each measuring cylinder from the same height and let it sit for observation.

[0088] 4. Determination of total colony count of products The total colony count test was carried out in accordance with the method described in the National Food Safety Standard for Food Microbiological Examination of Total Colony Count (GB4789.2-2016). Three parallel samples were taken and the arithmetic mean was calculated.

[0089] 5. Ash content test 1. Instruments and equipment a) Analytical balance: accurate to 0.001g; b) Box-type resistance furnace (muffle furnace); c) Porcelain crucible: 50 mL; d) Hydrochloric acid, nitric acid or hydrogen peroxide solution.

[0090] 2. Detection methods and steps a) First, clean the porcelain crucible that has been boiled in 1:1 hydrochloric acid, place it in a high-temperature furnace and heat it to about 650℃, maintain it for 30 minutes, cool it down slightly, take it out and cool it, and weigh it as W0.

[0091] b) Weigh about 3g of sample into a crucible (flatten the sample after weighing), record the sample mass as W1. Carbonize the sample in an electric furnace until smokeless, transfer it to a 650℃ muffle furnace for ash for 3h. If the ash is not complete, take it out and cool it, add a few drops of nitric acid or hydrogen peroxide, evaporate it and then transfer it to a high-temperature furnace for ash until white, transfer it to a dryer, cool it to room temperature, and weigh it as W2.

[0092] 3. Calculation Ash content (%) = (W2-W0) / W1 W0: mass of the crucible, g W1: mass of sample, g W2: Total mass of crucible and sample after ashing, g Take the arithmetic mean of three parallel samples. The allowable error of the parallel sample results is 0.2%, and the results are rounded to one decimal place.

[0093] The present invention also provides a Sanzan gum product, which is prepared by the above method; the Sanzan gum product has the following parameter indicators: acetyl content: 7.56-8.53%, glycerol acyl content: 12.67-14.97%, gel strength: 143.56-187.21g / cm 2 , total colony count: 679-891 CFU / g, ash content: 9.76-10.21%.

[0094] For those skilled in the art, according to the teachings of the present invention, without departing from the principles and spirit of the present invention, changes, modifications, substitutions and variations made to the implementation methods are still within the protection scope of the present invention.

Claims

1. An improved method for extracting high acyl trisammonium gum, characterized in that: The following steps are involved: A: adjusting the pH value of the Sphingomonas T-3 fermentation broth to 1.5-2.0 using an acidic regulator to obtain a mixed solution; B: After adjusting the pH value, the mixed solution is filtered through a plate and frame filter press to collect the precipitate, which is a fibrous material mass; C: Soaking the obtained fibrous material mass in anhydrous ethanol, the volume of the ethanol used being 75% of the volume of the initial extraction fermentation liquid, to obtain a material system; D: Use NaOH solution to adjust the pH value of the material system to 7.0-8.0, at which time the product begins to precipitate, and the precipitate is taken out through a plate and frame filter press; E: Soak the obtained precipitate in 95% ethanol, the volume of ethanol used is 25% of the volume of the initial extraction fermentation liquid, to obtain a mixed solution; F: After the mixed liquid is separated through a plate frame, the obtained wet material is wet crushed; G: The obtained wet material is dried at 55-75°C to a moisture content of 8-15% to obtain a dried product; H: The obtained dried product is crushed and then sieved to obtain the Sanzan gum product.

2. The improved method for extracting high acyl trisammonium gum according to claim 1, characterized in that: In step A, the acidic regulator is a solution of hydrochloric acid and acetic anhydride mixed in a volume ratio of 70-90:30-10.

3. The improved method for extracting high acyl trisammonium gum according to claim 1, characterized in that: In step A, a PTFE-lined stirring device is used to continuously stir for 30 minutes to ensure uniform mixing.

4. The improved method for extracting high acyl trisammonium gum according to claim 1, characterized in that: In step C, the ethanol concentration in the material system is adjusted to 85-91.6% (v / v).

5. The improved method for extracting high acyl trisammonium gum according to claim 1, characterized in that: In step D, the concentration of the NaOH solution is 2 mol / L.

6. The improved method for extracting high acyl trisammonium gum according to claim 1, characterized in that: In step E, the mixture was stirred for 30 min, and the ethanol concentration in the mixture was adjusted to 80-87.6% (v / v).

7. The improved method for extracting high acyl trisammonium gum according to claim 1, characterized in that: In step H, the crushed dried product is sieved using an 80-mesh screen.

8. A Sanzan glue product, characterized in that: Prepared according to the method described in any one of claims 1 to 7; the Sanzan gel product has the following parameter indicators: acetyl content: 7.56-8.53%, glycerol acyl content: 12.67-14.97%, gel strength: 143.56-187.21g / cm 2 , total colony count: 679-891 CFU / g, ash content: 9.76-10.21%.

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