Polygonatum sibiricum polysaccharide and mulberry composite beverage and preparation method of special stabilizer

Abstract

A preparation method of rhizoma polygonati polysaccharide, a mulberry composite drink and a special stabilizer comprises the following steps: preparation of a rhizoma polygonati polysaccharide extract: drying rhizoma polygonati, crushing, extracting with water, carrying out composite enzymolysis by adopting cellulase, hemicellulase and papain, and carrying out suction filtration, alcohol precipitation, centrifugation and freeze-drying to obtain the polysaccharide extract; the stabilizer is prepared by compounding carboxymethyl cellulose, pectin, sodium hexametaphosphate and sodium tripolyphosphate; the preparation method of the compound beverage comprises the following steps: mixing the rhizoma polygonati polysaccharide extract and the mulberry powder with sodium cyclamate, citric acid and a stabilizer, homogenizing, filtering, sterilizing and the like to obtain a finished product. Polygonatum sibiricum polysaccharide is used for replacing whole polygonatum sibiricum, insoluble substance precipitation is reduced, and the physiological activity of polysaccharide is reserved; the mulberry powder neutralizes the pungent smell of the rhizoma polygonati and improves the flavor and the health-care function; and the stabilizer enhances the stability and taste of the beverage. The obtained beverage is sour, sweet and palatable, uniform in color and stable in tissue state, and has the effects of regulating immunity, improving intestinal flora and the like.

Description

Technical Field

[0001] The present invention relates to a preparation method of polygonatum polysaccharide and its compound drink with mulberry and a special stabilizer. Background Art

[0002] Polygonatum sibiricum, also known as tiger ginger and chicken head ginseng, is the dried rhizome of Polygonatum kingianum Coll. et Hemsl., Polygonatum sibiricum Red. or Polygonatum cyrtonema Hua of the Liliaceae family, and has the functions of replenishing qi and nourishing yin, strengthening the spleen, moistening the lungs, and benefiting the kidney function. Polygonatum sibiricum is rich in natural polysaccharides, which have the effects of regulating intestinal flora, regulating human immune function, reducing blood lipid, and regulating blood pressure.

[0003] Mulberry, also known as mulberry fruit, mulberry kernel, and mulberry fruit, is the fruit spike of Morus alba L. of the Moraceae family, and has the effects of nourishing yin, tonifying the liver, tonifying the kidney, enriching blood, improving eyesight, beautifying hair, treating insomnia and neurasthenia, anti-fatigue, preventing and treating constipation, etc., and is used for yin deficiency of the liver and kidney, dizziness and tinnitus, palpitation and insomnia, early whitening of hair, thirst due to fluid deficiency, internal heat and polydipsia, and intestinal dryness and constipation.

[0004] At present, there are already polygonatum drinks on the market, but their functions are single. Refer to Chinese Patent CN02139736.8. Moreover, the pungent smell of polygonatum makes the flavor of the drink not easily acceptable to consumers. There is a lack of compound polygonatum drinks on the market, and some substances in polygonatum cannot be completely dissolved in water, and a large amount of precipitation will occur when directly made into a drink, affecting the taste of the drink. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a preparation method of polygonatum polysaccharide and its compound drink with mulberry and a special stabilizer. The compound drink prepared by this method has excellent flavor and taste, is beneficial to promoting physical and mental health and regulating intestinal flora, retains both the unique flavor of polygonatum and the physiological functions of polygonatum polysaccharide, and reduces the adverse effects of other components in polygonatum on the tissue state of the drink; the special stabilizer can not only improve the stability of the drink, extend the shelf life of the drink, but also further improve the nutritional value and taste of the drink.

[0006] To solve the above technical problems, the present invention provides a preparation method of polygonatum polysaccharide and its compound drink with mulberry and a special stabilizer, including the following steps:

[0007] (1) Preparation of polygonatum polysaccharide extract:

[0008] Drying: Select fresh polygonatum, wash and cut it into pieces, place it in an oven at 55°C, and dry it for 2 - 3 days until constant weight;

[0009] Crushing: Use a laboratory small crusher to grind the dried polygonatum into fine powder and sieve it;

[0010] Water extraction: Weigh a certain mass of polygonatum powder, add deionized water according to a material-liquid ratio of 1:20, shake well, and let it stand at room temperature for 30 min to obtain a polygonatum mixture;

[0011] Enzymatic hydrolysis: Add cellulase, hemicellulase, and papain to the polygonatum mixture in a mass ratio of 7:8:6, with the total addition amount accounting for 1.5% of the polygonatum mixture. Adjust the enzymatic hydrolysis time to 40 minutes and the enzymatic hydrolysis temperature to 50 °C for extraction to obtain an extract solution;

[0012] Suction filtration: Filter the obtained extract solution twice to obtain a clear filtrate;

[0013] Alcohol precipitation: Add three times the volume of absolute ethanol to the filtrate and place it in a refrigerator at 4 °C overnight;

[0014] Centrifugation: Then place it in a centrifuge and centrifuge at a speed of 5000 r / min for 15 minutes, and take the precipitate;

[0015] Freeze-drying: Freeze-dry the obtained precipitate at -67.4 °C for 3 - 4 days until constant weight to obtain a polygonatum polysaccharide extract for standby;

[0016] (2) Preparation of a special stabilizer:

[0017] By weight: Take 4 parts of carboxymethyl cellulose, 1 part of pectin, 1 part of sodium hexametaphosphate, and 1 part of sodium tripolyphosphate, mix them evenly to obtain a stabilizer for standby;

[0018] (3) Preparation of a compound beverage:

[0019] Stirring and dissolving: Add 1.5 g of polygonatum polysaccharide extract and 12.5 g of mulberry powder to 100 mL of water respectively, and dissolve most of the solids by stirring to obtain a mixed solution;

[0020] Formulation: Weigh 0.14 g of sodium cyclamate, 0.04 g of citric acid, and 0.14 g of stabilizer respectively and add them to the mixed solution prepared in step (1) for blending;

[0021] Homogenization: Homogenize the blended mixed solution. The homogenization conditions are 8000 r / min, for 5 minutes, and homogenize 2 times to make the homogenized liquid have no visible precipitate to the naked eye;

[0022] Filtration: Filter the homogenized liquid. The filtration conditions are 300 mesh, filter 3 times, remove impurities, and collect the filtrate;

[0023] Sterilization: Heat and sterilize the filtrate in a boiling water bath at 100 °C for 30 minutes to obtain the final beverage;

[0024] Cooling, filling, and storage: Cool the beverage to room temperature, fill it, and store it sealed in an environment at 4 °C.

[0025] Advantages of the present invention:

[0026] The preparation method of a polygonatum polysaccharide mulberry composite drink provided by the present invention has convenient and simple steps. The prepared composite drink has excellent flavor and taste, which is beneficial to promoting physical and mental health and regulating the intestinal flora. During the preparation process, due to the insoluble substances in polygonatum, precipitation will occur in the drink, affecting the taste of the drink. Therefore, polygonatum polysaccharide extract is used as an ingredient, which not only retains the unique flavor of polygonatum and the physiological functions of polygonatum polysaccharide, but also reduces the adverse effects of other components in polygonatum on the tissue state of the drink. The addition of mulberry powder can not only neutralize the pungent smell of polygonatum and improve the flavor of the drink, but also complement the efficacy of polygonatum, making the health care function of the drink more perfect. Sodium cyclamate and citric acid are used as flavor enhancers. At the same time, sodium cyclamate can reduce the blood glucose response and calorie intake, and has a certain auxiliary effect on controlling weight and blood glucose.

[0027] All the reagents required in the preparation method of polygonatum polysaccharide extract in the drink are edible substances, which are green and healthy and will not cause damage to the human body.

[0028] The special stabilizer in the drink can not only improve the stability of the drink and extend the shelf life of the drink, but also further improve the nutritional value and taste of the drink. Carboxymethyl cellulose not only acts as a thickener, dispersant and stabilizer, but also has the effect of improving intestinal function and promoting digestion; pectin is a water-soluble dietary fiber, which has thickening and stabilizing effects, and can also aid digestion and reduce cholesterol; sodium hexametaphosphate can increase viscosity, prevent turbidity and precipitation, stabilize natural pigments, protect the color of food and adjust the pH value; sodium tripolyphosphate is used as a moisture retainer, pH regulator and thickener, etc. Brief Description of the Drawings

[0029] Figure 1 It is a diagram showing the effect of polygonatum polysaccharide addition amount on the sensory evaluation of the drink.

[0030] Figure 2 It is a diagram showing the effect of sodium cyclamate addition amount on the sensory evaluation of the drink.

[0031] Figure 3 It is a diagram showing the effect of mulberry powder addition amount on the sensory evaluation of the drink. Detailed Description of the Invention

[0032] The preparation methods of polygonatum polysaccharide and its mulberry composite drink and the special stabilizer include the following steps:

[0033] (1) Preparation of polygonatum polysaccharide extract:

[0034] Drying: Select fresh polygonatum, wash and cut it into pieces, place it in an oven at 55°C, and dry it for 2 - 3 days until constant weight;

[0035] Crushing: Use a laboratory small crusher to grind the dried polygonatum into fine powder and sieve it;

[0036] Water extraction: Weigh a certain mass of polygonatum sibiricum powder, add deionized water at a material-liquid ratio of 1:20, shake well, and let it stand at room temperature for 30 min to obtain a polygonatum sibiricum mixture;

[0037] Enzymatic hydrolysis: Add cellulase, hemicellulase, and papain to the polygonatum sibiricum mixture in a mass ratio of 7:8:6, with the total addition accounting for 1.5% of the polygonatum sibiricum mixture. Adjust the enzymatic hydrolysis time to 40 min and the enzymatic hydrolysis temperature to 50 °C for extraction to obtain an extract;

[0038] Suction filtration: Filter the obtained extract twice to obtain a clear filtrate;

[0039] Alcohol precipitation: Add three times the volume of absolute ethanol to the filtrate and place it in a refrigerator at 4 °C overnight;

[0040] Centrifugation: Then centrifuge it in a centrifuge at a speed of 5000 r / min for 15 min and take the precipitate;

[0041] Freeze-drying: Freeze-dry the obtained precipitate at -67.4 °C for 3 - 4 days until constant weight to obtain polygonatum sibiricum polysaccharide extract for standby;

[0042] (2) Preparation of stabilizer:

[0043] By weight: Take 4 parts of carboxymethyl cellulose, 1 part of pectin, 1 part of sodium hexametaphosphate, and 1 part of sodium tripolyphosphate, mix well to obtain the stabilizer for standby;

[0044] (3) Preparation of compound drink:

[0045] Stir and dissolve: Add 1.5 g of polygonatum sibiricum polysaccharide extract and 12.5 g of mulberry powder to 100 mL of water respectively, and stir to dissolve most of the solids to obtain a mixed solution;

[0046] Blending: Weigh 0.14 g of sodium cyclamate, 0.04 g of citric acid, and 0.14 g of stabilizer respectively and add them to the mixed solution prepared in step (1) for blending;

[0047] Homogenization: Homogenize the blended mixed solution. The homogenization conditions are 8000 r / min, for 5 min, and homogenize twice to make the homogenized liquid have no visible precipitate to the naked eye;

[0048] Filtration: Filter the homogenized liquid. The filtration conditions are 300 mesh, filter 3 times to remove impurities, and collect the filtrate;

[0049] Sterilization: Heat and sterilize the filtrate in a boiling water bath at 100 °C for 30 min to obtain the final drink;

[0050] Cooling, filling, and storage: Cool the drink to room temperature, fill it, and store it sealed in a 4 °C environment.

[0051] In the above embodiments, the method for testing the polysaccharide content in the polygonatum polysaccharide extract is as follows: Dissolve 25 mg of glucose in 50 mL of deionized water. Then, take 0, 0.2, 0.4, 0.6, 0.8, 1.0, 1.2, 1.4, 1.6, 1.8, 2.0 mL and transfer them into 10-mL volumetric flasks. Mix the standard product, phenol, and concentrated sulfuric acid in volumes of 2, 1, and 5 mL respectively, and react at room temperature for 20 min. Measure the absorbance at 490 nm, and take the average value for each group after measuring 3 times. Using the detected mass concentration of glucose as the abscissa and the absorbance as the ordinate, prepare a standard curve y = 0.0135x + 0.1016, R 2 = 0.9986.

[0052] Dissolve the extracted polygonatum polysaccharide in deionized water to prepare a 0.1% (w / v) polysaccharide sample. Mix the sample, phenol, and concentrated sulfuric acid in volumes of 2, 1, and 5 mL respectively, and react at room temperature for 20 min; measure the absorbance at 490 nm, and take the average value for each group after measuring 3 times. The content of polygonatum polysaccharide can be known from the standard curve.

[0053] The formula is: Yield of polygonatum polysaccharide = Polygonatum polysaccharide (g, determined by the phenol-sulfuric acid method) / Polygonatum powder × 100%.

[0054] Table 1 Determination table of polysaccharide content in polygonatum polysaccharide extract

[0055]

[0056] Conduct a sensory evaluation on the prepared polygonatum polysaccharide mulberry composite beverage in this example. The sensory evaluation criteria are shown in Table 2, and the evaluation results are shown in Figures 1 - 3 .

[0057] Table 2 Sensory evaluation criteria for beverages

[0058]

[0059]

[0060] It can be seen from Figure 1 that polygonatum polysaccharide extracts with different masses (1.0%, 1, 5%, 2.0%, 2.5%) are added. When the addition amount of polygonatum polysaccharide extract is 2.0%, the sensory score is the highest, which is 89.93. When the addition amount of polygonatum polysaccharide extract is too low, the beverage is relatively tasteless and has a poor flavor. Continuing to increase the dosage of polygonatum polysaccharide extract will cause an increase in insoluble substances in the beverage, affecting the tissue state and texture. Therefore, select an addition amount of polygonatum polysaccharide extract of 1.0 - 2.0 g / 100 mL for the subsequent orthogonal experiment.

[0061] It can be seen from Figure 2It can be seen that different amounts of sodium cyclamate (0.08%, 0.1%, 0.12%, 0.14%) were added. When the addition amount of sodium cyclamate was 0.12, the sensory score was the highest, reaching 87.75. When the addition amount of sodium cyclamate was too low, the sweetness of the drink was insufficient and the flavor was poor. Continuing to increase the amount of sodium cyclamate would disrupt the sour-sweet balance of the drink, resulting in the drink being overly sweet. Therefore, an addition amount of sodium cyclamate of 0.1 - 0.14 g / 100 mL was selected for the subsequent orthogonal experiment.

[0062] It can be seen from Figure 3 that different amounts of mulberry powder (7.5%, 10.0%, 12.5%, 15.0%) were added. As the addition amount of mulberry powder increased, the difference in the fuzzy mathematics sensory score of the polygonatum polysaccharide - mulberry composite drink was relatively small. Therefore, based on cost savings, an addition amount of mulberry powder of 7.5 - 12.5 g / 100 mL was selected for the subsequent orthogonal experiment.

[0063] On the basis of the single - factor experiment, considering the calculation results of the fuzzy mathematics method, for different amounts of polygonatum polysaccharide, sodium cyclamate, and mulberry powder, the sensory scores of the polygonatum polysaccharide - mulberry composite drink were used to conduct a response surface experimental design with three factors and three levels, and each experiment was repeated 3 times. The experimental factor levels are shown in Table 3.

[0064] Table 3 Orthogonal experiment on the formula of polygonatum polysaccharide - mulberry composite drink

[0065]

[0066] The experimental results of the sensory scores of the polygonatum polysaccharide - mulberry composite drink for different amounts of polygonatum polysaccharide, sodium cyclamate, and mulberry powder are shown in Table 4.

[0067] Table 4 Results of orthogonal experiment and range analysis table.

[0068]

[0069]

[0070] According to Table 4, the range RC > RB > RA, indicating that the order of the influence of the above three factors on the score of the compound drink of polygonatum polysaccharide and mulberry is: C > B > A, that is, the amount of mulberry powder used has the greatest influence on the comprehensive score of the compound drink of polygonatum polysaccharide and mulberry, followed by sodium cyclamate, and polygonatum polysaccharide has the least influence. For factor A, k3 > k2 > k1, indicating that when the amount of polygonatum polysaccharide is 1.5 g / 100 mL, the comprehensive score of the compound drink of polygonatum polysaccharide and mulberry is the highest; for factor B, k3 > k2 > k1, indicating that when the amount of sodium cyclamate is 0.14 g / 100 mL, the comprehensive score of the compound drink of polygonatum polysaccharide and mulberry is the highest; for factor C, k3 > k2 > k1, indicating that when the amount of mulberry powder is 12.5 g / 100 mL, the comprehensive score of the compound drink of polygonatum polysaccharide and mulberry is the highest. The optimal combination of the three factors is A3B3C3, that is, when the amount of polygonatum polysaccharide is 1.5 g / 100 mL, the amount of sodium cyclamate is 0.14 g / 100 mL, and the amount of mulberry powder is 12.5 g / 100 mL. A3B3C3 does not appear in the orthogonal experiment combination, and a comparative experiment is carried out with the combination A3B3C2 with the highest score in the 9 orthogonal experiments. Finally, the best combination of the compound drink of polygonatum polysaccharide and mulberry is determined to be A3B3C3.

[0071] Table 5 Microbiological indicators of the compound drink of polygonatum polysaccharide and mulberry.

[0072] Serial number Detection index Method standard 1 Total number of colonies GB 4789.2 - 2022 2 Escherichia coli GB 4789.3 - 2016 3 Salmonella GB 4789.4 - 2024

[0073] Table 6 Microbiological indicators and results.

[0074] Project Index Result Total number of colonies 100 7CFU / mL Escherichia coli ≤0.3 Not detected Salmonella Not to be detected Not detected

[0075] The total number of colonies and coliforms in the compound drink of polygonatum polysaccharide and mulberry of this product meet the requirements of the National Food Safety Standard Beverage (GB 7101-2022), and no pathogenic bacteria are detected.

[0076] Table 7 Determination methods and results of physical and chemical indicators.

[0077] Project Method Content Total acid GB 12456—2021 0.91g / L Total sugar Phenol - sulfuric acid method 1.3mg / mL Total phenol Folin - Ciocalteu method 230.46μg GAE / mL Anthocyanin pH differential method 0.46mg / mL Flavonoid Spectrophotometry 1.49mg / mL

[0078] The pH value of the compound drink of polygonatum polysaccharide and mulberry is 3.85, the precipitation rate is 0.0672%, the total number of colonies is 6.7 CFU / mL, the total phenol content is 230.46 μg GAE / mL, the anthocyanin content is 4.62 mg / L, the total acid content is 0.91 g / L, the total sugar content is 1.3 mg / mL, and the total flavonoid content is 1.49 mg / mL. All physical and chemical indicators meet the national standards. The color is dark purple-red, the flavor is good, the taste is fresh and refreshing, the sweetness and sourness are moderate, the nature is stable, and it is clear and non-turbid.

Claims

1. Preparation method of polygonatum polysaccharide and mulberry composite drink and special stabilizer, characterized in that, It includes the following steps: (1) Preparation of polygonatum polysaccharide extract: Drying: Select fresh polygonatum, wash and cut it into pieces, place it in an oven at 55 °C, and dry for 2 - 3 days until constant weight; Crushing: Use a small laboratory crusher to grind the dried polygonatum into fine powder and sieve it; Water extraction: Weigh a certain mass of polygonatum powder, add deionized water at a material - to - liquid ratio of 1:20, shake well, and let it stand at room temperature for 30 min to obtain a polygonatum mixture; Enzymatic hydrolysis: Add cellulase, hemicellulase, and papain to the polygonatum mixture in a mass ratio of 7:8:6, with the total addition accounting for 1.5% of the polygonatum mixture. Adjust the enzymatic hydrolysis time to 40 min and the enzymatic hydrolysis temperature to 50 °C for extraction to obtain an extract; Suction filtration: Filter the obtained extract twice to obtain a clear filtrate; Alcohol precipitation: Add three - fold volume of absolute ethanol to the filtrate and place it in a refrigerator at 4 °C overnight; Centrifugation: Then centrifuge it in a centrifuge at a speed of 5000 r / min for 15 min and take the precipitate; Freeze - drying: Freeze - dry the obtained precipitate at - 67.4 °C for 3 - 4 days until constant weight to obtain the polygonatum polysaccharide extract for standby; (2) Preparation of a special stabilizer: By weight: Take 4 parts of carboxymethyl cellulose, 1 part of pectin, 1 part of sodium hexametaphosphate, and 1 part of sodium tripolyphosphate, mix them evenly to obtain the stabilizer for standby; (3) Preparation of the compound beverage: Stirring and dissolving: Add 1.5 g of polygonatum polysaccharide extract and 12.5 g of mulberry powder to 100 mL of water respectively, and stir to dissolve most of the solids to obtain a mixed solution; Formulation: Weigh 0.14 g of sodium cyclamate, 0.04 g of citric acid, and 0.14 g of stabilizer and add them to the mixed solution prepared in step (1) for blending; Homogenization: Homogenize the blended mixed solution. The homogenization conditions are 8000 r / min for 5 min, and homogenize twice to make the homogenate have no visible precipitate to the naked eye; Filtration: Filter the homogenate. The filtration condition is 300 mesh, and filter 3 times to remove impurities and collect the filtrate; Sterilization: Heat - sterilize the filtrate in a boiling water bath at 100 °C for 30 min to obtain the final beverage; Cooling, filling, and storage: Cool the beverage to room temperature, fill it, and store it sealed in a 4 °C environment.

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