A compound sweetener with antioxidant function and preparation method thereof

Abstract

The present invention discloses a compound sweetener with antioxidant properties and a preparation method thereof, belonging to the field of sweeteners. The present invention utilizes a double-encapsulation method, using a novel polydextrose complex salt structure as the outermost shell material, kappa-carrageenan as the secondary outer shell material, and a sweetener composition as the inner core to prepare the compound sweetener. The compound sweetener prepared by the present invention has a sugary flavor close to that of sucrose, without undesirable flavors such as an off-color sweetness, bitter aftertaste, metallic taste, or chemical taste. It also exhibits certain antioxidant properties and maintains stable properties during storage.

Description

Technical Field

[0001] The invention relates to a compound sweetener with antioxidant function and a preparation method thereof, belonging to the field of sweeteners. Background Art

[0002] High sugar intake is associated with a variety of chronic diseases, such as type 2 diabetes, obesity, cardiovascular and kidney diseases, so reducing sugar intake is crucial. Currently, a number of high-intensity sweeteners and sugar substitutes have been developed, resulting in relative sweetness levels dozens to hundreds of times greater than sucrose per unit mass, with no or low energy content and anti-caries properties. However, these products also suffer from impure sweetness, a delayed sweetness, and unpleasant flavors such as bitter aftertaste, metallic taste, and chemical taste compared to sucrose.

[0003] To address the lack of flavor in sugar substitutes, the technology of compounding sugar substitute sweeteners is needed. Sweet taste receptors contain multiple binding sites that can bind to different substances and produce characteristic sweet signals. This means that the flavor properties of different sugar substitutes can be used for modification. However, simply compounding sugar substitutes still fails to significantly reduce the sweetness difference from sucrose. This is mainly because the difference in the speed of receptor binding still exists.

[0004] Currently, some researchers are using sweetener encapsulation to better control the release of sweetness. For example, double emulsion microencapsulation achieves sustained release and stabilizes the sweetener, but it still struggles to fully mimic the release profile of sucrose in terms of taste. Other researchers are using starch-based nanomaterials to encapsulate active substances to improve their solubility and stability. However, applying these methods to encapsulate sweeteners still presents certain challenges. Summary of the Invention

[0005] To address these issues, the present invention utilizes a double-encapsulation method to prepare a compound sweetener, using a novel polydextrose complex salt structure as the outermost shell material, kappa-carrageenan as the secondary outer shell material, and a sweetener composition as the inner core. The compound sweetener prepared by the present invention has a flavor similar to sucrose, without unpleasant flavors such as an off-color sweetness, bitter aftertaste, metallic taste, or chemical taste, and exhibits certain antioxidant properties.

[0006] The first object of the present invention is to provide a method for preparing a compound sweetener with antioxidant function, comprising the following steps:

[0007] (1) dissolving the sweetener composition and κ-carrageenan in water at 60-100° C., adjusting the pH to 2.5-5.5, and drying to obtain a solid material A;

[0008] (2) dispersing starch in a neutral salt solution to obtain a starch solution with a concentration of 2 to 5 wt%; then adding a medium-temperature α-amylase to the starch solution for enzymatic hydrolysis; after the reaction is completed, adjusting the pH to 3.5 to 4.5, adding sugar alcohol, reacting at 85 to 95° C. in a vacuum for 5 to 15 minutes, then polymerizing at 120 to 130° C. for 60 to 90 minutes, cooling, adjusting the pH to 6.0 to 9.0, and oxidizing and decolorizing to obtain liquid material B;

[0009] (3) Adding solid material A and liquid material B into a microchannel reactor, controlling the feed solid-liquid mass ratio to be 1 to 9:1, reacting at 55 to 65° C. for 2 to 10 minutes to obtain a composite treatment liquid; then homogenizing the composite treatment liquid at 70 to 100 MPa for 5 to 10 minutes, circulating 3 to 5 times, and drying to obtain a compound sweetener with antioxidant function.

[0010] In one embodiment of the present invention, the dissolution in step (1) is carried out using water at 60 to 100° C. in combination with low-speed stirring, wherein the low-speed stirring is 500 to 1000 rpm.

[0011] In one embodiment of the present invention, the pH is adjusted in step (1) using citric acid or sodium citrate.

[0012] In one embodiment of the present invention, the sweetener composition in step (1) is three or four of sucralose, steviol glycosides, erythritol, and mogrosides.

[0013] In one embodiment of the present invention, the mass ratio of the sweetener composition, κ-carrageenan, and water in step (1) is 25-35:1-3:100.

[0014] In one embodiment of the present invention, the neutral salt in step (2) is one or more of potassium chloride, calcium chloride, magnesium sulfate, and magnesium chloride.

[0015] In one embodiment of the present invention, the neutral salt solution in step (2) is a neutral salt water solution with a mass concentration of 0.06% to 0.12%.

[0016] In one embodiment of the present invention, the starch in step (2) is starch with an amylopectin content of more than 90%, specifically waxy corn starch, waxy potato starch, etc.

[0017] In one embodiment of the present invention, the dosage of the medium-temperature amylase in step (2) is 8 to 20 U / g (starch); and the enzymatic hydrolysis reaction is carried out at 40 to 60° C. for 90 to 180 min.

[0018] In one embodiment of the present invention, the pH is adjusted to 3.5-4.5 in step (2) by using citric acid or sodium citrate.

[0019] In one embodiment of the present invention, the sugar alcohol in step (2) is sorbitol, and the mass concentration of the sugar alcohol is 10-15%.

[0020] In one embodiment of the present invention, step (2) adjusting the pH to 6.0-9.0 is performed using sodium bicarbonate or sodium carbonate.

[0021] In one embodiment of the present invention, the oxidative decolorization in step (2) is performed using a hydrogen peroxide solution, specifically at 20-30° C. (room temperature) for 30-60 min; the amount of the hydrogen peroxide solution added is 1-2 wt %; and the hydrogen peroxide solution is a 30% concentration of hydrogen peroxide solution.

[0022] In one embodiment of the present invention, the liquid material prepared in step (2) is a novel polydextrose complex salt structure.

[0023] In one embodiment of the present invention, the drying in steps (1) and (3) is spray drying, specifically, the feed nozzle diameter is 1.0 mm, the feed is carried out by a peristaltic pump, the flow rate is 0.5 to 3 L / h, the inlet drying air temperature is 140 to 160° C., the air flow rate is 30 to 40 L / h, and the outlet drying air temperature is 80 to 90° C.

[0024] In one embodiment of the present invention, the homogenization in step (3) is performed using a high-pressure microfluidizer.

[0025] The second object of the present invention is a compound sweetener with antioxidant function prepared by the method of the present invention.

[0026] The third object of the present invention is the application of the compound sweetener with antioxidant function in the field of food.

[0027] In one embodiment of the present invention, the compound sweetener with antioxidant function can be used to prepare beverages, cakes, bread, soft candies, etc.

[0028] [Beneficial Effects]

[0029] (1) The advantages of the compound sweetener with antioxidant function prepared by the present invention after dissolving in water are as follows: under the high osmotic effect of neutral salt, the amphiphilic mucus hydrogel covering the tongue shrinks, and the novel polydextrose complex salt structure combines with water to form hydrogen bonds, which then diffuses specifically and rapidly to the human sweet taste receptor site, releasing the sweetener composition. The macromolecular sweetener and the small molecule sweetener bind to the receptor proteins hT1R2 and hT1R3, and the salt ions bind to the calcium-sensing receptor, thereby producing a sweet sensation similar to sucrose.

[0030] (2) The present invention avoids the slow diffusion of non-caloric sweeteners caused by the amphiphilic mucus hydrogel covering the surface of the tongue. At the same time, the new polydextrose complex salt dissolves and locates quickly; it avoids the disadvantage that non-sugar sweeteners diffuse first to non-receptor sites on the receptor protein and then diffuse to the sweet receptor site, resulting in a delay in taste response; it inhibits the transmission of bitter signals, and ultimately produces signal transmission similar to that of sucrose.

[0031] (3) The compound sweetener prepared by the present invention has a certain antioxidant capacity, good solubility, and the properties of the sweetener are stable during storage. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 The electronic tongue comparison results of the compound sweeteners prepared in the examples and comparative examples and white sugar are shown.

[0033] Figure 2 PCA analysis of the electronic tongue results of the compound sweeteners and white sugar prepared in Examples and Comparative Examples. DETAILED DESCRIPTION

[0034] The following describes preferred embodiments of the present invention. It should be understood that the embodiments are for better explanation of the present invention and are not intended to limit the present invention.

[0035] Test method:

[0036] 1. pH stability test of compound sweetener aqueous solution:

[0037] Weigh 10g of compound sweetener and dissolve it in 100mL of water. Stir until fully dissolved as a standby solution.

[0038] Determine its stability in solutions with different pH values: use a graduated cylinder to measure the reserve solution in a beaker, add a certain amount of acetic acid and adjust the pH values to 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, and 7, respectively; pour the solution into a Pet bottle and store it at room temperature for 6 months.

[0039] The contents of various sugar substitutes in the solution were determined by HPLC.

[0040] 2. Temperature stability test of compound sweetener aqueous solution:

[0041] Weigh 10g of compound sweetener and dissolve it in 100mL of water. Stir until fully dissolved as a standby solution.

[0042] Use a graduated cylinder to measure 500 mL of the reserve solution into a beaker, and adjust the temperature in a water bath to different levels (60°C, 70°C, 80°C, 90°C, 100°C, 110°C, 120°C, 130°C, 140°C, 150°C) for 60 min each.

[0043] The contents of various sugar substitutes in the solution were determined by HPLC.

[0044] 3. Sensory evaluation of compound sweeteners:

[0045] The sensory evaluation of compound sweeteners and white sugar in terms of sweetness, astringency, aftertaste, metallic taste, chemical taste, and honey taste was compared as follows:

[0046] Aqueous solutions of 30% white sugar and 10% compound sweeteners were prepared respectively, and then 20 healthy and sensitive tasters were selected to evaluate the samples. They were required to thoroughly clean their mouths with 2 soda crackers and drinking purified water before tasting the samples. They were also required to rinse their mouths in time between every two cups of solution to reduce the interference caused by the residual taste of the previous sample. The rest time was 30s; the solution presentation volume was 15mL, and it was placed in a 30mL odorless test cup with a three-digit random code at room temperature. All samples were required to complete the scoring of all attributes and the experiment was repeated three times.

[0047] The sensory evaluation criteria and evaluation results are shown in Table 1 below.

[0048] Table 1 Sensory evaluation standards and reference samples

[0049]

[0050] 4. Changes in sweetness, color and morphology of aqueous solutions of compound sweeteners during storage:

[0051] The compound sweetener is stored in a cool environment at room temperature for a certain period of time, and is prepared into a 10% by mass aqueous solution. The sweetness is measured by sensory measurement, the color is measured by a colorimeter, and the tissue morphology is measured by turbidimetry.

[0052] 5. Electronic tongue evaluation of compound sweeteners:

[0053] The Smartongue / iTongue system was used. After the electrodes were preheated, data were collected from the samples at room temperature. Data collection was repeated three times for each sample.

[0054] 6. Determination of antioxidant function:

[0055] Weigh 1, 3, 5, 7, 9, 11, and 13 mg (dry basis) of sample powder respectively into 10 mL test tubes and add 2×10 -4 Prepare 4 mL of 1.5 mol / L DPPH ethanol solution, vortex and shake for 2 min, let it stand for 30 min at room temperature in the dark, and then centrifuge for 10 min (7000 rpm). Take the supernatant and use ethanol as a blank control. Measure the absorbance at 517 nm.

[0056] The DPPH free radical scavenging rate was calculated according to formula (1) as follows:

[0057]

[0058] Where A0 is the absorbance of the blank sample; A1 is the absorbance of the sample; and A2 is the absorbance measured when the ethanol solution replaces the DPPH solution.

[0059] The raw materials used in the embodiment are:

[0060] Waxy corn starch: 98% purity, 93% amylopectin content, Shanghai Yuanye Biotechnology Co., Ltd.

[0061] Sucralose: purity 98-100%; purchased from Anhui Jinhe Industrial Co., Ltd.

[0062] Stevioside: RA95% (SRE09); purchased from Rhine Biotechnology Co., Ltd.;

[0063] Mogroside: V50; purchased from Rhine Biotechnology Co., Ltd.;

[0064] Erythritol: 99.5-100.5%; purchased from Yuxing Biological (Group) Co., Ltd.

[0065] Mesophilic α-amylase: enzyme activity of 10,000 U / g, purchased from Beijing Solebow Technology Co., Ltd.

[0066] The raw materials of the examples and comparative examples can be purchased from commercial sources. Where the solvent is not specified, water is used as the solvent. Where the percentage is not specified, it is expressed in mass percentage.

[0067] Example 1

[0068] A method for preparing a compound sweetener with antioxidant function comprises the following steps:

[0069] (1) 30 g of a sweetener composition (sucralose, steviol glycosides, and erythritol in a mass ratio of 0.1:0.1:30) and 2 g of κ-carrageenan were dissolved in 100 g of 100°C water and stirred at 1000 rpm for 20 min; the pH was then adjusted to 5 with citric acid and spray dried (feed nozzle diameter 1.0 mm, air inlet temperature 150°C, outlet temperature 85°C, wind speed 40 L / min, feed rate 3 L / h) to obtain solid material A;

[0070] (2) Waxy corn starch was dispersed in a potassium chloride aqueous solution with a concentration of 0.12% wt% to obtain a starch solution with a concentration of 4 wt%; then, a medium-temperature α-amylase (added in an amount of 20 U / g (starch)) was added to the starch solution, and an enzymatic hydrolysis reaction was carried out at 50°C for 120 min; after the reaction, citric acid was added to adjust the pH to 4, and then sorbitol (mass concentration of 10%) was added, and the reaction was carried out at 90°C for 10 min under vacuum conditions, and a polymerization reaction was carried out at 125°C for 80 min, and then cooled to room temperature; sodium bicarbonate was used to adjust the pH to 8.0; finally, a hydrogen peroxide solution (concentration of 30%, addition amount of 2 wt%) was used for oxidative decolorization at 25°C for 45 min to obtain liquid material B;

[0071] (3) Solid material A and liquid material B were added to a microchannel reactor, and the mass ratio of the solid and liquid of the feed was controlled to be 5:1 (solid-liquid ratio), and the reaction was carried out at 65°C for 10 minutes to obtain a composite treatment liquid; the composite treatment liquid was then homogenized in a high-pressure microjet nanohomogenizer at 80 MPa for 6 minutes, and the cycle was repeated 3 times. Finally, it was spray-dried (the feed nozzle diameter was 1.0 mm, the inlet air temperature was 150°C, the outlet temperature was 85°C, the wind speed was 40 L / min, and the feed rate was 3 L / h) to obtain a compound sweetener with antioxidant function.

[0072] Example 2 (compounding of sweeteners)

[0073] The formula of the sweetener composition in step (1) of Example 1 was adjusted to a mass ratio of sucralose, steviol glycosides, mogroside, and erythritol of 0.1:0.1:0.02:30, and the other ingredients remained the same as in Example 1 to obtain a compound sweetener.

[0074] Example 3 (Ratio of the two embedded materials)

[0075] The mass ratio of solid material A to liquid material B in step (3) of Example 2 was adjusted to 6:1, and the other ingredients remained the same as in Example 2 to obtain a compound sweetener.

[0076] Example 4 (neutral salt ratio)

[0077] The potassium chloride in step (2) of Example 2 was adjusted to a mixed salt (the mass ratio of potassium chloride: magnesium chloride: calcium chloride was 1:1:1), and the other ingredients remained the same as in Example 2 to obtain a compound sweetener.

[0078] Example 5 (Concentration of Starch in the Novel Polydextrose Composite Salt)

[0079] The concentration of the starch solution in step (2) of Example 2 was adjusted to 3 wt %, and the other contents remained the same as in Example 2 to obtain a compound sweetener.

[0080] Example 6 (Temperature of embedding reaction)

[0081] Adjustment: The reaction temperature in the microchannel reactor in step (3) of Example 2 was adjusted to 50° C., and the rest remained consistent with Example 2 to obtain a compound sweetener.

[0082] Comparative Example 1

[0083] The sucralose in step (1) of Example 1 was omitted, and the mass ratio of stevioside to erythritol was adjusted to 0.2:30. Other ingredients remained the same as in Example 1 to obtain a compound sweetener.

[0084] Comparative Example 2

[0085] The steviol glycoside in step (1) of Example 1 was omitted, and the mass ratio of sucralose to erythritol was adjusted to 0.2:30. Other ingredients remained the same as in Example 1 to obtain a compound sweetener.

[0086] Comparative Example 3

[0087] Omit the steviol glycosides and sucralose in step (1) of Example 1, and use only erythritol. Other ingredients remain the same as in Example 1 to obtain a compound sweetener.

[0088] Comparative Example 4

[0089] The steviol glycoside in step (1) of Example 1 was adjusted to xylitol, and the other ingredients remained the same as in Example 1 to obtain a compound sweetener.

[0090] Comparative Example 5

[0091] The sucralose in step (1) of Example 1 was replaced with sorbitol, and the other ingredients remained the same as those in Example 1 to obtain a compound sweetener.

[0092] Comparative Example 6

[0093] The liquid material B in step (2) of Example 1 was adjusted to polydextrose, and the other ingredients remained the same as in Example 1 to obtain a compound sweetener.

[0094] Comparative Example 7

[0095] The liquid material B in step (2) of Example 1 was adjusted to β-cyclodextrin, and the other ingredients remained the same as in Example 1 to obtain a compound sweetener.

[0096] Comparative Example 8

[0097] The liquid material B in step (2) of Example 1 was adjusted to OSA starch, and the other ingredients remained the same as in Example 1 to obtain a compound sweetener.

[0098] Comparative Example 9

[0099] The kappa-carrageenan in step (1) of Example 1 was omitted, and the other ingredients were kept consistent with Example 1 to obtain a compound sweetener.

[0100] Comparative Example 10

[0101] The potassium chloride in step (2) of Example 1 was omitted, and the other ingredients were kept the same as in Example 1 to obtain a compound sweetener.

[0102] Comparative Example 11

[0103] The vacuuming step in step (2) of Example 1 was omitted, and the rest of the process remained the same as in Example 1 to obtain a compound sweetener.

[0104] Comparative Example 12

[0105] The step of adding sorbitol in step (2) of Example 1 was omitted, and the rest of the steps remained the same as in Example 1 to obtain a compound sweetener.

[0106] Comparative Example 13

[0107] The step of adding sorbitol in step (2) of Example 1 was omitted, and an equal amount of sorbitol was added in step (1); the rest of the steps were the same as in Example 1 to obtain a compound sweetener.

[0108] Comparative Example 14

[0109] The step of adding sorbitol in step (2) of Example 1 was omitted, and an equal amount of sorbitol was added in step (3); the rest of the steps were the same as in Example 1 to obtain a compound sweetener.

[0110] Comparative Example 15

[0111] The step of adding potassium chloride in step (2) of Example 1 was omitted, and an equal amount of potassium chloride was added in step (3); the rest was consistent with Example 1 to obtain a compound sweetener.

[0112] Comparative Example 16

[0113] The step of adding potassium chloride in step (2) of Example 1 was omitted, and an equal amount of potassium chloride was added in step (1); the rest was the same as in Example 1 to obtain a compound sweetener.

[0114] Comparative Example 17

[0115] The step of adjusting the pH in step (1) of Example 1 was omitted, and the rest was kept consistent with Example 1 to obtain a compound sweetener.

[0116] Comparative Example 18

[0117] Solid material A is directly used as the compound sweetener.

[0118] Comparative Example 19

[0119] The drying step (1) in Example 1 was omitted, and the rest of the steps were kept the same as in Example 1 to obtain a compound sweetener.

[0120] Comparative Example 20

[0121] The drying step in step (1) was omitted, and the obtained liquid A was directly homogenized with the liquid liquid B obtained in step (2) by a high-pressure microfluidizer at 80 MPa for 6 min, the cycle was repeated 3 times, and finally spray-dried. Other conditions were the same as in Example 1 to obtain a compound sweetener.

[0122] The obtained compound sweetener was subjected to performance testing, and the test results are as follows:

[0123] Table 2 shows the effect of pH on the stability of the compound sweetener of Example 2. As shown in Table 2, the compound sweetener of Example 2 is relatively stable under different pH conditions, with only a small loss at pH 3 and 3.5. This indicates that the compound sweetener has excellent acid resistance.

[0124] Table 2 Effect of pH value on the stability of the compound sweetener of Example 2

[0125]

[0126] Table 3 shows the effect of temperature on the stability of the compound sweetener of Example 2. As shown in Table 3, the compound sweetener of Example 2 has very good heat resistance and retains 100% of its sweetness even after being heated at 100° C. for 60 minutes.

[0127] Table 3 Effect of temperature on the stability of the compound sweeteners in Example 2

[0128]

[0129] Table 4 shows the changes in the quality of the aqueous solution of the compound sweetener of Example 2 during storage at different times. Table 4 shows that the sweetness, morphology, and antioxidant activity of the aqueous solution of the compound sweetener of Example 2 were well maintained during long-term storage. Furthermore, the sweetness of the resulting compound sweetener was three times that of 10% sucrose.

[0130] Table 4 Changes in the quality of sweetener aqueous solutions during storage at different times

[0131]

[0132] Note: The sweetness, color, and antioxidant activity of the solution marked "0 months" are all 100%. The indicators for different storage times are percentages based on the 0-month value. The sweetness of a 10% mass concentration solution at 0 months is three times that of 10% sucrose, and its antioxidant activity is 67%.

[0133] Table 5 Sensory evaluation results of compound sweeteners and white sugar

[0134]

[0135]

[0136] The electronic tongue comparison results and PCA analysis results of the compound sweeteners prepared in the examples and comparative examples and white sugar are as follows: Figure 1 and Figure 2 ,Depend on Figure 1 and Figure 2 It can be seen that Examples 1 to 6 are consistent with white sugar in overall flavor, while Comparative Examples 1 to 20 have certain differences from sucrose in sweetness, cooling sensation, sweetness persistence, bitterness and astringency, making them unable to completely simulate the taste of sucrose.

[0137] Although the present invention has been disclosed above in terms of preferred embodiments, it is not intended to limit the present invention. Anyone familiar with this technology can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be based on the definition of the claims.

Claims

1. A method for preparing a compound sweetener with antioxidant function, characterized in that: The steps include: (1) Dissolving a sweetener composition and kappa-carrageenan in water at 60-100° C., adjusting the pH to 2.5-5.5, and drying to obtain a solid material A; wherein the sweetener composition is three or four of sucralose, steviol glycosides, erythritol, and mogrosides; (2) Dispersing starch in a neutral salt solution to obtain a starch solution with a concentration of 2-5 wt%; then adding a medium-temperature α-amylase to the starch solution for enzymatic hydrolysis; after the reaction, adjusting the pH to 3.5-4.5, adding sugar alcohol, reacting at 85-95°C in vacuum for 5-15 min, and then polymerizing at 120-130°C for 60-90 min, cooling, adjusting the pH to 6.0-9.0, and oxidative decolorization to obtain liquid material B; (3) Solid material A and liquid material B were added to a microchannel reactor, and the feed solid-liquid mass ratio was controlled to be 1-9:

1. The reaction was carried out at 55-65 °C for 2-10 min to obtain a composite treatment liquid. The composite treatment liquid was then homogenized at 70-100 MPa for 5-10 min for 3-5 times and dried to obtain a compound sweetener with antioxidant function.

2. The method according to claim 1, characterized in that In step (1), the mass ratio of the sweetener composition, κ-carrageenan, and water is 25-35:1-3:

100.

3. The method according to claim 1, characterized in that The neutral salt in step (2) is one or more of potassium chloride, calcium chloride, magnesium sulfate, and magnesium chloride.

4. The method according to claim 1, wherein The dosage of the medium-temperature α-amylase in step (2) is 8 to 20 U / g starch; the enzymatic hydrolysis reaction is carried out at 40 to 60°C for 90 to 180 min.

5. The method according to claim 1, wherein In step (2), the sugar alcohol is sorbitol, and the mass concentration of the sugar alcohol is 10-15%.

6. The method according to claim 1, wherein In step (2), the oxidative decolorization is carried out by using a hydrogen peroxide solution.

7. The method according to claim 1, characterized in that In step (3), the homogenization is carried out using a high-pressure microfluidizer.

8. The compound sweetener with antioxidant function prepared by the method according to any one of claims 1 to 7.

9. Use of the compound sweetener with antioxidant function according to claim 8 in the food field.

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