Method for preparing functional sugar through ultrasonic-assisted co-crystallization

Abstract

The invention discloses a method for preparing functional sugar through ultrasonic-assisted co-crystallization, which comprises the following steps: heating a molasses raw material in a sugar boiling tank, continuously stirring to obtain a cane sugar supersaturated solution, maintaining the temperature of syrup to be lower than 120 DEG C, and monitoring the brix of the syrup in real time; when the brix of the syrup reaches 68-72 degrees Bx, transferring the syrup into a glass dish, cooling to 70 DEG C, and adding the camellia nitidissima leaf polyphenol extract, arabinose and camellia nitidissima micro powder into the syrup in a powder form; transferring the syrup into an ultrasonic water bath kettle, carrying out ultrasonic treatment at 25-35 DEG C, and continuously and mechanically stirring until solid substances appear; and transferring the obtained solid substance into a metal disc, and drying in a vacuum drying oven at 63-67 DEG C for 22-24 hours.

Description

Technical field:

[0001] The invention relates to a method for preparing functional sugar by ultrasound-assisted co-crystallization. Background technology:

[0002] Camellia chrysantha belongs to the genus Camellia of the Theaceae family and is one of the most precious plant species in the world. Camellia chrysantha is rich in nutrients, including soluble sugars, proteins, amino acids, trace elements, tea saponins, flavonoids and other ingredients, and has the effects of clearing away heat and detoxification, diuresis and dampness, anti-oxidation, and anti-aging. From the perspective of active ingredients, there are certain active natural product categories in Camellia chrysantha, such as dihydroxys, trihydroxys, flavonoids, alkaloids, etc. The anti-liver cancer effect of Camellia chrysantha may be the macroscopic manifestation of these potential active ingredients. However, the parts of these natural products with antioxidant activity are prone to lose activity during processing, so the stable storage method of active substances is the development focus of the present invention.

[0003] Sucrose co-crystallization is a promising method for encapsulating bioactive ingredients in food. By encapsulating the easily damaged and deteriorated active ingredients in the sucrose crystal structure through the co-crystallization technology, the storage stability of active substances such as polyphenols can be improved. CN102499353B discloses a method for efficient separation, extraction and stable storage of bayberry polyphenols. By co-crystallizing bayberry polyphenols with sucrose, a stable polyphenol microcapsule product can be obtained, which significantly improves the stability of polyphenols during storage. In addition, through the co-crystallization technology, low glycemic index monosaccharides such as arabinose can be introduced into the sucrose crystal structure at the same time to reduce the glycemic index of the obtained functional sugar product, and obtain the desired low glycemic index healthy functional sugar product. However, there is no report on the ultrasonic-assisted co-crystallization of arabinose, golden camellia micropowder, golden camellia tea polyphenol extract and honey. Summary of the invention:

[0004] The purpose of the present invention is to provide a method for preparing functional sugar by ultrasound-assisted co-crystallization.

[0005] The present invention is achieved through the following technical solutions:

[0006] A method for preparing functional sugar by ultrasound-assisted co-crystallization, the method comprising the following steps: heating molasses raw materials in a sugar boiling pot and continuously stirring to obtain a supersaturated sucrose solution, maintaining the syrup temperature below 120°C, and monitoring the syrup brax in real time; when the syrup brax reaches about 70°Bx, transferring the syrup to a glass dish, cooling to 70°C, adding chrysanthemi camellia polyphenol extract, arabinose and chrysanthemi camellia micropowder in powder form to the syrup; transferring the syrup to an ultrasonic water bath pot and ultrasonicating at 25-35°C, continuing to use mechanical stirring continuously until solid matter appears; transferring the obtained solid matter to a metal plate, and drying it at 63-67°C in a vacuum drying oven for 22-24 hours.

[0007] Preferably, the mass ratio of golden camellia tea polyphenol extract, arabinose and golden camellia powder is 0.4-0.7:5-8:0.4-0.7.

[0008] More preferably, the mass ratio of the golden camellia tea polyphenol extract, arabinose and golden camellia powder is 0.5-0.7:6-8:0.5-0.7.

[0009] Preferably, the mass ratio of golden camellia tea polyphenol extract to sucrose is 0.4-0.7:100.

[0010] Preferably, the particle size of the Camellia chrysantha powder is less than 30 microns.

[0011] The beneficial effects of the present invention are as follows: the sugar raw material used in the present invention is molasses, which saves the step of dissolving sucrose in water and saves costs; the particle size of the golden camellia powder used reaches the micron level, which plays a good nucleation role in the co-crystallization process; the crystallization time is effectively shortened by ultrasound-assisted crystallization; the golden camellia polyphenol extract is encapsulated by using syrup prepared from molasses through the co-crystallization technology, which retains the biological activity of the golden camellia polyphenol extract and improves the storage stability of the golden camellia polyphenol extract; the arabinose co-crystallization technology enables the prepared functional sugar to have a low glycemic function. Arabinose, golden camellia powder, golden camellia polyphenol extract and honey enable the prepared functional sugar product to have multiple health benefits at the same time. Specific implementation method:

[0012] The following is a further description of the present invention, rather than a limitation of the present invention.

[0013] The test method for the syrup brix in the following examples is the refractometry;

[0014] The calculation method of the recovery rate of crystallized sugar in the following examples is as follows: weight of crystallized sugar / (weight of original molasses*(molasses Brix*1.025-7.703)+amount of arabinose added+amount of camellia chrysantha powder added+amount of camellia chrysantha extract added).

[0015] The polyphenol content detection method in the following examples is the Folin-Ciocalteu colorimetric method to determine the total polyphenol content. In brief, 2.5 mg of gallic acid reference substance is weighed and placed in a 25 mL volumetric flask, and the volume is adjusted to the mark with distilled water to obtain the reference substance stock solution. 0, 0.25, 0.5, 0.75, 1.0, and 1.25 mL of the stock solution are respectively taken and placed in a 25 mL volumetric flask, 1.5 mL of Folin-Ciocalteu reagent is added, and 1.5 mL of 10% Na 2 CO 3 The solution was diluted to volume with distilled water, reacted at 25°C for 1 h, and the absorbance at 765 nm was measured.

[0016] The detection and calculation method of the encapsulation rate of the polyphenol extract of golden camellia flower in the following embodiment is: the encapsulation efficiency (%) is calculated by taking the concentration of the polyphenol extract of golden camellia flower in the final co-crystallization product (Y) and the initial concentration of the polyphenol extract of golden camellia flower in the loaded extract (X) as Y / X*100.

[0017] The test and calculation method of the storage stability of functional sugar in the following examples is as follows: by measuring the polyphenol content of the control sample and the experimental sample of the example under vacuum and lightless conditions at room temperature (30°C), the chemical stability of the polyphenol extract of golden camellia tea during storage is determined. The control sample is a mixture of polyphenol extract of golden camellia tea and crystallized sucrose (dispersed state). The control sample and the experimental sample of the example are both placed for 90 days and analyzed to obtain the residual polyphenol content. The storage stability of functional sugar is indicated by residual polyphenol content / polyphenol content in the original sample*100%.

[0018] Example 1

[0019] Heat 50g of molasses in a sugar boiling pot and stir continuously to obtain a supersaturated sucrose solution, maintain the syrup temperature below 120°C, and monitor the syrup brax in real time; when the syrup brax reaches about 70°Bx, transfer the syrup to a glass dish, and when it is cooled to 70°C, add 0.35g of golden camellia tea polyphenol extract (0.7g per 100g of sucrose), 4g of arabinose (8g per 100g of sucrose) and 0.35g of golden camellia powder with a particle size of 20-30 microns (0.7g per 100g of sucrose) into the glass dish. 0.7 g of sucrose (100 g) was added to the syrup in powder form; the syrup was transferred to an ultrasonic water bath, the ultrasonic temperature was 25°C, the ultrasonic power was 40 kHz, the ultrasonic time was 30 min, and mechanical stirring was continued at a rate of 400 rpm until solid matter appeared; the obtained solid matter was transferred to a metal dish and dried in a vacuum drying oven at 65°C for 24 h; then the size distribution was determined by passing through a 2 mm sieve, and the agglomerates were ground with a blade grinder.

[0020] The recovery rate of crystallized sugar was 68.3%, the encapsulation efficiency was 66.7%, and the storage stability of functional sugar was 79.4%.

[0021] Comparative Example 1

[0022] Weigh 0.7 g of golden camellia tea polyphenol extract, 8 g of arabinose, 0.7 g of golden camellia powder and 100 g of sucrose (commercially available white sugar) and mix them. The polyphenol content in the mixture was measured before storage and after 90 days, and the storage stability was calculated to be 35.7%.

[0023] From the comparison between Example 1 and Comparative Example 1, it can be seen that the syrup prepared by the molasses of the present invention is used to encapsulate the polyphenol extract of Camellia chrysantha, which retains the biological activity of the polyphenol extract of Camellia chrysantha and improves the storage stability of the polyphenol extract of Camellia chrysantha.

[0024] Comparative Example 2:

[0025] Reference Example 1, except that no Camellia chrysantha powder was added.

[0026] Heat 50g of molasses raw material in a sugar boiling pot and stir continuously to obtain a supersaturated sucrose solution, maintain the syrup temperature below 120°C, and monitor the syrup brax in real time; when the syrup brax reaches about 70°Bx, transfer the syrup to a glass dish, and when it is cooled to 70°C, add 0.35g of golden camellia tea polyphenol extract (0.7g per 100g of sucrose) and 4g of arabinose (8g per 100g of sucrose) to the syrup; transfer the syrup to an ultrasonic water bath, the ultrasonic temperature is 25°C, the ultrasonic power is 40kHz, the ultrasonic time is 30min, and mechanical stirring is continued at a stirring rate of 400rpm until solid matter appears; transfer the obtained solid matter to a metal plate and dry it in a vacuum drying oven at 65°C for 24h; then determine its size distribution through a 2mm sieve, and grind the agglomerates with a blade grinder.

[0027] The recovery rate of crystallized sugar was 45.2%, the encapsulation efficiency was 50.3%, and the storage stability of functional sugar was 32.4%.

[0028] Comparison between Example 1 and Comparative Example 2 shows that the particle size of the Camellia chrysantha powder used reaches the micron level, which plays a good nucleation role in the co-crystallization process, resulting in a higher recovery rate of crystallized sugar, better encapsulation efficiency and storage stability of functional sugar.

[0029] Comparative Example 3:

[0030] Refer to Example 1, except that no golden camellia tea polyphenol extract and arabinose were added.

[0031] 50g of molasses raw material is heated in a sugar boiling pot and stirred continuously to obtain a supersaturated sucrose solution, the syrup temperature is maintained below 120°C, and the syrup brax is monitored in real time; when the syrup brax reaches about 70°Bx, the syrup is transferred to a glass dish, and when it is cooled to 70°C, 0.35g of golden camellia micropowder with a particle size of 20-30 microns (0.7g is added for every 100g of sucrose) is added to the syrup in powder form; the syrup is transferred to an ultrasonic water bath pot, the ultrasonic temperature is 25°C, the ultrasonic power is 40kHz, the ultrasonic time is 30min, and mechanical stirring is continued continuously at a stirring rate of 400rpm until solid matter appears; the obtained solid matter is transferred to a metal plate and dried in a vacuum drying oven at 65°C for 24h; then its size distribution is determined by passing through a 2mm sieve, and the agglomerates are ground with a blade grinder.

[0032] The recovery rate of crystallized sugar was 53.6%, the encapsulation efficiency was 42.7%, and the storage stability of functional sugar was 48.9%.

[0033] From the comparison between Example 1 and Comparative Example 3, it can be seen that the addition of golden camellia tea polyphenol extract and arabinose can increase the recovery rate of crystalline sugar, and improve the encapsulation efficiency and storage stability of functional sugar.

[0034] Example 2

[0035] Heat 50g of molasses in a sugar boiling pot and stir continuously to obtain a supersaturated sucrose solution, maintain the syrup temperature below 120°C, and monitor the syrup brax in real time; when the syrup brax reaches about 70°Bx, transfer the syrup to a glass dish, and when it is cooled to 70°C, add 0.3g of golden camellia tea polyphenol extract (0.6g per 100g of sucrose), 3.5g of arabinose (7g per 100g of sucrose) and 0.3g of golden camellia powder with a particle size of 20-30 microns (0.6g per 100g of sucrose) to the glass dish. 00g sucrose (0.6g) was added to the syrup in powder form; the syrup was transferred to an ultrasonic water bath, the ultrasonic temperature was 30°C, the ultrasonic power was 30kHz, the ultrasonic time was 40min, and mechanical stirring was continued at a stirring rate of 500rpm until solid matter appeared; the obtained solid matter was transferred to a metal dish and dried in a vacuum drying oven at 65°C for 24h; then the size distribution was determined by passing through a 2mm sieve, and the agglomerates were ground with a blade grinder.

[0036] The recovery rate of crystallized sugar was 62.7%, the encapsulation efficiency was 67.8%, and the storage stability of functional sugar was 69.5%.

[0037] Example 3

[0038] Heat 50g of molasses in a sugar boiling pot and stir continuously to obtain a supersaturated sucrose solution, maintain the syrup temperature below 120°C, and monitor the syrup brax in real time; when the syrup brax reaches about 70°Bx, transfer the syrup to a glass dish, and when it is cooled to 70°C, add 0.25g of golden camellia polyphenol extract (0.5g per 100g of sucrose), 3g of arabinose (6g per 100g of sucrose) and 0.25g of golden camellia micropowder with a particle size of 20-30 microns (0.5g per 100g of sucrose) to the glass dish. 00g sucrose (0.5g) was added to the syrup in powder form; the syrup was transferred to an ultrasonic water bath, the ultrasonic temperature was 35°C, the ultrasonic power was 20kHz, the ultrasonic time was 50min, and mechanical stirring was continued at a stirring rate of 600rpm until solid matter appeared; the obtained solid matter was transferred to a metal dish and dried in a vacuum drying oven at 65°C for 24h; then the size distribution was determined by passing through a 2mm sieve, and the agglomerates were ground with a blade grinder.

[0039] The recovery rate of crystallized sugar was 61.4%, the encapsulation efficiency was 66.7%, and the storage stability of functional sugar was 79.4%.

[0040] Example 4

[0041] Heat 50g of molasses in a sugar boiling pot and stir continuously to obtain a supersaturated sucrose solution, maintain the syrup temperature below 120°C, and monitor the syrup brax in real time; when the syrup brax reaches about 70°Bx, transfer the syrup to a glass dish, and when it is cooled to 70°C, add 0.2g of golden camellia tea polyphenol extract (0.4g per 100g of sucrose), 2.5g of arabinose (5g per 100g of sucrose) and 0.2g of golden camellia powder with a particle size of 20-30 microns (0.4g per 100g of sucrose) into the glass dish. 00g sucrose (0.4g) was added to the syrup in powder form; the syrup was transferred to an ultrasonic water bath, the ultrasonic temperature was 25°C, the ultrasonic power was 40kHz, the ultrasonic time was 30min, and mechanical stirring was continued at a stirring rate of 400rpm until solid matter appeared; the obtained solid matter was transferred to a metal dish and dried in a vacuum drying oven at 65°C for 24h; then the size distribution was determined by passing through a 2mm sieve, and the agglomerates were ground with a blade grinder.

[0042] The recovery rate of crystallized sugar was 63.2%, the encapsulation efficiency was 69.7%, and the storage stability of functional sugar was 49.0%.

[0043] Example 5

[0044] Heat 50g of molasses in a sugar boiling pot and stir continuously to obtain a supersaturated sucrose solution, maintain the syrup temperature below 120°C, and monitor the syrup brax in real time; when the syrup brax reaches about 70°Bx, transfer the syrup to a glass dish, and when it is cooled to 70°C, add 0.35g of golden camellia tea polyphenol extract (0.7g per 100g of sucrose), 4g of arabinose (8g per 100g of sucrose) and 0.35g of golden camellia powder with a particle size of 20-30 microns (0.7g per 100g of sucrose) to the glass dish. 00g sucrose (0.7g) was added to the syrup in powder form; the syrup was transferred to an ultrasonic water bath, the ultrasonic temperature was 30°C, the ultrasonic power was 30kHz, the ultrasonic time was 40min, and mechanical stirring was continued at a stirring rate of 500rpm until solid matter appeared; the obtained solid matter was transferred to a metal dish and dried in a vacuum drying oven at 65°C for 24h; then the size distribution was determined by passing through a 2mm sieve, and the agglomerates were ground with a blade grinder.

[0045] The recovery rate of crystallized sugar was 59.2%, the encapsulation efficiency was 68.3%, and the storage stability of functional sugar was 48.5%.

[0046] Example 6

[0047] Heat 50g of molasses in a sugar boiling pot and stir continuously to obtain a supersaturated sucrose solution, maintain the syrup temperature below 120°C, and monitor the syrup brax in real time; when the syrup brax reaches about 70°Bx, transfer the syrup to a glass dish, and when it is cooled to 70°C, add 0.3g of golden camellia tea polyphenol extract (0.6g per 100g of sucrose), 3.5g of arabinose (7g per 100g of sucrose) and 0.3g of golden camellia powder with a particle size of 20-30 microns (0.6g per 100g of sucrose) to the glass dish. 00g sucrose (0.6g) was added to the syrup in powder form; the syrup was transferred to an ultrasonic water bath, the ultrasonic temperature was 35°C, the ultrasonic power was 20kHz, the ultrasonic time was 50min, and mechanical stirring was continued at a stirring rate of 600rpm until solid matter appeared; the obtained solid matter was transferred to a metal dish and dried in a vacuum drying oven at 65°C for 24h; then the size distribution was determined by passing through a 2mm sieve, and the agglomerates were ground with a blade grinder.

[0048] The recovery rate of crystallized sugar was 66.5%, the encapsulation efficiency was 57.9%, and the storage stability of functional sugar was 37.8%.

[0049] Example 7

[0050] Heat 50g of molasses in a sugar boiling pot and stir continuously to obtain a supersaturated sucrose solution, maintain the syrup temperature below 120°C, and monitor the syrup brax in real time; when the syrup brax reaches about 70°Bx, transfer the syrup to a glass dish, and when it is cooled to 70°C, add 0.25g of golden camellia polyphenol extract (0.5g per 100g of sucrose), 3g of arabinose (6g per 100g of sucrose) and 0.25g of golden camellia micropowder with a particle size of 20-30 microns (0.5g per 100g of sucrose) to the glass dish. 00g sucrose (0.5g) was added to the syrup in powder form; the syrup was transferred to an ultrasonic water bath, the ultrasonic temperature was 25°C, the ultrasonic power was 40kHz, the ultrasonic time was 30min, and mechanical stirring was continued at a stirring rate of 400rpm until solid matter appeared; the obtained solid matter was transferred to a metal dish and dried in a vacuum drying oven at 65°C for 24h; then the size distribution was determined by passing through a 2mm sieve, and the agglomerates were ground with a blade grinder.

[0051] The recovery rate of crystallized sugar was 58.5%, the encapsulation efficiency was 53.4%, and the storage stability of functional sugar was 39.6%.

[0052] Example 8

[0053] Heat 50g of molasses in a sugar boiling pot and stir continuously to obtain a supersaturated sucrose solution, maintain the syrup temperature below 120°C, and monitor the syrup brax in real time; when the syrup brax reaches about 70°Bx, transfer the syrup to a glass dish, and when it is cooled to 70°C, add 0.2g of golden camellia tea polyphenol extract (0.4g per 100g of sucrose), 2.5g of arabinose (5g per 100g of sucrose) and 0.2g of golden camellia powder with a particle size of 20-30 microns (0.4g per 100g of sucrose) into the glass dish. 00g sucrose (0.4g) was added to the syrup in powder form; the syrup was transferred to an ultrasonic water bath, the ultrasonic temperature was 30°C, the ultrasonic power was 30kHz, the ultrasonic time was 40min, and mechanical stirring was continued at a stirring rate of 500rpm until solid matter appeared; the obtained solid matter was transferred to a metal dish and dried in a vacuum drying oven at 65°C for 24h; then the size distribution was determined by passing through a 2mm sieve, and the agglomerates were ground with a blade grinder.

[0054] The recovery rate of crystallized sugar was 66.3%, the encapsulation efficiency was 63.5%, and the storage stability of functional sugar was 40.6%.

[0055] Example 9

[0056] Heat 50g of molasses in a sugar boiling pot and stir continuously to obtain a supersaturated sucrose solution, maintain the syrup temperature below 120°C, and monitor the syrup brax in real time; when the syrup brax reaches about 70°Bx, transfer the syrup to a glass dish, and when it is cooled to 70°C, add 0.35g of golden camellia tea polyphenol extract (0.7g per 100g of sucrose), 4g of arabinose (8g per 100g of sucrose) and 0.35g of golden camellia powder with a particle size of 20-30 microns (0.7g per 100g of sucrose) to the glass dish. 00g sucrose (0.7g) was added to the syrup in powder form; the syrup was transferred to an ultrasonic water bath, the ultrasonic temperature was 35°C, the ultrasonic power was 20kHz, the ultrasonic time was 50min, and mechanical stirring was continued at a stirring rate of 600rpm until solid matter appeared; the obtained solid matter was transferred to a metal dish and dried in a vacuum drying oven at 65°C for 24h; then the size distribution was determined by passing through a 2mm sieve, and the agglomerates were ground with a blade grinder.

[0057] The recovery rate of crystallized sugar was 51.7%, the encapsulation efficiency was 54.5%, and the storage stability of functional sugar was 67.2%.

Claims

1. A method for preparing functional sugars by ultrasound-assisted co-crystallization, characterized in that: The method comprises the following steps: heating molasses raw materials in a sugar boiling pot and stirring continuously to obtain a supersaturated sucrose solution, maintaining the syrup temperature below 120°C, and monitoring the syrup brax in real time; when the syrup brax reaches 68-72°Bx, transferring the syrup to a glass dish, cooling to 70°C, adding golden camellia tea polyphenol extract, arabinose and golden camellia micropowder in powder form to the syrup; transferring the syrup to an ultrasonic water bath pot and ultrasonicating at 25-35°C, continuously stirring mechanically until solid matter appears; transferring the obtained solid matter to a metal plate, and drying it in a vacuum drying oven at 63-67°C for 22-24 hours.

2. The method according to claim 1, characterized in that: The mass ratio of golden camellia tea polyphenol extract, arabinose and golden camellia powder is 0.4-0.7:5-8:0.4-0.

7.

3. The method according to claim 1, characterized in that The mass ratio of golden camellia tea polyphenol extract, arabinose and golden camellia powder is 0.5-0.7:6-8:0.5-0.

7.

4. The method according to claim 1, characterized in that The mass ratio of golden camellia tea polyphenol extract to sucrose is 0.4-0.7:

100.

5. The method according to claim 1, characterized in that The particle size of Camellia chrysantha micropowder is <30 microns.