Soybean milk beverage with high ligustilide content and preparation process thereof
Through ultra-low temperature freezing treatment and liquid nitrogen freezing process combined with black soy milk dissolution, enzyme reaction and ultrasonic crushing technology, the problem of low degradation and extraction efficiency of angelica lactone content in Angelica is solved, and soy milk drinks with high angelica lactone content are prepared. A unique and efficient process flow is achieved.
Patent Information
- Application Number
- CN202411559585.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-04
- Publication Date
- 2025-01-10
AI Technical Summary
The prior art is difficult to effectively retain and increase the content of oxypropion lactone in angelica volatile oil, and the processing technology is complex, which affects its stability and extraction efficiency.
The angelica was crushed by ultra-low temperature freezing treatment and liquid nitrogen freezing process. Combined with black soy milk dissolution, enzyme reaction and ultrasonic crushing technology, a high-grade soy milk drink with a content of more than 80μg/g of lactone was prepared.
The content of oxopropion lactone is greatly retained, and the crushing efficiency and extraction efficiency are improved. The prepared soy milk drink has a unique flavor and is simple and easy to produce in industrial form.
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of food processing, and in particular to a soy milk beverage with high ligustilide content and a preparation process thereof. Background Art
[0003] Black beans, also known as black beans and shovel beans, are the black seeds of soybeans, a legume plant. Black beans are rich in protein, fat, phospholipids, vitamins, essential amino acids and trace elements. Its protein content is much higher than other beans. Black beans also contain cardiac glycosides, soybean saponins, flavonoids, antioxidant substances and other functional factors. Modern nutritional analysis shows that every 100g of black beans contains 36g of protein, 15.9g of fat, 23.4g of carbohydrates, 17.36mg of vitamin E, 7mg of iron, 4.18mg of zinc, 1377mg of potassium, and 6.79μg of selenium. The black bean polysaccharides and anthocyanins contained in black beans can remove free radicals in the human body and delay aging; the isoflavones in black beans can effectively block the proliferation of blood vessels in malignant tumors, thereby delaying or preventing the occurrence of tumors; the vitamin E in black beans is an antioxidant that can play a role in anti-wrinkle and beauty.
[0004] Modern research has found that angelica is rich in volatile oils, polysaccharides, organic acids and other chemical components. Angelica volatile oil is a volatile aromatic substance in the root of angelica, mainly composed of phthalide compounds such as ligustilide and butenylphthalide, which has multiple effects such as lowering blood pressure, anti-inflammatory, anti-tumor, and antioxidant. Among them, ligustilide is the main indicator for evaluating the quality of angelica volatile oil, and is usually used as a measure of the stability of angelica volatile oil. Ligustilide has an active butenyl group in its structure, which is prone to chemical reactions such as hydrolysis, dehydrogenation, and oxidation when placed at room temperature. It is sensitive to light, heat, oxygen and other conditions. External conditions such as light and oxygen will accelerate its isomerization process, and its stability is poor. Studies have shown that the content of ligustilide dropped from 99.48% to 41.97% after being placed at room temperature for half a month.
[0005] Research scholars have conducted relatively more research on the processing technology of angelica sinensis and its active ingredient angelica oil, but less research on the processing technology of high ligustilide content. Summary of the invention
[0006] The purpose of the present invention is to provide a soy milk beverage with a high ligustilide content and a preparation process thereof. After angelica is subjected to ultra-low temperature freezing treatment and made into angelica powder, it is dissolved in black soybean milk, subjected to enzyme reaction, and subjected to ultrasonic crushing process to prepare a soy milk beverage with a high ligustilide content of more than 80 μg / g and a unique flavor.
[0007] In order to achieve the above object, the technical solution adopted by the present invention is as follows:
[0008] The present specification provides a preparation process of black soybean milk with high ligustilide content, comprising:
[0009] The angelica is subjected to ultra-low temperature freezing and crushing treatment to prepare angelica powder;
[0010] Mixing angelica powder and black soybean milk in a set ratio to form a primary slurry;
[0011] Mixing cellulase and the primary slurry in a set ratio and reacting for a set time under constant temperature conditions to form a secondary slurry;
[0012] In a low temperature environment of -4°C to +4°C, the secondary slurry is subjected to ultrasonic grinding to form a soy milk beverage with a high ligustilide content of more than 80 μg / g.
[0013] After the angelica medicinal material is subjected to ultra-low temperature freezing treatment, the content of ligustilide in angelica oil, the effective ingredient of angelica medicinal material, is greatly retained, and the crushing efficiency is greatly increased. The crushed angelica powder is more conducive to full fusion with black soybean milk. When the crushed angelica powder is dissolved in black soybean milk, it is fully stirred for 2 to 5 minutes to make the angelica powder fully dissolved in the black soybean milk. The fat-soluble vitamins and antioxidants such as vitamin E and vitamin K contained in the black soybean milk can reversely protect the ligustilide in angelica oil. Cellulase can decompose plant cell walls and further release the medicinal ingredients in angelica. The reaction under constant temperature conditions can effectively ensure the activity of the enzyme to improve efficiency. Ultrasonic waves can further break up plant cell walls and cell membranes to fully release ligustilide.
[0014] According to the above method, after the angelica is ultra-low temperature frozen and made into angelica powder, it is dissolved in black soybean milk, subjected to enzyme reaction, and ultrasonic crushing process to prepare a soybean milk beverage with a high ligustilide content of more than 80 μg / g and a unique flavor.
[0015] Furthermore, the angelica is subjected to ultra-low temperature freezing treatment using a liquid nitrogen freezing process and then crushed into angelica powder.
[0016] The ultra-low temperature rapid freezing treatment of Angelica sinensis using liquid nitrogen freezing technology can effectively prevent the degradation of ligustilide, greatly retaining the content of ligustilide in angelica oil, the effective ingredient of Angelica sinensis. The ultra-low temperature liquid nitrogen freezing process can make the Angelica sinensis tissue brittle and easy to crush to obtain finer powder, which is convenient for subsequent operations.
[0017] Furthermore, the angelica root subjected to the ultra-low temperature freezing treatment is crushed at 35-45° C. into angelica root powder of 80-200 meshes.
[0018] Ligustilide is very easy to undergo chemical reactions such as hydrolysis, dehydrogenation, and oxidation. Low temperature environment can inhibit the occurrence of these reactions and effectively retain its activity. Making angelica into fine particles of angelica powder is more conducive to the dissolution of angelica powder and is conducive to increasing the content of ligustilide in soy milk beverages.
[0019] Furthermore, in the primary slurry, the mass ratio of angelica powder to black soybean milk is 1:90-100.
[0020] Furthermore, in the secondary slurry, the concentration of the cellulase is 1.5% to 5%.
[0021] Cellulase can decompose plant cell walls and, through enzymatic reactions, can increase the content of ligustilide in the solution. A cellulase concentration of 1.5% to 5% can both ensure the efficiency of the enzymatic reaction and avoid side reactions and increased costs caused by excessive enzyme concentrations.
[0022] Furthermore, the set time is 30 to 40 minutes.
[0023] An extraction time that is too short may result in insufficient extraction of ligustilide; an extraction time that is too long may affect the flavor of the soy milk beverage; an extraction time of 30 to 40 minutes can ensure that cellulase is in full contact with the plant cell wall and carry out an effective enzymatic reaction, thereby increasing the extraction rate of ligustilide.
[0024] Furthermore, the constant temperature condition refers to using 40-50°C liquid for liquid phase insulation.
[0025] Appropriate temperature can promote the activity of cellulase. 40-50℃ is the most suitable temperature for cellulase, which can ensure the efficiency of enzymatic reaction and avoid the destruction of ligustilide by high temperature, so as to increase the content of ligustilide in soy milk beverage. Liquid phase insulation can keep the temperature of black soy milk stable and ensure the uniformity of enzymatic reaction.
[0026] Furthermore, the secondary slurry is subjected to ultrasonic grinding in a low temperature environment constructed by an ice-water mixture, and the ultrasonic grinding time is 1.5 to 2 hours.
[0027] Ultrasonic waves can further break plant cells and fully release active ingredients such as ligustilide. During ultrasonic crushing, placing black soybean milk in a low-temperature environment constructed by an ice-water mixture can effectively prevent the destruction of ligustilide. The ultrasonic crushing time is controlled at 1.5 to 2 hours. Sufficient ultrasonic crushing time can ensure the full release of ligustilide, increase the content of ligustilide in soybean milk drinks, and avoid the loss of active ingredients caused by excessive ultrasound.
[0028] Furthermore, the black soybean milk is prepared by mixing black soybean powder and 40-50°C warm water, wherein the mass ratio of the black soybean powder to 40-50°C warm water is 1:8-10.
[0029] The present specification also provides a soy milk beverage with a high ligustilide content, which is prepared according to the above-mentioned soy milk beverage preparation process, and is characterized in that the content of ligustilide in the soy milk beverage is above 80 μg / g.
[0030] Due to the adoption of the above technical solution, the present invention has the following beneficial effects:
[0031] 1. After being subjected to ultra-low temperature rapid freezing treatment, the content of ligustilide in angelica oil, the effective ingredient of angelica, is greatly retained, and the crushing efficiency is greatly increased; the crushed angelica powder is fully dissolved in black soybean milk, and the fat-soluble vitamins and antioxidants such as vitamin E and vitamin K contained in black soybean milk are used to reversely protect the ligustilide in angelica oil; cellulase is used to decompose the plant cell wall to further release the effective ingredients in angelica; ultrasonic crushing technology is used to further break up the plant cells to fully release ligustilide. According to the above method, after angelica is subjected to ultra-low temperature freezing treatment and made into angelica powder, it can be prepared into a soy milk beverage with a high ligustilide content of more than 80μg / g and a unique flavor after being dissolved in black soybean milk, enzyme reaction, and ultrasonic crushing process.
[0032] 2. The preparation process provided by the present invention is simple to operate and is easy to industrialize. DETAILED DESCRIPTION
[0033] Some embodiments of the present invention are described in detail below. In the absence of conflict, the features of the following embodiments can be combined with each other.
[0034] The endpoints and any values of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the endpoint values of each range, the endpoint values of each range and the individual point values, and the individual point values can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.
[0035] A process for preparing a soymilk beverage with a high ligustilide content, comprising but not limited to the following steps:
[0036] (1) Cut the angelica root into 0.1-0.3 cm thin slices;
[0037] (2) After the angelica slices are subjected to ultra-low temperature rapid freezing treatment by liquid nitrogen freezing process, the angelica slices are crushed into 100 mesh angelica powder at 35-45° C.;
[0038] (3) mixing black bean powder and 40-50° C. warm water in a set ratio to prepare black bean milk, wherein the mass ratio of black bean powder to 40-50° C. warm water is 1:10; mixing angelica powder and black bean milk in a set ratio to form a primary slurry, wherein the mass ratio of angelica powder to black bean milk in the primary slurry is 1:90-100, and stirring thoroughly for 2-5 minutes;
[0039] (4) mixing the cellulase and the primary slurry in a set ratio, and reacting for a set time under a constant temperature condition to form a secondary slurry, wherein: the concentration of the cellulase in the secondary slurry is 3%, the set time is 30 to 40 minutes, and the constant temperature condition refers to using a 45° C. liquid for liquid phase insulation;
[0040] (5) The secondary slurry is subjected to ultrasonic grinding in a low temperature environment constructed by an ice-water mixture, and the ultrasonic grinding time is 1.5 to 2 hours to form a black soybean milk beverage with a high ligustilide content exceeding 80 μg / g.
[0041] The method is adopted to prepare black soybean milk, and the content of ligustilide in the prepared black soybean milk is tested by high performance liquid chromatography analysis, and the content of ligustilide is above 80 μg / g.
[0042] The effect of this method is demonstrated by some embodiments and comparative examples below.
[0043] In the following examples and comparative examples, the test methods used are all conventional methods unless otherwise specified; the raw materials used are all raw materials that can be obtained from conventional commercial channels, among which Angelica sinensis was purchased from Bozhou Xier Chinese Herbal Medicine Co., Ltd.; after preparation, the content of ligustilide in the prepared black soybean milk was tested by high performance liquid chromatography.
[0044] Example 1
[0045] The preparation process comprises the following steps:
[0046] (1) Cut the angelica root into 0.1 cm thin slices;
[0047] (2) using a liquid nitrogen freezing process to rapidly freeze the angelica slices at an ultra-low temperature of -196°C, and then pulverizing the angelica slices at a temperature of 45°C to a size of 100 mesh;
[0048] (3) Dissolve 18 g of pure black bean milk powder in 180 g of 45°C warm water, then dissolve 2.0 g of ground angelica powder in the black bean milk in a 45°C constant temperature water bath, and stir thoroughly for 2 min;
[0049] (4) Extraction was performed using cellulase at a concentration of 3% and the solution was placed in a constant temperature water bath at 45°C for 30 min;
[0050] (5) The solution was ultrasonically crushed at a low temperature of 0° C. (the solution was placed in an ice-water mixture) using ultrasonic crushing technology for 1.5 h.
[0051] It was determined that the content of ligustilide in black soybean milk was 96.63 μg / g.
[0052] Example 2
[0053] The preparation process comprises the following steps:
[0054] (1) Cut the angelica root into 0.3 cm thin slices;
[0055] (2) using a liquid nitrogen freezing process to rapidly freeze the angelica slices at an ultra-low temperature of -196°C, and then pulverizing the angelica slices at a temperature of 45°C to a size of 100 mesh;
[0056] (3) Dissolve 18 g of pure black bean milk powder in 180 g of 45°C warm water, then dissolve 2.0 g of ground angelica powder in the black bean milk in a 45°C constant temperature water bath, and stir thoroughly for 5 min;
[0057] (4) Extraction was performed using cellulase at a concentration of 3% and the solution was placed in a constant temperature water bath at 45°C for 40 min;
[0058] (5) The solution is ultrasonically crushed at a low temperature of 0° C. (the solution is placed in an ice-water mixture) using ultrasonic crushing technology for 2 h.
[0059] It was determined that the content of ligustilide in black soybean milk was 90.27 μg / g.
[0060] Example 3
[0061] The preparation process comprises the following steps:
[0062] (1) Cut the angelica root into 0.2 cm thin slices;
[0063] (2) using a liquid nitrogen freezing process to rapidly freeze the angelica slices at an ultra-low temperature of -196°C, and then pulverizing the angelica slices at a temperature of 45°C to a size of 100 mesh;
[0064] (3) Dissolve 18 g of pure black bean milk powder in 180 g of 45°C warm water, then dissolve 2.0 g of ground angelica powder in the black bean milk in a 45°C constant temperature water bath, and stir thoroughly for 3 min;
[0065] (4) Extraction was performed using cellulase at a concentration of 3% and the solution was placed in a constant temperature water bath at 45°C for 30 min;
[0066] (5) The solution was ultrasonically crushed at a low temperature of 0° C. (the solution was placed in an ice-water mixture) using ultrasonic crushing technology for 2 h.
[0067] It was determined that the content of ligustilide in black soybean milk was 93.13 μg / g.
[0068] Comparative Example 1
[0069] The preparation process comprises the following steps:
[0070] (1) Cut the angelica root into 0.1 cm thin slices;
[0071] (2) crushing the angelica slices at a temperature of 45° C. and grinding them into 100 mesh;
[0072] (3) Dissolve 18 g of pure black bean milk powder in 180 g of 45°C warm water, then dissolve 2.0 g of ground angelica powder in the black bean milk in a 45°C constant temperature water bath, and stir thoroughly for 2 min;
[0073] (4) Extraction was performed using cellulase at a concentration of 3% and the solution was placed in a constant temperature water bath at 45°C for 30 min;
[0074] (5) The solution was ultrasonically crushed at a low temperature of 0° C. (the solution was placed in an ice-water mixture) using ultrasonic crushing technology for 1.5 h.
[0075] It was determined that the content of ligustilide in black soybean milk was 36.78μg / g.
[0076] The main difference between Comparative Example 1 and Examples 1 to 3 is that no liquid nitrogen ultra-low temperature rapid freezing treatment is performed.
[0077] Comparative Example 2
[0078] The preparation process comprises the following steps:
[0079] (1) Cut the angelica root into 0.2 cm thin slices;
[0080] (2) using a liquid nitrogen freezing process to rapidly freeze the angelica slices at an ultra-low temperature of -196°C, and then pulverizing the angelica slices at a temperature of 45°C to a size of 100 mesh;
[0081] (3) Dissolve 18 g of pure black bean milk powder in 180 g of 45°C warm water, then dissolve 2.0 g of ground angelica powder in the black bean milk in a 45°C constant temperature water bath, and stir thoroughly for 3 min;
[0082] (4) Extraction was performed using cellulase at a concentration of 3% and the solution was placed in a constant temperature water bath at 95°C for 30 min;
[0083] (5) Using ultrasonic pulverization technology, the solution was ultrasonically pulverized at 55°C (the solution was placed in a 55°C constant temperature water bath) for 1.5 h.
[0084] It was determined that the content of ligustilide in black soybean milk was 51.29 μg / g.
[0085] The main difference between Comparative Example 2 and Examples 1 to 3 is that during ultrasonic pulverization, the solution was placed in a constant temperature water bath at 55°C.
[0086] Comparative Example 3
[0087] The preparation process comprises the following steps:
[0088] (1) Cut the angelica root into 0.3 cm thin slices;
[0089] (2) using a liquid nitrogen freezing process to rapidly freeze the angelica slices at an ultra-low temperature of -196°C, and then pulverizing the angelica slices at a temperature of 45°C to a size of 100 mesh;
[0090] (3) Dissolve 2.0 g of ground angelica powder in 198 g of pure water at 45 °C and stir thoroughly for 5 min;
[0091] (4) Extraction was performed using cellulase at a concentration of 3% and the solution was placed in a constant temperature water bath at 45°C for 30 min;
[0092] (5) The solution was ultrasonically crushed at a low temperature of 0° C. (the solution was placed in an ice-water mixture) using ultrasonic crushing technology for 1.5 h.
[0093] It was determined that the content of ligustilide in black soybean milk was 39.89μg / g.
[0094] The main difference between Comparative Example 3 and Examples 1 to 3 is that the black soybean milk base is replaced with water.
[0095] Comparative Example 4
[0096] The preparation process comprises the following steps:
[0097] (1) Cut the angelica root into 0.1 cm thin slices;
[0098] (2) using a liquid nitrogen freezing process to rapidly freeze the angelica slices at an ultra-low temperature of -196°C, and then pulverizing the angelica slices at a temperature of 45°C to a size of 100 mesh;
[0099] (3) Dissolve 18 g of pure black bean milk powder in 180 g of 45°C warm water, then dissolve 2.0 g of ground angelica powder in the black bean milk in a 45°C constant temperature water bath, and stir thoroughly for 2 min;
[0100] (4) Extraction was performed using cellulase at a concentration of 1% and the solution was placed in a constant temperature water bath at 45°C for 30 min;
[0101] (5) The solution was ultrasonically crushed at a low temperature of 0° C. (the solution was placed in an ice-water mixture) using ultrasonic crushing technology for 1.5 h.
[0102] It was determined that the content of ligustilide in black soybean milk was 48.63μg / g.
[0103] The main difference between Comparative Example 4 and Examples 1 to 3 is that the concentration of cellulase is 1%.
[0104] The ligustilide content of the prepared black soybean milk was tested by high performance liquid chromatography (test results are shown in Table 1).
[0105] Reagents: Methanol was of chromatographic grade.
[0106] Standard product: Ligustilide standard product, purity>99.01%.
[0107] Preparation of sample solution: Accurately weigh 25 mg of black soybean milk, dilute with methanol, make up to 25 mL volumetric flask, mix well and place at room temperature, filter with a microporous membrane (0.45 μm), and take the filtrate as the test solution for testing.
[0108] Table 1 Schemes and ligustilide contents of the embodiments and comparative examples
[0109] Test items Ligustilide content (μg / g) Example 1 96.63 Example 2 90.27 Example 3 93.13 Comparative Example 1 36.78 Comparative Example 2 51.29 Comparative Example 3 39.89 Comparative Example 4 48.63
[0110] It can be seen from the above experiments that the angelica slices are quickly frozen at -196°C by liquid nitrogen, and then crushed to 100 mesh at 35-45°C. 18g of pure black bean milk powder is dissolved in 180g of 45°C warm water, and then 2.0g of the ground angelica powder is dissolved in black soybean milk in a 45°C constant temperature water bath and stirred for 2-5min. Extraction is carried out using 3% concentration of cellulase. During the extraction, the solution is reacted in a 45°C constant temperature water bath for 30-40min. The solution is ultrasonically crushed at a low temperature of 0°C (the solution is placed in an ice-water mixture) using ultrasonic crushing technology, and the ultrasonic time is 1.5-2h. Compared with comparative examples 1-4, the black soybean milk prepared using the above preparation process has a unique flavor and a high content of ligustilide, and the content of ligustilide is above 80μg / g.
[0111] The above is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily thought of by a person skilled in the art within the technical scope disclosed by the present invention should be included in the protection scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims
1. A process for preparing a soybean milk beverage with a high ligustilide content, characterized in that: include: The angelica is subjected to ultra-low temperature freezing and crushing treatment to prepare angelica powder; Mixing angelica powder and black soybean milk in a set ratio to form a primary slurry; Mixing cellulase and the primary slurry in a set ratio and reacting for a set time under constant temperature conditions to form a secondary slurry; In a low temperature environment of -4°C to +4°C, the secondary slurry is subjected to ultrasonic grinding to form a soy milk beverage with a high ligustilide content of more than 80 μg / g.
2. The process for preparing soybean milk beverage according to claim 1, characterized in that: The angelica is ultra-low temperature frozen by liquid nitrogen freezing process and then crushed into angelica powder.
3. The process for preparing soybean milk beverage according to claim 2, characterized in that: The angelica root subjected to the ultra-low temperature freezing treatment is crushed at 35-45° C. into angelica root powder of 80-200 meshes.
4. The process for preparing soybean milk beverage according to claim 1, characterized in that: In the primary slurry, the mass ratio of angelica powder to black soybean milk is 1:90-100.
5. The process for preparing soybean milk beverage according to claim 1, characterized in that: In the secondary slurry, the concentration of the cellulase is 1.5% to 5%.
6. The process for preparing soybean milk beverage according to claim 5, characterized in that: The setting time is 30 to 40 minutes.
7. The process for preparing soybean milk beverage according to claim 6, characterized in that: The constant temperature condition refers to using 40-50°C liquid for liquid phase insulation.
8. The process for preparing soybean milk beverage according to claim 1, characterized in that: The secondary slurry is subjected to ultrasonic grinding in a low temperature environment constructed by an ice-water mixture, and the ultrasonic grinding time is 1.5 to 2 hours.
9. The process for preparing a soy milk beverage according to any one of claims 1 to 8, characterized in that: The black soybean milk is prepared by mixing black soybean powder and 40-50°C warm water, wherein the mass ratio of the black soybean powder to the 40-50°C warm water is 1:8-10.
10. A soymilk beverage with a high ligustilide content, prepared by the soymilk beverage preparation process according to any one of claims 1 to 9, characterized in that: The content of ligustilide in the soy milk beverage is above 80 μg / g.