Production process of mesembryanthemum crystallinum extract
By using a decolorizing agent made from a compound of food-grade activated carbon and diatomaceous earth, along with a strong acidic cation exchange resin and ultrafiltration membrane technology, the problems of residual organic solvents and unscientific decolorization and deacidification in ice plant extract have been solved, achieving efficient and low-cost production of ice plant extract.
Patent Information
- Application Number
- CN202511450058.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-11
- Publication Date
- 2026-01-16
AI Technical Summary
Existing methods for extracting ice plant often result in high levels of residual organic solvents, which affects food safety. Furthermore, the decolorization and deacidification processes are not scientifically sound, leading to poor product purity and quality. In addition, the production process is complex and costly.
Food-grade activated carbon and diatomaceous earth are used as a decolorizing agent, combined with a strong acidic cation exchange resin and an ultrafiltration membrane for decolorization and deacidification. The process involves simple equipment and procedures, including raw material pretreatment, extraction, filtration, concentration and drying, while controlling parameters such as temperature and pressure.
It improves the extraction rate of active ingredients and the purity of the product, reduces production costs, meets food safety standards, and simplifies the production process.
Smart Images
Figure CN121343665A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of biological extraction, in particular to a production process of ice leaf extract. BACKGROUND
[0002] Ice leaf, scientific name of Mesembryanthemum crystallinum, as a new functional vegetable, is rich in various components beneficial to human body, such as amino acids, minerals and unique secondary metabolites; research shows that ice leaf extract has the effects of supplementing electrolytes, regulating body metabolism and antioxidant, and has broad application prospects in the fields of sports drinks, health foods and nutritional supplements.
[0003] The traditional ice leaf extraction method is mainly organic solvent extraction method, but the residual amount is too high after extraction with organic solvent, which does not meet the relevant standards of food safety, limiting the application of the extract in the fields of food and health products, and the residual organic solvent also causes harm to human health; secondly, the existing decolorization process mostly adopts single activated carbon decolorization method, and the addition amount of activated carbon is usually determined by experience, lacking scientific basis, which easily leads to excessive or insufficient decolorization, affecting the purity of the product; the existing deacidification process adopts chemical neutralization method, but introduces new impurity ions, which affects the quality of the extract; in addition, the existing ice leaf extract production process relies on complex equipment and tedious operation process, which consumes a large amount of energy and resources, further increasing the production cost. SUMMARY
[0004] The purpose of the present application is to provide an ice leaf extract production process to solve the technical problems existing in the prior art.
[0005] In order to achieve the above-mentioned purpose of the application, the technical scheme adopted by the present application is:
[0006] The application discloses a production process of an extract of Ilex hainanensis, which comprises the following steps: S1, raw material selection and pretreatment; S2, extraction; S3, decolorization; S4, deacidification; S5, purification; S6, concentration and drying; and S7, quality inspection.
[0007] Further, the plate-and-frame filter in the S2 step adopts a polypropylene filter cloth with a pore size of 0.32-0.45 Further, the resin in the S4 step is treated by being soaked in a 5%-8% hydrochloric acid solution for 1-2 hours and continuously stirred, then washed with deionized water until the pH value is 5-6, then soaked in a 5%-8% sodium hydroxide solution for 2-3 hours, then washed with deionized water until the pH value is 7-8, and finally soaked in deionized water for 1-1.5 hours.
[0008] Further, the plate-and-frame filter in the S2 step adopts a polypropylene filter cloth with a pore size of 0.32-0.45 Further, the resin in the S4 step is treated by being soaked in a 5%-8% hydrochloric acid solution for 1-2 hours and continuously stirred, then washed with deionized water until the pH value is 5-6, then soaked in a 5%-8% sodium hydroxide solution for 2-3 hours, then washed with deionized water until the pH value is 7-8, and finally soaked in deionized water for 1-1.5 hours.
[0009] Further, the ultrafiltration system in the S5 step comprises an ultrafiltration membrane assembly, a high-pressure pump, a pressure gauge and a temperature control system; the ultrafiltration membrane in the ultrafiltration membrane assembly is made of polyether sulfone material, and has a molecular weight cut-off range of 1000-5000 Da.
[0010] Further, the S7 step comprises intermediate control and finished product control; the intermediate control comprises extraction liquid concentration detection, color detection after decolorization, acidity detection after deacidification and purity detection after purification; the finished product control comprises sensory index detection, physicochemical index detection and microbial index detection.
[0011] Compared with the prior art, the present application has the following beneficial effects:
[0012] (1) The present application improves the extraction rate and integrity of effective ingredients by selecting raw materials, pretreating and extracting, which can more fully extract the amino acids, minerals and other nutrients in the ice vegetables, thereby improving the utilization rate of raw materials;
[0013] (2) The present application selects food-grade activated carbon and diatomite as decolorizing agents through the decolorization and deacidification steps, which makes the decolorization effect more ideal and avoids the loss of effective ingredients caused by excessive decolorization; the selection and treatment of strong acid cation exchange resin can effectively remove acidic substances in the ice vegetable extract, improve the stability and taste of the product, and meet the needs of different application fields;
[0014] (3) The present application is simple to operate and does not require complex equipment, and the ion exchange resin can be recycled, and the ultrafiltration membrane can also be reused after cleaning, which reduces the cost of auxiliary materials and thus reduces the overall production cost. BRIEF DESCRIPTION OF DRAWINGS
[0015] Figure 1 The flowchart of the present application. DETAILED DESCRIPTION
[0016] In order to make the content of the present application more easily understood, the technical solutions in the embodiments of the present application will be described clearly and completely below in conjunction with the drawings in the embodiments of the present application. The same parts are denoted by the same reference numerals. It should be noted that the words "front", "back", "left", "right", "up" and "down" used in the following description refer to the directions in the drawings, and the words "inner" and "outer" refer to the directions towards or away from the geometric center of a particular part.
[0017] Example 1:
[0018] As shown in the drawings, Figure 1 The present embodiment provides an ice vegetable extract production process, comprising the following steps:
[0019] S1: Raw material selection and pretreatment. After washing, the ice plant is drained and then placed in a crushing device for crushing. The crushed ice plant is then sieved to form uniform particles of 2mm. Specifically, fresh, non-rotten, and pest-free ice plant is selected, and its growing environment meets the requirements of GB / T 19630 "Requirements for Organic Product Production, Processing, Labelling and Management System". Ice plant grown in areas with industrial pollution and pesticide abuse should be avoided. The qualified ice plant is placed in a washing tank and rinsed with running water for 3 minutes. During the rinsing process, it is gently stirred to remove surface mud, dust and residual impurities. After washing, the ice plant is allowed to drain naturally or centrifuged to avoid excessive moisture, which could lead to inaccurate extraction liquid-to-material ratio in the subsequent process.
[0020] S2: Extraction. Crushed ice plant particles and deionized water are added to an extraction tank at a mass ratio of 1:8. The temperature is controlled at 60℃, and extraction is carried out for 2 hours. Intermittent stirring is used during extraction to ensure sufficient contact between the ice plant particles and water, improving extraction uniformity. After extraction, the extract is filtered through a plate and frame filter press to obtain a preliminary extract. The plate and frame filter press has a pore size of 0.32 mm. The filter cloth is made of polypropylene, and the filtration pressure is controlled at 0.35MPa. Before filtration, the extract is cooled to 40℃ to avoid deformation of the filter cloth due to high temperature.
[0021] S3: Decolorization. Food-grade activated carbon and diatomaceous earth are mixed in a 2:1 mass ratio as the decolorizing agent. The activated carbon has adsorption capacity and can adsorb pigment molecules; the diatomaceous earth has good filtration properties. 3% (by mass) of the mixed decolorizing agent is added to the preliminary extract, and the mixture is stirred at 55°C for 40 minutes at a stirring speed of 80 r / min to ensure sufficient contact between the decolorizing agent and the extract. The decolorized extract is then filtered using a filtration device to ensure complete removal of the decolorizing agent and residual impurities.
[0022] S4: Deacidification. The decolorized extract is passed through an ion exchange column packed with the treated resin at a flow rate of 1 BV / h for deacidification. The acidity of the effluent is monitored in real time, and the feeding is stopped when the acidity reaches a preset standard. The preset standard is that the pH of the resin-saturated effluent is continuously greater than 6. The resin treatment steps are as follows: the resin is soaked in a 5% hydrochloric acid solution for 1 hour with continuous stirring; then rinsed with deionized water until the pH value is 5; then soaked in a 5% sodium hydroxide solution for 2 hours; then rinsed with deionized water until the pH value is 7; then soaked in deionized water for 1 hour to allow the resin to fully swell; after the resin is saturated, a regenerant of twice the resin volume (5% hydrochloric acid solution) is used for regeneration treatment. During the regeneration treatment, the regeneration flow rate is controlled at 2 BV / h and the regeneration time is 1.5 hours. Then, the regenerated resin is rinsed with deionized water until neutral and can be recycled.
[0023] S5: Purification. The deacidified and decolorized solution is fed into an ultrafiltration system using cross-flow filtration at a velocity of 2 m / s. The operating pressure is controlled at 0.1 MPa and the operating temperature at 25°C to remove macromolecular impurities such as proteins and polysaccharides, thereby improving the purity of the extract. The purified solution permeating through the membrane is collected in a sealed storage tank. The ultrafiltration system includes an ultrafiltration membrane module, a high-pressure pump, a pressure gauge, and a temperature control system. The ultrafiltration membrane in the ultrafiltration membrane module is made of polyethersulfone material with a molecular weight cutoff of 1000 Da.
[0024] S6: Concentration and drying. The purified solution is placed in a double-effect external circulation vacuum concentrator, and the vacuum degree is controlled at -0.08MPa and the concentration temperature is controlled at 50℃. When the solid content is 20%, the concentration is stopped. The concentrated solution is placed in a centrifugal spray dryer, and the inlet air temperature is controlled at 180℃, the outlet air temperature is controlled at 80℃, the feed rate is controlled at 20L / h, and the atomizing disc speed is controlled at 15000r / min for drying. The dried powder is cooled to room temperature and then sieved to obtain ice plant extract powder. The concentration and drying steps can retain the nutrients, color and aroma of ice plant extract, while improving the solubility and flowability of the product.
[0025] S7: Quality Inspection. The dried ice plant extract powder obtained in step S6 and each subsequent step are tested, and qualified products are packaged for later use. Step S7 includes intermediate control and finished product control. Intermediate control includes extract concentration testing, color testing after decolorization, acidity testing after deacidification, and purity testing after purification. The specific method for color testing after decolorization is to test each batch of decolorized extract three times, and to test the turbidity of the filtrate after filtration. The specific method for acidity testing after deacidification is to test the pH value of the effluent. Finished product control includes sensory index testing, physicochemical index testing, and microbiological index testing. Physicochemical index testing includes testing the moisture, ash content, and effective ingredient content of the finished product. Microbiological index testing uses the plate count method to test the total bacterial count, coliform bacteria, and other microbiological indicators to ensure that the product meets food safety standards.
[0026] Example 2:
[0027] This embodiment provides a process for producing ice plant extract, including the following steps:
[0028] S1: Raw material selection and pretreatment. After washing, the ice plant is drained and then placed in a crushing device for crushing. The crushed ice plant is then sieved to form uniform 5mm particles. Specifically, fresh, non-rotten, and pest-free ice plant is selected, and its growing environment meets the requirements of GB / T 19630 "Requirements for Organic Product Production, Processing, Labelling and Management System". Ice plant grown in areas with industrial pollution and pesticide abuse should be avoided. The qualified ice plant is placed in a washing tank and rinsed with running water for 5 minutes. During the rinsing process, it is gently stirred to remove surface mud, dust and residual impurities. After washing, the ice plant is allowed to drain naturally or centrifuged to avoid excessive moisture, which could lead to inaccurate extraction liquid-to-material ratio in the subsequent process.
[0029] S2: Extraction. Crushed ice plant particles and deionized water are added to an extraction tank at a mass ratio of 1:12. The temperature is controlled at 80℃, and extraction is carried out for 3 hours. Intermittent stirring is used during extraction to ensure sufficient contact between the ice plant particles and water, improving extraction uniformity. After extraction, the extract is filtered through a plate and frame filter press to obtain a preliminary extract. The plate and frame filter press uses a pore size of 0.45 mm. The filter cloth is made of polypropylene, and the filtration pressure is controlled at 0.5MPa. Before filtration, the extract is cooled to 50℃ to avoid deformation of the filter cloth due to high temperature.
[0030] S3: Decolorization. Food-grade activated carbon and diatomaceous earth are mixed in a 3:1 mass ratio as the decolorizing agent. The activated carbon has adsorption capacity and can adsorb pigment molecules; the diatomaceous earth has good filtration properties. 5% (by mass) of the mixed decolorizing agent is added to the preliminary extract, and the mixture is stirred at 60°C for 60 minutes at a speed of 100 r / min to ensure sufficient contact between the decolorizing agent and the extract. The decolorized extract is then filtered using a filtration device to ensure complete removal of the decolorizing agent and residual impurities.
[0031] S4: Deacidification. The decolorized extract is passed through an ion exchange column packed with the treated resin at a flow rate of 1.5 BV / h for deacidification. The acidity of the effluent is monitored in real time, and the feeding is stopped when the acidity reaches a preset standard. The preset standard is that the pH of the resin-saturated effluent is continuously greater than 6. The resin treatment steps are as follows: the resin is soaked in an 8% hydrochloric acid solution for 2 hours with continuous stirring; then rinsed with deionized water until the pH value is 6; then soaked in an 8% sodium hydroxide solution for 3 hours; then rinsed with deionized water until the pH value is 8; then soaked in deionized water for 1.5 hours to allow the resin to fully swell; after the resin is saturated, a regenerant of 3 times the resin volume (6% hydrochloric acid solution) is used for regeneration treatment. During the regeneration treatment, the regeneration flow rate is controlled at 2.5 BV / h and the regeneration time is 2 hours. Then, the regenerated resin is rinsed with deionized water until neutral and can be recycled.
[0032] S5: Purification. The deacidified and decolorized solution is fed into an ultrafiltration system using cross-flow filtration at a velocity of 3 m / s. The operating pressure is controlled at 0.2 MPa and the operating temperature at 35°C to remove macromolecular impurities such as proteins and polysaccharides, thereby improving the purity of the extract. The purified solution permeating through the membrane is collected in a sealed storage tank. The ultrafiltration system includes an ultrafiltration membrane module, a high-pressure pump, a pressure gauge, and a temperature control system. The ultrafiltration membrane in the ultrafiltration membrane module is made of polyethersulfone material with a molecular weight cutoff of 5000 Da.
[0033] S6: Concentration and drying. The purified solution is placed in a double-effect external circulation vacuum concentrator, and the vacuum degree is controlled at -0.09MPa and the concentration temperature is controlled at 60℃. When the solid content is 30%, the concentration is stopped. The concentrated solution is placed in a centrifugal spray dryer, and the inlet air temperature is controlled at 200℃, the outlet air temperature is controlled at 90℃, the feed rate is controlled at 30L / h, and the atomizing disc speed is controlled at 20000r / min for drying. The dried powder is cooled to room temperature and then sieved to obtain ice plant extract powder. The concentration and drying steps can retain the nutrients, color and aroma of ice plant extract, while improving the solubility and flowability of the product.
[0034] S7: Quality Inspection. The dried ice plant extract powder obtained in step S6 and each subsequent step are tested, and qualified products are packaged for later use. Step S7 includes intermediate control and finished product control. Intermediate control includes extract concentration testing, color testing after decolorization, acidity testing after deacidification, and purity testing after purification. The specific method for color testing after decolorization is to test each batch of decolorized extract three times, and to test the turbidity of the filtrate after filtration. The specific method for acidity testing after deacidification is to test the pH value of the effluent. Finished product control includes sensory index testing, physicochemical index testing, and microbiological index testing. Physicochemical index testing includes testing the moisture, ash content, and effective ingredient content of the finished product. Microbiological index testing uses the plate count method to test the total bacterial count, coliform bacteria, and other microbiological indicators to ensure that the product meets food safety standards.
[0035] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.
Claims
1. A process for the production of an extract of Gynura divaricata, characterized in that: The method comprises the following steps: S1: raw material selection and pretreatment, draining the washed ice vegetables, then putting them into a crushing device for crushing, and sieving the crushed ice vegetables; S2: extraction, putting the crushed ice vegetable particles and deionized water into an extraction tank according to a mass ratio of 1:8-1:12, controlling the temperature at 60-80 DEG C, and extracting for 2-3 h, wherein intermittent stirring is adopted during the extraction; after the extraction is completed, the extraction liquid is filtered in a plate and frame filter to obtain a preliminary extraction liquid; S3: decolorization, using food-grade activated carbon and diatomite as a decolorizing agent, adding the decolorizing agent into the preliminary extraction liquid according to a mass ratio of 2:1-3:1, stirring and decolorizing at 55-60 DEG C for 40-60 min, and controlling the stirring speed at 80-100 r / min; then filtering to obtain a decolorized extraction liquid; S4: deacidification, passing the decolorized extraction liquid through an ion exchange column filled with treated resin at a flow rate of 1-1.5 BV / h to remove acid, and stopping the liquid feeding when the acidity reaches a preset standard; S5: purification, putting the deacidified decolorized liquid into an ultrafiltration system, adopting a cross-flow filtration mode, controlling the cross-flow speed at 2-3 m / s, controlling the operating pressure at 0.1-0.2 MPa, and controlling the operating temperature at 25-35 DEG C; collecting the purified liquid passing through the membrane in a sealed storage tank; S6: concentration and drying, putting the purified liquid into a double-effect external-circulation vacuum concentrator, controlling the vacuum degree at-0.08--0.09 MPa, and controlling the concentration temperature at 50-60 DEG C; stopping the concentration when the solid content is 20%-30%; putting the concentrated liquid into a centrifugal spray dryer, controlling the air inlet temperature at 180-200 DEG C, the air outlet temperature at 80-90 DEG C, the feeding rate at 20-30 L / h, and the atomizing disc rotating speed at 15000-20000 r / min to dry the liquid; cooling the dried powder to room temperature, and sieving to obtain ice vegetable extract powder; S7: quality inspection, detecting the ice vegetable extract powder obtained in the step S6 and each step, and packaging the qualified product.
2. The production process of the Gynura medica extract according to claim 1, characterized by: The plate-and-frame filter in the S2 step uses a filter cloth of polypropylene material with a pore size of 0.32-0.45 MPa.
3. The production process of the Gynura medica extract according to claim 1, characterized by: In the step S4, the treatment of the resin comprises the following steps: soaking the resin in a 5%-8% hydrochloric acid solution for 1-2 h while continuously stirring; then washing the resin with deionized water until the pH value is 5-6; then soaking the resin in a 5%-8% sodium hydroxide solution for 2-3 h; then washing the resin with deionized water until the pH value is 7-8; and then soaking the resin in deionized water for 1-1.5 h.
4. The production process of the Gynura medica extract according to claim 1, characterized by: In the step S5, the ultrafiltration system comprises an ultrafiltration membrane assembly, a high-pressure pump, a pressure gauge and a temperature control system; the ultrafiltration membrane in the ultrafiltration membrane assembly is made of polyether sulfone material, and has a molecular weight cut-off range of 1000-5000 Da.
5. The production process of the Gynura medica extract according to claim 1, characterized by: In the step S7, the quality inspection comprises intermediate control and finished product control; the intermediate control comprises extraction liquid concentration detection, color detection after decolorization, acidity detection after deacidification and purity detection after purification; and the finished product control comprises sensory index detection, physical and chemical index detection and microbial index detection.