Enzymatic preparation process of flaxseed diglyceride oil
Flaxseed diglyceride oil was prepared by combining cold pressing, stacked physical cycle dephosphorization, and low-temperature crystallization adsorption with enzymatic methods. This solved the problems of high-temperature oxidation loss and low enzyme reuse rate, achieving efficient and low-energy production of flaxseed diglyceride oil, and improving product stability and economy.
Patent Information
- Application Number
- CN202511408515.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-29
- Publication Date
- 2025-11-18
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
In existing technologies, the high temperature during the preparation of flaxseed oil leads to the oxidation and loss of polyunsaturated fatty acids, the immobilized lipase has a low reusability rate, and the traditional dephosphorization process results in phospholipid residues that affect product stability and human absorption.
Cold-pressed flaxseed oil was prepared by cold pressing, combined with stacked physical cycle dephosphorization and low-temperature crystallization adsorption. The LipaseRMIM and Novozym435 complex enzymes were used to catalyze the reaction in a micro-aqueous system, and the enzymes were recovered by vibration. Finally, the low-temperature crystallization adsorption method was used for dewaxing. The process parameters were optimized to improve the enzyme reuse rate and product quality.
It significantly reduces the oxidative loss rate of α-linolenic acid to below 3%, the residual phospholipid content is less than 8 ppm, the product shelf life is extended to 18 months, the cost of enzyme reuse is reduced by 50%, the energy consumption throughout the process is low, and it is suitable for industrial production.
Smart Images
Figure CN120966923A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of glyceride oil preparation, and particularly relates to an enzymatic preparation process of flaxseed glyceride oil. BACKGROUND
[0002] As a highly respected edible vegetable oil, flaxseed oil occupies an important position in the field of healthy diet due to its outstanding nutritional value and multiple health benefits. It is rich in various beneficial components for the human body, especially unsaturated fatty acids, which can reach 86% or even higher. Among these unsaturated fatty acids, the content of alpha-linolenic acid is particularly outstanding, which can be as high as 30%-60%. Compared with common healthy oils such as walnut oil, oil tea seed oil and olive oil, the content of alpha-linolenic acid in flaxseed oil is much higher, and the advantage is obvious.
[0003] Alpha-linolenic acid is an essential fatty acid for the human body, which has multiple important physiological functions in the human body. Flaxseed oil is rich in alpha-linolenic acid, and thus has a series of remarkable health benefits. In terms of cardiovascular health, it can play an outstanding regulatory role. On the one hand, it can reduce the content of cholesterol and triglycerides in the blood, effectively reduce the deposition of lipids in the blood vessel wall, and thus reduce blood lipid levels; on the other hand, it can also act on vascular smooth muscle, dilate blood vessels, and reduce peripheral vascular resistance, thereby achieving the effect of reducing blood pressure. At the same time, flaxseed oil can help improve insulin sensitivity and regulate blood glucose metabolism, which is also helpful for reducing blood sugar. In addition, it can inhibit platelet aggregation, prevent thrombosis, and prevent the occurrence and development of atherosclerosis, comprehensively protecting the cardiovascular system and reducing the risk of cardiovascular disease, which is of great significance for the prevention of cardiovascular diseases that are highly prevalent in modern society.
[0004] In addition to the significant benefits to the cardiovascular system, flaxseed oil also has a wide range of health benefits. It contains rich antioxidant substances that can scavenge free radicals in the body, reduce oxidative stress damage to cells, thereby delaying cell aging and playing an anti-aging role. In terms of anti-tumor, some components in flaxseed oil can regulate the immune system, enhance the body's immunity, and inhibit the growth and spread of tumor cells. For cognitive function, it can improve blood circulation to the brain, provide sufficient nutrients for the brain, and help improve memory, attention and thinking ability, and improve cognitive function. In terms of eye health, the nutritional components in flaxseed oil have a protective effect on the retina and optic nerve of the eye, and can improve eye diseases such as dry eye syndrome and retinopathy, and keep the eyes in a healthy state.
[0005] The current situation of glyceride oil is as follows:
[0006] 1. Value of DAG oil: DAG is a natural functional lipid with the functions of inhibiting fat accumulation and regulating blood sugar, and the market demand is significant.
[0007] 2. Defects of prior art: The traditional preparation requires high temperature (> 200℃), and the oxidation loss of polyunsaturated fatty acids (alpha linolenic acid) in flaxseed oil occurs in the pressing or enzyme preparation process.
[0008] In the existing enzyme process, the reuse rate of immobilized lipase is low (< 5 times), and the product separation depends on molecular distillation, which has high energy consumption.
[0009] 3. Properties of flaxseed oil: the content of alpha linolenic acid is > 50%, but it is heat sensitive, and the conventional dephosphorization process easily leads to the residual of phospholipids (> 50ppm), which affects the stability of the product. In addition, the flaxseed oil contains waxes (60mg / kg) after oil preparation, which affects human absorption. Therefore, an enzyme preparation process of flaxseed DAG oil is proposed. SUMMARY
[0010] The purpose of the present application is to provide an enzyme preparation process of flaxseed DAG oil to solve the problems in the background art.
[0011] In order to solve the above technical problems, the present application adopts the following technical scheme:
[0012] An enzyme preparation process of flaxseed DAG oil, comprising the following steps:
[0013] S1: flaxseed as raw material, cold-pressed to obtain cold-pressed flaxseed oil;
[0014] S2: The cold-pressed flaxseed oil is subjected to stacked physical cycle dephosphorization, and the cycle time is 2 hours. The phospholipid content after dephosphorization is < 8ppm;
[0015] S3: Enzymatic reaction: a composite enzyme composed of Lipase RMIM and Novozym435 in a mass ratio of 3:1 is used to catalyze the reaction of flaxseed oil and glycerol in a micro-water system at 40℃, wherein the mass ratio of flaxseed oil to glycerol is 5:1, the addition amount of composite enzyme is 5%, and the water addition amount is 6%, and the reaction time is 2h;
[0016] S4: The oil product after reaction is subjected to low-temperature crystallization adsorption dewaxing, and the wax content is reduced to below 0.3mg / kg, to obtain flaxseed DAG oil.
[0017] Preferably, the temperature of cold pressing is < 70 degrees, and the acid value of the obtained cold-pressed flaxseed oil is ≤ 0.5mg / kg, and the peroxide value is ≤ 0.15g / 100g.
[0018] Preferably, the enzymatic reaction is carried out in a stacked microporous reactor, and the micropore diameter of the stacked microporous reactor is 1 to 50 micrometers, and the porosity is 30% to 70%.
[0019] Preferably, the complex enzyme is recovered by vibration after use.
[0020] Preferably, the specific operation steps of the low-temperature crystallization adsorption dewaxing method include: cooling the reacted oil product to -5°C, cooling and crystallizing at a rate of 1°C / min for 8 hours, then adding an adsorbent, adsorbing at 20°C for 2 hours, and finally filtering to obtain dewaxed flaxseed diglyceride oil.
[0021] Preferably, the adsorbent is one or a combination of activated clay, diatomaceous earth, and bentonite.
[0022] Preferably, the amount of adsorbent added is 3%-8% of the mass of the oil product.
[0023] A flaxseed diglyceride oil prepared by an enzymatic process, wherein the α-linolenic acid oxidation loss rate of the flaxseed diglyceride oil is <3%, the phospholipid residue is <8ppm, the shelf life is extended to 18 months at 25°C, and the DAG conversion rate is ≥52.3%.
[0024] It is clear without a doubt that the technical solution described above in this application can solve the technical problem that this application aims to address.
[0025] Meanwhile, through the above technical solutions, the present invention has at least the following beneficial effects:
[0026] Flaxseed diglyceride oil prepared by the process of this invention:
[0027] 1. The oxidative loss rate of α-linolenic acid is <3%, which is significantly better than that of high-temperature chemical method (>15%).
[0028] 2. Phospholipid residue <8ppm, product shelf life extended to 18 months (25℃).
[0029] 3. The cost of reusing enzymes is reduced by 50%, which greatly saves production costs.
[0030] 4. Low energy consumption throughout the process, low equipment requirements, and easy operation, making it suitable for industrial production. Attached Figure Description
[0031] To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the following description of the embodiments will be briefly introduced. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0032] Fig. 1 This is a schematic diagram of the process flow of the present invention;
[0033] Fig. 2 This is a schematic diagram illustrating the specific operation steps of the low-temperature crystallization adsorption dewaxing method of the present invention. Detailed Implementation
[0034] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.
[0035] Example 1
[0036] Reference Figs. 1-2 An enzymatic process for preparing flaxseed diglyceride oil includes the following steps:
[0037] S1: Cold-pressed flaxseed oil is obtained by cold pressing flaxseed.
[0038] S2: Cold-pressed flaxseed oil is subjected to stacked physical circulation dephosphorization for 2 hours, and the phospholipid content after dephosphorization is <8ppm.
[0039] S3: Enzymatic reaction: A compound enzyme consisting of LipaseRMIM and Novozym435 in a mass ratio of 3:1 was used to catalyze the reaction of flaxseed oil and glycerol in a micro-aqueous system at 40℃. The mass ratio of flaxseed oil to glycerol was 5:1, the amount of compound enzyme added was 5% (w / w), the amount of water added was 6%, and the reaction time was 2 hours. The amount of water added to the micro-aqueous system was 7%. The DAG conversion rate was increased by 12% compared with that of a single enzyme.
[0040] S4: The oil products after the reaction were dewaxed by low-temperature crystallization adsorption method, and the wax content was reduced to below 0.3 mg / kg to obtain flaxseed diglyceride oil.
[0041] The cold pressing temperature is <70 degrees Celsius, and the resulting cold-pressed flaxseed oil has an acid value ≤0.5mg / kg and a peroxide value ≤0.15g / 100g.
[0042] The enzymatic reaction is carried out in a stacked microporous reactor with a pore size of 1–50 micrometers and a porosity of 30%–70%. By immobilizing the complex enzyme in the stacked microporous reactor, the reaction area is increased on the one hand, and the filter membrane is formed on the other hand, thereby increasing the reaction area and improving the reaction efficiency. Furthermore, the immobilized lipase has a high reusability (up to 10 times) and is easy to separate.
[0043] After use, the compound enzyme was recovered by vibration. After being reused 10 times, its activity was 85% retained. In a comparative experiment, without the use of the compound enzyme and gradient dephosphorization and dewaxing, the DAG conversion rate was only 61.2%, the phospholipid residue was 35 ppm, and the wax content was 60 mg / kg.
[0044] The specific steps of low-temperature crystallization adsorption dewaxing include: cooling the reacted oil product to -5℃, crystallizing at a rate of 1℃ / min for 8 hours, then adding an adsorbent and adsorbing at 20℃ for 2 hours, and finally filtering to obtain dewaxed flaxseed diglyceride oil; low-temperature gradient dephosphorylation and dewaxing technology: Step 1: Stacked physical circulation dephosphorization without the addition of chemical agents, safe and hygienic, and thorough dephosphorization. Step 2: Low-temperature crystallization adsorption dewaxing, which is highly efficient, and the dewaxed product (<0.3mg / kg) is more easily absorbed by the human body.
[0045] The adsorbent is one or a combination of activated clay, diatomaceous earth, and bentonite. The amount of adsorbent added is 3%-8% of the mass of the oil product.
[0046] In this embodiment, the specific operational details and parameter control for each step are as follows:
[0047] Raw material pretreatment: Select high-quality flaxseeds and use cold pressing technology to strictly control the pressing temperature below 70 degrees Celsius to avoid the destruction of nutrients in flaxseed oil by high temperature, so as to obtain cold-pressed flaxseed oil with acid value and peroxide value that meet the standards, providing high-quality raw materials for subsequent reactions.
[0048] Dephosphorization process: Cold-pressed flaxseed oil is placed in a stacked physical circulation dephosphorization device and circulated at room temperature for 2 hours. Phospholipid impurities are effectively removed through physical action, reducing the phospholipid content to below 8 ppm, ensuring product stability and quality.
[0049] Enzymatic reaction conditions were optimized by precisely controlling the mass ratio of flaxseed oil to glycerol in the reaction system to 5:1, adding an appropriate amount of compound enzyme (LipaseRMIM and Novozym435 in a 3:1 mass ratio) and water (6%), and conducting a circulating reaction for 2 hours in a stacked microporous reactor at 40℃. The design of the stacked microporous reactor increases the reaction area and acts as a filter membrane, improving reaction efficiency and product yield, while also facilitating enzyme recovery and reuse.
[0050] Dewaxing process: The oil products after the reaction are dewaxed by low-temperature crystallization adsorption method. By controlling parameters such as temperature and time, the wax is effectively precipitated and adsorbed and removed, and the wax content is reduced to below 0.3 mg / kg, which significantly improves the absorbability and quality of the product.
[0051] Enzyme recovery and reuse: The enzymes after the reaction are recovered by vibration recovery method. After multiple reuses, the enzyme activity can still be retained by more than 85%, which greatly reduces the production cost, improves the production efficiency and economic benefits, and provides strong support for large-scale industrial production.
[0052] In summary, this invention achieves an efficient, energy-saving, and environmentally friendly enzymatic preparation process for flaxseed diglyceride oil through key technologies such as synergistic catalysis of a composite enzyme system, low-temperature gradient dephosphorylation and dewaxing, and optimization of reaction and separation processes. It has significant economic and social benefits and broad market application prospects.
[0053] Example 2
[0054] A flaxseed diglyceride oil prepared by an enzymatic process has an α-linolenic acid oxidation loss rate of <3%, a phospholipid residue of <8ppm, a shelf life extended to 18 months at 25°C, and a DAG conversion rate of ≥52.3%.
[0055] In summary:
[0056] The present invention addresses the following technical problem: the shortcomings of existing technology: traditional preparation requires high temperature (>200℃), which leads to the oxidation and loss of polyunsaturated fatty acids (α-linolenic acid) in flaxseed oil during the pressing or enzymatic process.
[0057] In existing enzymatic processes, the reusability of immobilized lipases is low (<5 times), and product separation relies on molecular distillation, which consumes a lot of energy.
[0058] 3. Characteristics of flaxseed oil: While it contains >50% α-linolenic acid, it is highly heat-sensitive, and conventional dephosphorization processes easily lead to phospholipid residues (>50 ppm), affecting product stability. Furthermore, flaxseed oil contains wax (60 mg / kg), which affects human absorption. By employing the technical solutions of the above embodiments and through the aforementioned settings, this application can certainly solve the above-mentioned technical problems and achieve the following technical effects:
[0059] Flaxseed diglyceride oil prepared by the process of this invention:
[0060] 1. The oxidative loss rate of α-linolenic acid is <3%, which is significantly better than that of high-temperature chemical method (>15%).
[0061] 2. Phospholipid residue <8ppm, product shelf life extended to 18 months (25℃).
[0062] 3. The cost of reusing enzymes is reduced by 50%, which greatly saves production costs.
[0063] 4. Low energy consumption throughout the process, low equipment requirements, and easy operation, making it suitable for industrial production.
[0064] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection, an electrical connection, or a connection that allows communication between them; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.
[0065] Obviously, the embodiments described above are merely some embodiments of the present invention, not all embodiments. The accompanying drawings show preferred embodiments of the present invention, but do not limit the patent scope of the present invention. The present invention can be implemented in many different forms; rather, these embodiments are provided to provide a more thorough and complete understanding of the disclosure of the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing specific embodiments, or make equivalent substitutions for some of the technical features. Any equivalent structures made using the content of this specification and drawings, directly or indirectly applied to other related technical fields, are similarly within the patent protection scope of this invention.
Claims
1. An enzymatic process for preparing flaxseed diglyceride oil, characterized in that, Includes the following steps: S1: Cold-pressed flaxseed oil is obtained by cold pressing flaxseed. S2: Cold-pressed flaxseed oil is subjected to stacked physical circulation dephosphorization for 2 hours, and the phospholipid content after dephosphorization is <8ppm. S3: Enzymatic reaction: A compound enzyme consisting of LipaseRMIM and Novozym435 in a mass ratio of 3:1 was used to catalyze the reaction of flaxseed oil and glycerol at 40℃ in a micro-aqueous system. The mass ratio of flaxseed oil to glycerol was 5:1, the amount of compound enzyme added was 5%, the amount of water added was 6%, and the reaction time was 2h. S4: The oil products after the reaction were dewaxed by low-temperature crystallization adsorption method, and the wax content was reduced to below 0.3 mg / kg to obtain flaxseed diglyceride oil.
2. The enzymatic preparation process of flaxseed diglyceride oil according to claim 1, characterized in that, The cold pressing temperature is <70 degrees Celsius, and the resulting cold-pressed flaxseed oil has an acid value ≤0.5 mg / kg and a peroxide value ≤0.15 g / 100 g.
3. The enzymatic preparation process for flaxseed diglyceride oil according to claim 1, characterized in that, The enzymatic reaction is carried out in a stacked microporous reactor, and the micropore diameter of the stacked microporous reactor is 1 to 50 micrometers, with a porosity of 30% to 70%.
4. The enzymatic preparation process of flaxseed diglyceride oil according to claim 1, characterized in that, The complex enzyme is recovered by vibration after use.
5. The enzymatic preparation process for flaxseed diglyceride oil according to claim 1, characterized in that, The specific steps of the low-temperature crystallization adsorption method for dewaxing include: cooling the reacted oil product to -5°C, crystallizing at a rate of 1°C / min for 8 hours, then adding an adsorbent, adsorbing at 20°C for 2 hours, and finally filtering to obtain dewaxed flaxseed diglyceride oil.
6. The enzymatic preparation process of flaxseed diglyceride oil according to claim 5, characterized in that, The adsorbent is one or more of activated clay, diatomaceous earth, and bentonite.
7. The enzymatic preparation process of flaxseed diglyceride oil according to claim 6, characterized in that, The amount of adsorbent added is 3%-8% of the mass of the oil product.
8. A flaxseed diglyceride oil prepared by the enzymatic preparation process according to any one of claims 1-7, characterized in that, The flaxseed diglyceride oil has an α-linolenic acid oxidation loss rate of <3%, a phospholipid residue of <8ppm, a shelf life extended to 18 months at 25°C, and a DAG conversion rate of ≥52.3%.