Efficient preparation process for functional modification of flour
By spraying the enhancing solution before wheat grinding and utilizing the synergistic effect of β-cyclodextrin, OSA, GOX and quercetin, the problem of short shelf life of whole wheat flour was solved, and the flour quality stability and production efficiency were improved.
Patent Information
- Application Number
- CN202511094900.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-06
- Publication Date
- 2025-10-10
AI Technical Summary
Whole wheat flour has a short shelf life and is prone to oxidation, rancidity, and microbial growth, which limits its market expansion.
A synergistic solution is sprayed before wheat is crushed. The synergistic solution contains β-cyclodextrin, octenylsuccinic anhydride (OSA), glucose oxidase (GOX) and quercetin. Through synergistic effects, it blocks lipid oxidation, inhibits mold metabolism and scavenges free radicals, forming a hydrophobic anchor-hydrophilic shell structure to improve adsorption uniformity.
Significantly extend the shelf life of whole wheat flour, improve ingredient stability, simplify the process, reduce production costs, optimize adsorption uniformity, and ensure stable flour quality.
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Figure CN120753366A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of flour processing, and specifically to an efficient preparation process for functionalized modification of flour. Background Art
[0002] Flour on the market mainly falls into two categories: regular refined flour and whole-wheat flour. During processing, the bran and germ of regular refined flour are removed, leaving only the endosperm. This results in a fine texture and a soft taste, making it commonly used in making various refined pasta dishes. However, this processing method also results in a significant loss of nutrients, resulting in lower levels of dietary fiber, vitamins, and minerals.
[0003] In comparison, whole-wheat flour retains the bran, germ, and endosperm, providing a more comprehensive nutritional profile. It's rich in dietary fiber, B vitamins, minerals, and various antioxidants. As people's health awareness continues to improve and their focus on the nutritional value of food continues to grow, whole-wheat flour, due to its outstanding nutritional advantages, is becoming increasingly popular among consumers and is widely used in making healthy foods such as whole-wheat bread and whole-wheat biscuits.
[0004] However, whole-wheat flour has a short shelf life. This is because the bran and germ contain high levels of oil and other nutrients that are easily digested by microorganisms. During storage, the oils easily oxidize and become rancid, triggering various biochemical reactions and allowing microorganisms to thrive. These factors combine to cause whole-wheat flour to deteriorate relatively quickly, limiting the further expansion of the whole-wheat food market. Therefore, developing a functionalized modification process that can effectively extend the shelf life of whole-wheat flour has become a pressing technical challenge in the flour processing industry. Summary of the Invention
[0005] In order to solve the problems in the prior art, the present invention provides an efficient preparation process for functionalized modification of flour to solve the above problems.
[0006] To achieve the above object, the present invention provides the following technical solutions:
[0007] An efficient preparation process for functionalized flour modification involves spraying a synergistic solution onto wheat after impurity removal and tempering before grinding into flour. The synergistic solution comprises the following components: β-cyclodextrin, octenylsuccinic anhydride (OSA), glucose oxidase (GOX), and quercetin.
[0008] Preferably, β-cyclodextrin, octenylsuccinic anhydride (OSA), glucose oxidase (GOX) and quercetin are dissolved separately to prepare β-cyclodextrin solution: octenylsuccinic anhydride (OSA) microemulsion, glucose oxidase (GOX) solution and quercetin solution, and then the above four solutions are mixed to obtain a synergistic solution; the specific mixing steps are as follows:
[0009] The beta-cyclodextrin solution is used as a base solution in the mixing tank, a water bath is maintained at 40±2 DEG C, and low-speed stirring is used;
[0010] The prepared OSA microemulsion is slowly added to the beta-cyclodextrin solution, and stirring is continuously performed during the addition process, and the temperature is maintained at 40 DEG C during the stirring process;
[0011] After the dropwise addition is completed, the pH of the mixed solution is adjusted to 8.0-8.5 by using 0.1M NaOH, and stirring is continuously performed for 10 minutes;
[0012] The mixed solution is cooled to below 30 DEG C, and the GOX enzyme solution and the quercetin solution are sequentially added, and the addition should be performed in the dark, and the mixed solution is uniformly stirred to obtain a synergistic solution.
[0013] As preferred, beta-cyclodextrin and distilled water are weighed according to the mass / volume ratio, wherein the concentration of the beta-cyclodextrin is 1%(w / v); the distilled water is preheated to 40±2 DEG C, and the beta-cyclodextrin is slowly added, and stirring is continuously performed until the beta-cyclodextrin is completely dissolved to form a transparent solution.
[0014] As preferred, octenyl succinic anhydride (OSA), anhydrous ethanol and distilled water are weighed according to the mass ratio, wherein OSA:anhydrous ethanol:distilled water = 1:50:449; the distilled water is preheated to 40±2 DEG C and is ready for use; the OSA and the anhydrous ethanol are mixed and stirred until the OSA is completely dissolved to form a uniform oil phase; under the condition of continuous stirring, the oil phase is added dropwise into the preheated distilled water, the dropwise addition time is greater than or equal to 15 minutes, after the dropwise addition is completed, stirring is continuously performed for 10 minutes, and a semi-transparent microemulsion is formed.
[0015] As preferred, glucose oxidase (GOX) powder and distilled water are weighed, wherein the addition amount of the GOX powder is 3.0g of the GOX powder corresponding to 100g of the distilled water; the GOX enzyme solution is obtained by stirring and dissolving.
[0016] As preferred, quercetin 0.5g, anhydrous ethanol 50g and distilled water 949.5g are weighed; and the quercetin solution is obtained by stirring and dissolving.
[0017] As preferred, the amount of the synergistic solution added to 1kg of wheat is 10-15ml.
[0018] As preferred, after the wheat is crushed into whole wheat flour, the whole wheat flour is placed in an environment at 40 DEG C-50 DEG C for 1-2h.
[0019] Compared with the prior art, the present application has the beneficial effects that:
[0020] Compared with the prior art, the present application has the beneficial effects that:
[0021] 1. Significantly Extends the Shelf Life of Whole-Wheat Flour: By spraying a synergistic solution containing β-cyclodextrin, octenylsuccinic anhydride (OSA), glucose oxidase (GOX), and quercetin onto wheat before milling, the ingredients work synergistically. β-cyclodextrin locks in unsaturated fatty acids, blocking the lipid oxidation chain reaction; OSA esterifies with starch, destroying the starch crystals, hindering amylose rearrangement, and slowing the rate of staling; GOX consumes dissolved oxygen, inhibiting mold aerobic metabolism; and quercetin scavenges free radicals, halting lipid peroxidation. This combined effect effectively extends the shelf life of whole-wheat flour, for example, extending the storage life of whole-wheat bread to 45 days at 30°C, addressing the short shelf life of whole-wheat flour that has limited market expansion.
[0022] 2. Simplified process flow: The synergistic solution is sprayed immediately before the wheat is crushed. In this way, the synergistic solution can be fully mixed with the wheat during the subsequent crushing process. There is no need to set up a special mixing process, which reduces the production process, improves production efficiency and reduces production costs.
[0023] 3. Improve the stability of ingredient efficacy: The hydrophobic inner and hydrophilic outer cavity structure of β-cyclodextrin can include quercetin and GOX enzyme, reducing the photolytic loss of quercetin and the attenuation of GOX enzyme activity, ensuring the stability of these two ingredients in the process of extending the shelf life, thereby ensuring the reliability and sustainability of the entire process in extending the shelf life of whole wheat flour.
[0024] 4. Optimizing adsorption uniformity: β-cyclodextrin can be compounded with OSA microemulsion to form a "hydrophobic anchor-hydrophilic shell" structure, which improves the adsorption uniformity of the synergistic solution on the starch surface, avoids excessive starch esterification caused by local excessive concentration, and enables the esterification reaction between OSA and starch to proceed more evenly and effectively, further optimizing the quality of whole wheat flour and playing a positive role in extending the shelf life. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.
[0026] Figure 1 Flowchart of the entire flour preparation process. DETAILED DESCRIPTION
[0027] In order to make the purpose, features, and advantages of this application more obvious and easy to understand, the technical solutions in the embodiments of this application will be clearly and completely described below in conjunction with the drawings in the embodiments of this application. Obviously, the embodiments described below are only part of the embodiments of this application, not all of the embodiments. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of this application.
[0028] 1. Pretreatment of wheat
[0029] The wheat is screened and impurities are removed by using equipment such as vibrating screens and flat rotary screens to separate straw, sand and other impurities.
[0030] Weigh about 50g of wheat after cleaning and place it in an open iron box. Its weight is W1. Place it in a 105℃ oven for drying. After drying for 30 minutes, take out the iron box, dry the lid of the iron box, and weigh it after cooling. Repeat the above steps of drying for 30 minutes, cooling and weighing until the difference between two adjacent weights is less than 0.005g. Stop the drying operation and take the last weighing value as the final constant weight value W2. Calculate the moisture content of the wheat according to the following formula: Moisture (%) = (W1-W2) / W1
[0031] The target moisture content of hard wheat is 15.5% to 17.5%, and that of soft wheat is 14.0% to 15.0%.
[0032] 2. Tempering of Wheat
[0033] The wheat obtained after the pretreatment in step 1 was tempered. The wheat used in this example was Jimai 44, a durum wheat. The target moisture content during tempering was 16%. The wheat was tempered with distilled water, sprayed with water, and transferred to a wheat cleaning cabinet for 24-30 hours.
[0034] 3. Prepare the synergistic solution
[0035] 1. Prepare β-cyclodextrin solution by weighing 50 g of β-cyclodextrin and 4950 g of distilled water. Preheat the distilled water to 40 ± 2°C in a water bath. Slowly add β-cyclodextrin and stir until completely transparent.
[0036] 2. OSA solution: weigh 4 g of OSA solution, 200 g of anhydrous ethanol, and 1796 g of distilled water; adjust the distilled water to 40°C, first mix OSA and ethanol, then add 40°C distilled water dropwise and stir to form a microemulsion.
[0037] 3. GOX enzyme solution: weigh 3 g of GOX powder (5000 U / g) and 100 g of distilled water; stir and dissolve to obtain GOX enzyme solution.
[0038] 4. Quercetin solution: weigh 0.5 g of quercetin, 50 g of anhydrous ethanol, and 949.5 g of distilled water; stir and dissolve to obtain a quercetin solution.
[0039] The steps for preparing and mixing the synergistic solution are as follows:
[0040] The prepared β-cyclodextrin solution was placed in a mixing tank as the base liquid, maintained in a water bath at 40±2°C, and stirred at a low speed.
[0041] Slowly add all of the prepared OSA microemulsion to the β-cyclodextrin solution while stirring continuously during the addition process. Maintain the temperature at 40°C during the stirring process. The addition time should be ≥15 minutes to avoid local excessive concentration causing entrapment.
[0042] After the addition is complete, the pH of the mixture is adjusted to 8.0-8.5 with 0.1 M NaOH (the measured value is usually initial pH ≈ 5.5).
[0043] Continue stirring for 10 minutes to allow the system to reach acid-base equilibrium.
[0044] The mixed solution was cooled to below 30°C, and the GOX enzyme solution (150 g) and quercetin ethanol solution (1 L) prepared above were added in sequence. The mixture should be protected from light during addition, and the mixture was mixed and stirred to obtain a synergistic solution.
[0045] When the wheat is tempered and ready for crushing, spray the synergistic solution on the surface of the wheat. The synergistic solution has a short validity period, which is ≤ 1 hour from the completion of mixing to the end of spraying.
[0046] β-cyclodextrin is a cyclic oligosaccharide composed of seven glucose units, forming a hydrophobic interior and hydrophilic exterior cavity. This cavity can incorporate fat-soluble molecules, locking in the unsaturated fatty acids in whole-wheat flour and blocking the lipid oxidation chain reaction. It can also incorporate quercetin and GOX enzymes, reducing quercetin photolysis loss and GOX enzyme activity attenuation.
[0047] It can also be combined with OSA microemulsion to form a "hydrophobic anchor-hydrophilic shell" structure, improving the uniformity of the enhanced solution's adsorption on the starch surface and preventing localized over-esterification of the starch due to excessive concentration. Octenylsuccinic anhydride (OSA) esterifies with starch hydroxyl groups under alkaline conditions to form starch octenylsuccinate (OSA starch). The OSA groups disrupt the starch's crystalline regions, while the hydrophobic chains hinder the rearrangement of amylose, slowing the rate of staling. This extends the storage life of whole-wheat bread at 30°C to 45 days. OSA is pre-emulsified in an ethanol-water system (40°C) to prevent direct contact with β-cyclodextrin, which could lead to encapsulation failure, and ensure that esterification occurs first.
[0048] The function of GOX enzyme solution is to consume dissolved oxygen and block the aerobic metabolism of molds (such as Aspergillus and Penicillium). The five phenolic hydroxyl groups of quercetin scavenges free radicals through hydrogen bond donor (HBD) and single electron transfer (SET), terminates lipid peroxidation, reduces TBARS value by 40%, and blocks the generation of hydroxyl radicals.
[0049] 4. Wheat Grinding
[0050] The wheat obtained in step 3 was divided into 5 groups, A, B, C, D, and E, and then a control experiment was carried out;
[0051] The wheat in groups A, B, C, and D is placed on a conveyor belt. A nozzle is installed above the conveyor belt to spray the wheat with a sun-drying synergistic solution. The speed of the nozzle spraying the sun-drying synergistic solution is related to the speed of the wheat transported by the conveyor belt, which is 10-15 ml / kg. For example, the conveyor belt used by our company has a speed of 0.5 m / s, a wheat density of 750 kg / m³, a cross-section width of 0.3 m, and a material layer height of 0.05 m; its spraying rate is ≈12.5 mL / kg.
[0052] In one embodiment A, the spraying rate is 10 mL / kg; in one embodiment B, the spraying rate is 12.5 mL / kg; in one embodiment C, the spraying rate is 13.5 mL / kg; in one embodiment D, the spraying rate is 15 mL / kg;
[0053] The conveyor belt then transports the wheat to a grinder for grinding to obtain whole wheat flour; the obtained flour is placed at 40-50°C for 1-2 hours to finally obtain modified whole wheat flour.
[0054] The wheat in group E was placed on a conveyor belt and directly transported to a grinder to obtain whole wheat flour.
[0055] Subsequently, the whole wheat flour obtained from the five groups of wheat, A, B, C, D, and E, was stored in the dark at room temperature, and the odor of the flour was tested every 30 days. The test data are shown in Table 1.
[0056] Table 1
[0057]
[0058] The fatty acid value produced by oil hydrolysis is an important indicator of flour deterioration. Therefore, the fatty acid value of flour is tested every 30 days. The specific test data are shown in Table 2. The unit is mg / 100g, calculated on a wet basis.
[0059] Table 2
[0060]
[0061] In terms of odor, Groups A, B, C, and D all maintained a normal wheat aroma during the early stages of storage (30-60 days), indicating that spraying the synergistic solution before grinding had little effect on the short-term flour odor. However, as time progressed, to 90 days and beyond, Group E, which had not been sprayed with the synergistic solution, developed a distinct sour smell at 90 days. While Groups A, B, C, and D all developed a slightly sweet fermented smell, at 150 days, Group A exhibited a strong rancid smell, while Groups B, C, and D developed a distinct sour smell. This suggests that spraying the synergistic solution can delay the deterioration of flour odor to a certain extent, and that different spraying rates have an impact on this delaying effect. Groups B, C, and D were slightly better than Group A in inhibiting odor deterioration, indicating that in this process, a spraying rate of 12.5-15 mL / kg performs better in maintaining flour odor stability.
[0062] Fatty acid values were lower in Group A than in Group E at all time points tested, demonstrating that the flour functionalization modification process of the present invention, by spraying the synergistic solution before wheat milling, effectively inhibits oil hydrolysis, thereby delaying flour deterioration. Comparing the fatty acid values of Groups A, B, C, and D at 30 days showed little difference, indicating that spraying rates of 10-15 mg / kg initially inhibited oil hydrolysis. However, over time, the fatty acid values of Groups C and D increased more slowly at 60, 90, 120, and 150 days, suggesting that a spray rate of 13.5-15 mL / kg may be more effective in long-term oil hydrolysis inhibition and controlling flour deterioration. The data for Groups C and D showed little difference, indicating that increasing the spray rate to 13.5 mg / kg had little effect on inhibiting oil hydrolysis. This series of data provides a strong basis for optimizing the spraying rate of the synergistic solution to achieve a more ideal flour shelf life extension effect.
[0063] As described above, the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them. Although the present application has been described in detail with reference to the above embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the above embodiments, or make equivalent replacements for some of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the spirit and scope of the technical solutions of the embodiments of the present application.
Claims
1. An efficient preparation process for functionalized modification of flour, characterized in that: After the wheat is removed from the wheat and tempered, it is sprayed with a synergistic solution before being crushed and ground into flour. The synergistic solution contains the following components: beta-cyclodextrin, octenylsuccinic anhydride (OSA), glucose oxidase (GOX) and quercetin.
2. An efficient preparation process for functionalized modification of flour, characterized in that: β-cyclodextrin, octenylsuccinic anhydride (OSA), glucose oxidase (GOX) and quercetin are dissolved separately to prepare β-cyclodextrin solution: octenylsuccinic anhydride (OSA) microemulsion, glucose oxidase (GOX) solution and quercetin solution, and then the above four solutions are mixed to obtain a synergistic solution; the specific mixing steps are as follows: Place the β-cyclodextrin solution as the base liquid in a mixing tank, maintain a water bath at 40±2℃, and stir at a low speed; Slowly add all of the prepared OSA microemulsion to the β-cyclodextrin solution, stirring continuously during the addition process, and maintain the temperature at 40°C during the stirring process; After the addition was complete, the pH of the mixture was adjusted to 8.0-8.5 with 0.1 M NaOH and stirring was continued for 10 minutes; The mixed solution was cooled to below 30°C, and GOX enzyme solution and quercetin solution were added in sequence. The addition should be protected from light, and the mixture was mixed and stirred to obtain a synergistic solution.
3. The efficient preparation process for functionalized flour modification according to claim 2, characterized in that: The β-cyclodextrin solution was prepared as follows: β-cyclodextrin and distilled water were weighed in a mass-to-volume ratio, wherein the β-cyclodextrin concentration was 1% (w / v); the distilled water was preheated to 40±2°C, and the β-cyclodextrin was slowly added, with continuous stirring until it was completely dissolved to form a transparent solution.
4. The efficient preparation process for functionalized flour modification according to claim 2, characterized in that: Weigh octenylsuccinic anhydride (OSA), anhydrous ethanol, and distilled water in a mass ratio of 1:50:449; preheat distilled water to 40±2°C and set aside; first mix OSA with anhydrous ethanol and stir until completely dissolved to form a uniform oil phase; under continuous stirring, add the oil phase dropwise to the preheated distilled water for ≥15 minutes. After the addition is complete, continue stirring for 10 minutes to form a translucent microemulsion.
5. The efficient preparation process for functionalized modification of flour according to claim 2, characterized in that: Glucose oxidase (GOX) powder and distilled water were weighed, wherein the amount of GOX powder added was 3.0 g per 100 g of distilled water; and the mixture was stirred and dissolved to obtain a GOX enzyme solution.
6. The efficient preparation process for functionalized modification of flour according to claim 2, characterized in that: Weigh 0.5 g of quercetin, 50 g of anhydrous ethanol, and 949.5 g of distilled water; stir and dissolve to obtain a quercetin solution.
7. The efficient preparation process for functionalized flour modification according to claim 1, characterized in that: The amount of enhanced solution added per 1kg of wheat is 10~15ml.
8. The efficient preparation process for functionalized flour modification according to claim 1, characterized in that: After the wheat is crushed into whole wheat flour, the whole wheat flour is placed in an environment of 40℃~50℃ for 1~2h.