Oligosaccharide pectin gels loaded with a fat-soluble active ingredient and methods for their preparation

CN117678751BActive Publication Date: 2026-08-18HEBEI AGRICULTURAL UNIV.
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Patent Information

Application Number
CN202410004343.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-01-02
Publication Date
2026-08-18
Estimated Expiration
2044-01-02

AI Technical Summary

Technical Problem

但由于乳液稳定性差,不易包埋完全川陈皮素,可将其制备成乳液凝胶

Benefits of technology

[0025] (1) Noriheptacortin has excellent anti-cancer, anti-inflammatory, anti-allergic, and antioxidant effects. However, noriheptacortin has multiple methoxy groups, low polarity, planar structure, high hydrophobicity, high lipid solubility, and low bioavailability. Furthermore, pectin emulsions have poor stability and are not easily encapsulated completely. This invention utilizes oligosaccharides to prepare an oligosaccharide pectin emulsion gel that can stably load lipid-soluble active ingredients. This emulsion gel can solve the problem of emulsion instability and overcome the limitation of hydrogels in only delivering hydrophilic substances. It can prevent flocculation and aggregation and may prolong the intestinal drug release time.

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Abstract

The application provides an oligosaccharide pectin gel loaded with fat-soluble active ingredients and a preparation method thereof, and relates to the field of food processing technology. The application mixes and extracts pectin from fruit processing by-products after pretreatment and hydrochloric acid solution; directly mixes fat-soluble active ingredients with pectin or embeds fat-soluble active ingredients with essential oils and then mixes the essential oils with pectin to obtain pectin loaded with fat-soluble ingredients; adjusts the pH of the pectin, adds gluconolactone and oligosaccharides, and obtains oligosaccharide pectin gel loaded with fat-soluble ingredients after heating and cooling. The application obtains low-sugar emulsion gel jellies and soft candies with good appearance and taste, meets the market demand for low-sugar, rich-in-prebiotics and polyphenol emulsion jellies, has the functional properties of regulating intestinal flora, anti-cancer, anti-inflammatory, anti-allergic and anti-oxidation, and has a simple processing technology, is easy to popularize, and has a wide market prospect.
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Description

Technical Field

[0001] This invention relates to the field of food processing technology, specifically to an oligosaccharide gum gel loaded with fat-soluble active ingredients and its preparation method. Background Technology

[0002] Pectin is a water-soluble linear polysaccharide with galacturonic acid (GalA) as its backbone, mainly found in the cell walls of higher plants. Based on the degree of esterification, pectin is generally classified into high-methoxyl (HM) pectin (degree of esterification DE>50%) and low-methoxyl (LM) pectin (DE<50%). HM gel formation requires low pH and a high concentration of soluble solids, while LM gel formation requires calcium... 2+ The participation of HM and the presence of a small number of ions. HM, compared to LM, does not require Ca... 2+ Under certain conditions, gel formation can be achieved by adjusting the acid-to-sugar ratio. At higher sugar concentrations, the interaction between HM molecules and water molecules weakens, while the interaction between pectin molecules becomes more favorable, enhancing the gel stability of the pectin. Fruit-derived pectins are mostly high-methoxyl pectins. High-methoxyl pectin gels are "cold-set pectins," exhibiting rapid gelation at high temperatures and good thermal stability and gelling properties. However, high-methoxyl pectin gels require excessively high sugar concentrations, and high sugar intake may increase health risks.

[0003] Oligosaccharides are less sweet and lower in calories than sucrose, and possess good moisturizing properties and high viscosity. The stability of oligosaccharides depends on the content of sugar residues, ring form, end-group configuration, and linkage type. Functional oligosaccharides are generally low-degree polymeric sugars formed by 2–10 monosaccharides linked by glycosidic bonds. They are non-digestible carbohydrates with unique physiological functions that selectively promote the proliferation and growth of specific intestinal microorganisms, benefiting host health. Oligosaccharides can prevent tooth decay, improve diarrhea, and have immune activity and anti-tumor effects. Oligosaccharide prebiotics are less sweet than sucrose, cannot be utilized by putrefactive bacteria in the human mouth, cannot be digested and absorbed by the human intestine, and have a low caloric value. Therefore, they are widely used in functional sweeteners and are a high-quality sugar substitute.

[0004] Fat-soluble active ingredients such as nonotrimonin are abundant in citrus pomace and possess various beneficial biological activities, such as regulating metabolic disorders, anti-inflammation, and anti-cancer properties. However, due to its high melting point, high hydrophobicity, and poor water solubility, its bioavailability is low. Therefore, the human body has difficulty effectively absorbing and utilizing nonotrimonin, which greatly limits its biological activity and industrial application. Encapsulating fat-soluble nutrients such as β-carotene, lycopene, and vitamin D3 using nanoemulsions can effectively improve their bioavailability. However, due to the poor stability of emulsions, it is difficult to completely encapsulate nonotrimonin; therefore, it can be prepared as an emulsion gel.

[0005] Emulsion gels are semi-solid materials with stable spatial network structures and strong mechanical properties. They are gel systems formed on the basis of emulsions through certain induction methods, mainly including two gel formation mechanisms: emulsion droplet filling and gel matrix encapsulation and re-aggregation of droplets. Due to their excellent encapsulation properties and controlled-release advantages, emulsion gels can effectively improve the storage and transport of bioactive substances, increasing their bioavailability, and are often used in drug delivery and targeted delivery. Emulsion gels can solve the problem of emulsion instability and overcome the limitation of hydrogels in delivering only hydrophilic substances. They can prevent flocculation and aggregation, and may prolong the release time of drugs into the intestine.

[0006] Therefore, it is particularly important to develop a new method for preparing pectin gels rich in oligosaccharide prebiotics loaded with fat-soluble active ingredients and possessing a stable spatial network structure. Summary of the Invention

[0007] In view of this, the present invention aims to provide a method for preparing oligosaccharide pectin gel loaded with fat-soluble active ingredients, thereby obtaining a low-sugar prebiotic pectin gel with excellent appearance and taste. The pectin gel is loaded with fat-soluble active ingredients, has a dense gel network, good elasticity, and strong cohesion.

[0008] To achieve the above-mentioned objectives, the present invention provides the following technical solution:

[0009] This invention provides a method for preparing oligosaccharide gum gel loaded with a fat-soluble active ingredient, comprising the following steps:

[0010] The pretreated fruit processing byproducts are mixed with hydrochloric acid solution to obtain a mixture. The mixture is stirred, cooled, and filtered to obtain a filtrate. The filtrate is then precipitated with alcohol and filtered to obtain pectin.

[0011] After the pectin is dried, a pectin solution is prepared. After the pectin solution is swollen, 0.2-0.3 mg / mL of tangeretin is added. After ultrasonic dissolution, the pH value is adjusted to 2-3.5. Gluconolactone and oligosaccharides are added. After heating, the solution is cooled and solidified to obtain pectin gel.

[0012] This invention also provides a method for preparing oligosaccharide gum gel loaded with a fat-soluble active ingredient, comprising the following steps:

[0013] The pretreated fruit processing byproducts are mixed with hydrochloric acid solution to obtain a mixture. The mixture is stirred, cooled, and filtered to obtain a filtrate. The filtrate is then precipitated with alcohol and filtered to obtain pectin.

[0014] After drying, the pectin is prepared into a pectin solution, which is then swollen and used as the aqueous phase. Medium-chain triglycerides and bergamot oil are mixed to obtain a mixed oil. 1-5 mg / mL of hesperidin is weighed and added to the mixed oil and dissolved by ultrasonication to obtain the oil phase. The aqueous phase and oil phase are mixed at a mass ratio of 6-15:1-3 and homogenized to obtain a pectin emulsion.

[0015] The pH of the pectin emulsion was adjusted to 2-3.5, gluconolactone and oligosaccharides were added, and after heating, the mixture was cooled and solidified to obtain pectin gel.

[0016] Preferably, the oligosaccharide includes stachyose or dextran.

[0017] More preferably, the amount of stachyose added is 60% to 70%; and the amount of dextran added is 30% to 40%.

[0018] Preferably, the stirring is carried out at 70-80°C for 2-3 hours at a speed of 1000-1200 rpm.

[0019] Preferably, the ultrasound is performed at 40–60°C for 60–99 minutes.

[0020] Preferably, the mass ratio of the pretreated fruit processing by-product to the hydrochloric acid solution is 1:10-30.

[0021] Preferably, during alcohol precipitation, the volume ratio of the filtrate to ethanol is 1:1 to 5.

[0022] More preferably, the alcohol precipitation time is 12 to 24 hours.

[0023] Preferably, the mass ratio of the medium-chain triglycerides to bergamot oil is 0.5–2:0.5–2.

[0024] Compared with the prior art, the present invention has the following advantages:

[0025] (1) Noriheptacortin has excellent anti-cancer, anti-inflammatory, anti-allergic, and antioxidant effects. However, noriheptacortin has multiple methoxy groups, low polarity, planar structure, high hydrophobicity, high lipid solubility, and low bioavailability. Furthermore, pectin emulsions have poor stability and are not easily encapsulated completely. This invention utilizes oligosaccharides to prepare an oligosaccharide pectin emulsion gel that can stably load lipid-soluble active ingredients. This emulsion gel can solve the problem of emulsion instability and overcome the limitation of hydrogels in only delivering hydrophilic substances. It can prevent flocculation and aggregation and may prolong the intestinal drug release time.

[0026] (2) This invention utilizes oligosaccharides to prepare gels. Oligosaccharides are a type of prebiotic. Prebiotics refer to organic substances that are not digested and absorbed by the host but can selectively promote the metabolism and proliferation of beneficial bacteria in the body, thereby improving the host's health. This invention utilizes the gelling properties of pectin and adds oligosaccharides with prebiotic effects to the pectin emulsion gel system, which can further regulate the influence of the host's intestinal flora and its metabolites on the body's health.

[0027] (3) This invention uses waste fruit peels and residues as raw materials, which improves the utilization rate of fruit peels and residues and yields more nutritious components; the process of this invention is simple, environmentally friendly, and has a high utilization rate of raw materials. Attached Figure Description

[0028] Figure 1 This is a flowchart of the pectin gel preparation steps of the present invention;

[0029] Figure 2 This is a photograph of the citrus processing byproducts used in this invention.

[0030] Figure 3 This is a photograph of the pectin extraction process of this invention.

[0031] Figure 4 A photograph of the emulsion gel prepared according to the present invention;

[0032] Figure 5 Pectin gels prepared with different added sugars;

[0033] Figure 6 Pectin emulsion gels prepared with different added sugars;

[0034] Figure 7 Analysis of the water-holding capacity of various gels in this invention;

[0035] Figure 8 This is for the determination of gel interaction forces in this invention. Detailed Implementation

[0036] This invention provides a method for preparing oligosaccharide gum gel loaded with a fat-soluble active ingredient, comprising the following steps:

[0037] The pretreated fruit processing byproducts are mixed with hydrochloric acid solution to obtain a mixture. The mixture is stirred, cooled, and filtered to obtain a filtrate. The filtrate is then precipitated with alcohol and filtered to obtain pectin.

[0038] In specific embodiments of the present invention, the fruit processing byproducts include, but are not limited to, fruit peels and pulp after fruit processing, see below. Figure 2In a specific embodiment of the present invention, the pretreatment includes washing, cutting, drying, and pulverizing the fruit processing by-products. In a specific embodiment of the present invention, the fruit processing by-products are cut into 3-4 cm pieces. 3 The material is then dried. In a specific embodiment of the invention, an oven is preferably used for drying, and the drying temperature is preferably 40-50°C; the pulverization is preferably carried out using a high-speed blender, and the pulverization time is preferably 1-2 minutes.

[0039] In this invention, the mass ratio of the pretreated fruit processing by-product to the hydrochloric acid solution is preferably 1:10-30, more preferably 1:20. In this invention, a magnetic stirrer is preferably used for stirring, and the stirring conditions are preferably 70-80°C for 2-3 hours at a speed of 1000-1200 rpm. After stirring, the mixture is cooled and filtered through eight layers of gauze to remove the filter residue, obtaining the filtrate. In this invention, the volume ratio of the filtrate to ethanol is preferably 1:1-5, more preferably 1:3, and the alcohol precipitation time is preferably 12-24 hours. After precipitation, the filtrate is filtered through a 400-mesh filter bag to obtain pectin. Figure 3 In this invention, the ethanol is preferably 95% ethanol.

[0040] In this invention, the pectin obtained above is dried and then a pectin solution is prepared. 0.2–0.3 mg / mL of hesperidin is added, and the solution is dissolved by sonication. The pH is adjusted to 2–3.5, and gluconolactone and oligosaccharides are added. The solution is heated to 50–70°C and then cooled to solidify, obtaining a pectin gel. In this invention, the drying process is preferably carried out in an oven at 40–50°C to obtain dried pectin. In this invention, a pectin solution with a mass ratio of 1–2% is preferably prepared using distilled water. After adding 0.2–0.3 mg / mL of hesperidin, the solution is preferably sonicated at 40–60°C for 60–99 min to dissolve the hesperidin. More preferably, the sonication is performed at 45–55°C for 75–85 min. In this invention, a citrate buffer solution is preferably used to adjust the pH to 2–3.5. In this invention, a mass ratio of 1–2% of gluconolactone is preferably added.

[0041] In this invention, the oligosaccharides include stachyose or dextran. The amount of stachyose added is 60% to 70% by mass; the amount of dextran added is 30% to 40% by mass. In a specific embodiment of this invention, the amount of oligosaccharides added is as follows: the amount of stachyose added is 60% by mass of pectin, that is, 6g of stachyose is added to 4g of pectin solution; the amount of dextran added is 40% by mass, that is, 2.7g of sugar is added to 4g of pectin solution.

[0042] This invention also provides a method for preparing oligosaccharide gum gel loaded with a fat-soluble active ingredient, comprising the following steps:

[0043] The pretreated fruit processing byproducts are mixed with hydrochloric acid solution to obtain a mixture. The mixture is stirred, cooled, and filtered to obtain a filtrate. The filtrate is then precipitated with alcohol and filtered to obtain pectin.

[0044] In a specific embodiment of the present invention, the fruit processing by-products include, but are not limited to, fruit peels and pomace after fruit processing. In a specific embodiment of the present invention, the pretreatment includes washing, cutting, drying, and pulverizing the fruit processing by-products. In a specific embodiment of the present invention, the fruit processing by-products are cut into 3-4 cm pieces. 3 The material is then dried. In a specific embodiment of the invention, an oven is preferably used for drying, and the drying temperature is preferably 40-50°C; the pulverization is preferably carried out using a high-speed blender, and the pulverization time is preferably 1-2 minutes.

[0045] In this invention, the mass ratio of the pretreated fruit processing by-product to the hydrochloric acid solution is preferably 1:10-30, more preferably 1:20. In this invention, a magnetic stirrer is preferably used for stirring, and the stirring conditions are preferably 70-80°C for 2-3 hours at a speed of 1000-1200 rpm. After stirring, the mixture is cooled and filtered through eight layers of gauze to remove the filter residue, obtaining a filtrate. In this invention, the volume ratio of the filtrate to ethanol is preferably 1:1-5, more preferably 1:3, and the alcohol precipitation time is preferably 12-24 hours. After precipitation, the filtrate is filtered through a 400-mesh filter bag to obtain pectin. In this invention, the ethanol is preferably 95% concentration ethanol.

[0046] In this invention, the pectin is dried and then a pectin solution is prepared. The pectin solution is swollen and used as the aqueous phase. Medium-chain triglycerides and bergamot oil are mixed to obtain a mixed oil. 1-5 mg / mL of citronellol is weighed and added to the mixed oil and dissolved by ultrasonication to obtain the oil phase. The obtained aqueous and oil phases are mixed at a mass ratio of 6-15:1-3 and homogenized to obtain a pectin emulsion. (See...) Figure 4In this invention, the drying process is preferably carried out in an oven at a temperature of 40-50°C to obtain dried pectin. In this invention, a pectin solution with a mass ratio of 1-2% is preferably prepared using distilled water. The pectin solution is preferably placed in a refrigerator at 4°C for 1-2 days to swell and completely dissolve, and then used as the aqueous phase. In this invention, medium-chain triglycerides and bergamot oil are mixed at a mass ratio of 0.5-2:0.5-2, more preferably at a mass ratio of 1:1, to obtain a mixed oil. Noriheptacortin is added, and the mixture is preferably sonicated at 40-60°C for 60-99 minutes to dissolve the noriheptacortin, obtaining the oil phase. The obtained aqueous and oil phases are preferably mixed at a mass ratio of 9:1, and then homogenized using a T25 homogenizer at 9000-10000 rpm for 5-10 minutes, followed by homogenization using a high-pressure homogenizer at 500-700 bar, repeated 3-4 times to obtain a pectin emulsion. In this invention, the ultrasonic conditions are more preferably ultrasonic at 45-55°C for 75-85 minutes.

[0047] In this invention, the pH of the pectin emulsion is adjusted to 2-3.5, gluconolactone and oligosaccharides are added, and the mixture is heated to 50-70°C and then cooled to solidify, thus obtaining a pectin gel. In this invention, a citrate buffer solution is preferably used to adjust the pH to 2-3.5. In this invention, 1-2% by mass of gluconolactone is preferably added.

[0048] In this invention, the oligosaccharide includes stachyose or dextran. The amount of stachyose added is 60%–70%; the amount of dextran added is 30%–40%. In a specific embodiment of this invention, the amount of oligosaccharide added is as follows: the amount of stachyose added is 60% by mass of pectin, that is, 6g of stachyose is added to 4g of pectin solution; the amount of dextran added is 40% by mass, that is, 2.7g of sugar is added to 4g of pectin solution.

[0049] In this invention, a mixed oil is obtained by mixing medium-chain triglycerides and bergamot oil as a carrier for the fat-soluble component noriheptacortine. A pectin emulsion system is obtained in the form of oil in water, and the preparation of the pectin emulsion gel can further improve the bioavailability of the fat-soluble component.

[0050] The pectin gel preparation method provided by this invention includes two methods: first, after obtaining pectin, directly mixing the fat-soluble active ingredient with the pectin; or encapsulating the fat-soluble active ingredient with essential oil and then mixing it with pectin to obtain pectin loaded with the fat-soluble ingredient. The preparation process is as follows: Figure 1 The pectin gel does not contain a mixed oil loaded with fat-soluble active ingredients, while the pectin emulsion gel is prepared by adding oil containing fat-soluble active ingredients to pectin and then gelling the emulsion. Both gels are prepared under high-sugar, high-acid conditions. Furthermore, this invention, by adding oligosaccharides with prebiotic effects to the pectin gel system, can further regulate the influence of the host's gut microbiota and its metabolites on the body's health.

[0051] The technical solutions provided by the present invention will be described in detail below with reference to the embodiments, but they should not be construed as limiting the scope of protection of the present invention.

[0052] Unless otherwise specified, the following test methods and detection methods are all conventional methods; unless otherwise specified, the reagents and raw materials are all commercially available.

[0053] Example 1

[0054] A method for preparing citrus pectin gel includes the following steps:

[0055] (1) Sample preparation:

[0056] Use fresh citrus fruits as raw materials, wash them with clean water, drain them, and peel them;

[0057] (2) Preparation of pectin:

[0058] Wash and cut the citrus peel from step (1) into 4cm pieces. 3 The residue was dried in an oven at 50℃ and ground in a high-speed blender for 2 minutes to obtain a dry powder. 50g of the residue and 1000g of pH 2 HCl solution were placed in a 1L beaker, with a weight ratio of residue to hydrochloric acid solution of 1:20. A magnetic stirrer was set to stir at 80℃ for 2 hours at 1200 rpm. After stirring, the mixture was cooled and filtered through eight layers of gauze to remove the filter residue, yielding a filtrate. The volume ratio of the filtrate to ethanol was 1:3, and the alcohol precipitation time was 12 hours. After precipitation, the filtrate was filtered through a 400-mesh filter bag to obtain pectin, which was then dried in an oven at 50℃ to obtain dried citrus pectin.

[0059] (3) Preparation of pectin gel:

[0060] A 1% (w / v) citrus pectin solution was prepared with distilled water. 0.244 mg / mL of norepinephrine was added, and the solution was sonicated at 50°C for 99 min to dissolve the norepinephrine. After mixing evenly, the pH of the emulsion was adjusted to 2.8 with citric acid. 2% (w / v) dextran lactone and 60% (w / v) stachyose were added, and the solution was heated at 60°C for 5 min with constant stirring. The solution was then cooled at 4°C for 24 h to solidify, yielding citrus pectin gel.

[0061] Example 2

[0062] The difference from Example 1 is that 60% (w / v) stachyose is replaced with 40% (w / v) dextran, while the other steps remain the same.

[0063] Example 3

[0064] A method for preparing pear pectin gel includes the following steps:

[0065] (1) Sample preparation

[0066] Fresh snow pears are used as raw material; juice is extracted and filtered to obtain pear pulp.

[0067] (2) Preparation of pectin

[0068] The pear pomace from step (1) was dried in an oven at 50°C and ground in a blender for 2 minutes to obtain a dry powder. 50g of the pomace and 1000g of a pH 2 HCl solution were placed in a 1L beaker, with a weight ratio of pomace to hydrochloric acid solution of 1:20. A magnetic stirrer was set to stir at 80°C for 2 hours at a speed of 1200 rpm. After stirring, the mixture was cooled and filtered through eight layers of gauze to remove the filter residue, yielding a filtrate. The volume ratio of the filtrate to ethanol was 1:3, and the ethanol precipitation time was 12 hours. After precipitation, the filtrate was filtered through a 400-mesh filter bag to obtain pectin, which was then dried in an oven at 50°C to obtain dried pear pectin.

[0069] (3) Preparation of pectin gel

[0070] A 1% pear pectin solution was prepared with distilled water, and 0.244 mg / mL of tangeretin was added. The solution was sonicated at 50°C for 99 min to dissolve the tangeretin. After mixing evenly, the pH of the emulsion was adjusted to 2.8 with citric acid. 2% (w / v) dextran lactone and 60% (w / v) stachyose were added. The mixture was heated at 60°C for 5 min with constant stirring, and then cooled at 4°C for 24 h to solidify, thus obtaining pear pectin gel.

[0071] Example 4

[0072] The difference from Example 3 is that 60% (w / v) stachyose is replaced with 40% (w / v) dextran, while the other steps remain the same.

[0073] Example 5

[0074] A method for preparing a citrus pectin emulsion gel includes the following steps:

[0075] (1) Sample preparation

[0076] Use fresh citrus fruits as raw materials, wash them with clean water, drain them, and peel them;

[0077] (2) Preparation of pectin

[0078] Wash and cut the citrus peel from step (1) into 4cm pieces. 3The residue was dried in an oven at 50℃ and ground in a high-speed blender for 2 minutes to obtain a dry powder. 50g of the residue and 1000g of pH 2 HCl solution were placed in a 1L beaker, with a weight ratio of residue to hydrochloric acid solution of 1:20. A magnetic stirrer was set to stir at 80℃ for 2 hours at 1200 rpm. After stirring, the mixture was cooled and filtered through eight layers of gauze to remove the filter residue, yielding a filtrate. The volume ratio of the filtrate to ethanol was 1:3, and the alcohol precipitation time was 12 hours. After precipitation, the filtrate was filtered through a 400-mesh filter bag to obtain pectin, which was then dried in an oven at 50℃ to obtain dried citrus pectin.

[0079] (3) Emulsion preparation:

[0080] The pectin obtained in step (2) was prepared into a 1% pectin solution by mass. The solution was placed on a magnetic stirrer at 900 rpm and stirred for 1 day until completely dissolved, obtaining the pectin solution as the aqueous phase. Medium-chain triglycerides and bergamot oil were mixed at a mass ratio of 1:1, and 2 mg / mL of citronellol was added. The mixture was sonicated at 50°C for 99 min to dissolve the citronellol, obtaining the oil phase. The aqueous and oil phases were mixed at a mass ratio of 9:1 and homogenized at 10,000 rpm for 5 min using a T25 homogenizer. This homogenization was then repeated three times to obtain the pectin emulsion.

[0081] (4) Preparation of emulsion gel:

[0082] The pectin emulsion obtained in step (3) was adjusted to pH 2.8 with citric acid, and 2% (w / v) glucan lactone and 60% (w / v) stachyose were added. The mixture was heated at 60°C for 5 minutes with constant stirring, and then placed in a 4°C refrigerator to cool and solidify for 24 hours to obtain citrus pectin emulsion gel.

[0083] Example 6

[0084] The difference from Example 5 is that 60% (w / v) stachyose is replaced with 40% (w / v) dextran, while the other steps remain the same.

[0085] Example 7

[0086] A method for preparing a pear pectin emulsion gel includes the following steps:

[0087] (1) Sample preparation

[0088] Fresh snow pears are used as raw material; juice is extracted and filtered to obtain pear pulp.

[0089] (2) Preparation of pectin

[0090] The pear pomace from step (1) was dried in an oven at 50°C and ground in a blender for 2 minutes to obtain a dry powder. 50g of the pomace and 1000g of a pH 2 HCl solution were placed in a 1L beaker, with a weight ratio of pomace to hydrochloric acid solution of 1:20. A magnetic stirrer was set to stir at 80°C for 2 hours at a speed of 1200 rpm. After stirring, the mixture was cooled and filtered through eight layers of gauze to remove the filter residue, yielding a filtrate. The volume ratio of the filtrate to ethanol was 1:3, and the ethanol precipitation time was 12 hours. After precipitation, the filtrate was filtered through a 400-mesh filter bag to obtain pectin, which was then dried in an oven at 50°C to obtain dried pear pectin.

[0091] (3) Emulsion preparation:

[0092] The pectin obtained in step (2) was prepared into a 1% pectin solution by mass. The solution was placed on a magnetic stirrer at 900 rpm and stirred for 1 day until completely dissolved, obtaining the pectin solution as the aqueous phase. Medium-chain triglycerides and bergamot oil were mixed at a mass ratio of 1:1, and 2 mg / mL of citronellol was added. The mixture was sonicated at 50°C for 99 min to dissolve the citronellol, obtaining the oil phase. The aqueous and oil phases were mixed at a mass ratio of 9:1 and homogenized at 10,000 rpm for 5 min using a T25 homogenizer. This homogenization was then repeated three times to obtain the pectin emulsion.

[0093] (4) Preparation of emulsion gel:

[0094] The pectin emulsion obtained in step (3) was adjusted to pH 2.8 with citric acid, and 2% (w / v) dextran lactone and 60% (w / v) stachyose were added. The mixture was heated at 60°C for 5 minutes with constant stirring, and then placed in a 4°C refrigerator to cool and solidify for 24 hours to obtain pear pectin emulsion gel.

[0095] Example 8

[0096] The difference from Example 7 is that 60% (w / v) stachyose is replaced with 40% (w / v) dextran, while the other steps remain the same.

[0097] Comparative Example 1

[0098] The difference from Example 1 is that 60% (w / v) stachyose is replaced with 60% (w / v) sucrose, while the other steps remain the same.

[0099] Comparative Example 2

[0100] The difference from Example 3 is that 60% (w / v) stachyose is replaced with 60% (w / v) sucrose, while the other steps remain the same.

[0101] Comparative Example 3

[0102] The difference from Example 5 is that 60% (w / v) stachyose is replaced with 60% (w / v) sucrose, while the other steps remain the same.

[0103] Comparative Example 4

[0104] The difference from Example 7 is that 60% (w / v) stachyose is replaced with 60% (w / v) sucrose, while the other steps remain the same.

[0105] Example 9

[0106] Examples 1-8 and Comparative Examples 1-4 were named citrus pectin stachyose gel (CP-Sta), citrus pectin dextran gel (CP-Dex), pear pectin stachyose gel (PP-Sta), pear pectin dextran gel (PP-Dex), citrus pectin emulsion stachyose gel (CPE-Sta), citrus pectin emulsion dextran gel (CPE-Dex), pear pectin emulsion stachyose gel (PPE-Sta), pear pectin emulsion dextran gel (PPE-Dex), citrus pectin sucrose gel (CP-Suc), pear pectin sucrose gel (PP-Suc), citrus pectin emulsion sucrose gel (CPE-Suc), and pear pectin emulsion sucrose gel (PPE-Suc), respectively. Pectin gels and pectin emulsion gels prepared from citrus and pear pectin using different sugars (see...) Figure 5-6 The methods for determining physicochemical properties are as follows:

[0107] (1) The texture parameters of the gel were determined using a texture analyzer, and the strength of the obtained pectin gel was analyzed. The analyzer parameters are as follows: cylindrical extrusion probe TA / 36; front probe speed, 5.0 mm / s; measurement speed 1.0 mm / s; rear probe speed 5.0 mm / s; compression distance: 40%. The test results are shown in Table 1.

[0108]

[0109]

[0110] The textural results are shown in Table 1. Hardness reflects the gel strength and density of the gel network. There are significant differences in hardness between pectins prepared with different pectins and oligosaccharides. Among the three sugars, pear pectin gel and emulsion gel are harder than citrus pectin gel, and sucrose gel has the highest hardness compared to the other two oligosaccharides. The high hardness of pear pectin gel and emulsion gel may be due to the large molecular weight and high methoxy content of pear pectin, resulting in strong gelling force. For citrus pectin and emulsion gels, there is no significant difference in hardness between the two oligosaccharides; pear stachyose pectin gel is harder than pear emulsion gel. Overall, the hardness of pectin gel is greater than that of emulsion gel, possibly because heating during emulsion gel preparation causes emulsion demulsification, oil aggregation, and trapping within the gel network, thus reducing gel hardness.

[0111] Elasticity refers to the ability to return to its original shape after strain is removed. Compared to the three sugar gels of pear pectin and citrus pectin, pear pectin gel and emulsion gel have higher elasticity than citrus pectin gel and emulsion gel. Overall, pear dextran pectin gel and emulsion gel have the highest elasticity. Compared to the three sugar gels of citrus, stachyose has the lowest elasticity, while there is no significant difference between sucrose and dextran gels. Chewability refers to the energy required to chew solid food, while adhesiveness refers to the energy required for the sample to reach a stable state when broken or swallowed. The chewability and adhesiveness of the two pectin gels and emulsion gels show similar trends, with pear pectin and sucrose pectin gel and emulsion gel having the highest chewability and adhesiveness. The chewability and adhesiveness of the three citrus pectin gels and emulsion gels are all low and there is no significant difference. Compared to pear pectin gel and emulsion gel, citrus pectin gel and emulsion gel have lower hardness, elasticity, chewability, and adhesiveness, indicating a weaker gel system. Cohesion refers to the internal bonding strength of a sample, its ability to resist external damage and maintain its integrity. Among the three sugars, dextran gel exhibits the strongest cohesiveness, sucrose the weakest, and pear gel shows the strongest cohesiveness compared to citrus gel. Resilience indicates the degree to which a deformed sample recovers from deformation under the same speed and pressure conditions that caused the deformation. Citrus gel shows higher resilience than pear gel, while dextran gel exhibits the lowest resilience.

[0112] (2) The water-holding capacity of the gel was determined by centrifugation at 10,000 rpm for 15 minutes. After centrifugation, the water was removed, and the water-holding capacity was obtained based on the weight ratio before and after centrifugation. The test results are as follows: Figure 7 .

[0113] Water-holding results as follows Figure 7 The water-holding capacity indirectly reflects the density of the gel network. Among the three sugars, pear pectin gel has a higher water-holding capacity than citrus gel. However, for stachyose and dextran gels, the emulsion gel has a higher water-holding capacity than the pectin gel, and the dextran gel has a higher water-holding capacity than the stachyose gel. Therefore, among oligosaccharide gels, the dextran gel has a denser gel network.

[0114] (3) In the gel preparation process, oligosaccharides were added followed by urea, followed by heating and cooling to solidify pectin gel. The hardness was measured using a texture analyzer, and hydrogen bonds were determined. The test results are as follows: Figure 8 .

[0115] The result of the interaction forces is as follows Figure 8 Urea can break hydrogen bonds between polymers and molecules. It was found that the hardness of other gels, except for stachyose and dextran emulsion gels, tended to decrease after urea was added, indicating that the interaction force is hydrogen bonding.

[0116] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A method for preparing an oligosaccharide gum gel loaded with a fat-soluble active ingredient, characterized in that, Includes the following steps: The pretreated fruit processing byproducts are mixed with hydrochloric acid solution to obtain a mixture. The mixture is stirred, cooled, and filtered to obtain a filtrate. The filtrate is then precipitated with alcohol and filtered to obtain pectin. The pectin is dried and then a pectin solution is prepared. After swelling, 0.2-0.3 mg / mL of nobiletin is added to the pectin solution. After ultrasonic dissolution, the pH value is adjusted to 2-3.

5. Gluconolactone and oligosaccharides are added. After heating, the mixture is cooled and solidified to obtain pectin gel. The oligosaccharides are stachyose or glucan. The amount of stachyose added is 60%~70%; the amount of dextran added is 30%~40%.

2. A method for preparing an oligosaccharide gum gel loaded with a fat-soluble active ingredient, characterized in that, Includes the following steps: The pretreated fruit processing byproducts are mixed with hydrochloric acid solution to obtain a mixture. The mixture is stirred, cooled, and filtered to obtain a filtrate. The filtrate is then precipitated with alcohol and filtered to obtain pectin. The pectin is dried and then a pectin solution is prepared. The pectin solution is swollen and then used as the aqueous phase. Medium-chain triglycerides and bergamot oil were mixed to obtain a mixed oil. 1-5 mg / mL of noriheptacorlin was weighed and added to the mixed oil and dissolved by ultrasonication to obtain the oil phase. The aqueous phase and the oil phase were mixed at a mass ratio of 6-15:1-3 and homogenized to obtain a pectin emulsion. The pH of the pectin emulsion is adjusted to 2-3.5, gluconolactone and oligosaccharides are added, and after heating, the mixture is cooled and solidified to obtain pectin gel; the oligosaccharides are stachyose or glucan. The amount of stachyose added is 60%~70%; the amount of dextran added is 30%~40%. The mass ratio of the medium-chain triglycerides to bergamot oil is 0.5~2:0.5~2.

3. The method for preparing oligosaccharide gum gel according to claim 1 or 2, characterized in that, The stirring is carried out at 70~80℃ for 2~3 hours at a speed of 1000~1200 rpm.

4. The method for preparing oligosaccharide gum gel according to claim 1 or 2, characterized in that, The ultrasound conditions are 40~60℃ for 60~99 minutes.

5. The method for preparing oligosaccharide gum gel according to claim 1 or 2, characterized in that, The mass ratio of the pretreated fruit processing by-products to the hydrochloric acid solution is 1:10~30.

6. The method for preparing oligosaccharide gum gel according to claim 1 or 2, characterized in that, During alcohol precipitation, the volume ratio of the filtrate to ethanol is 1:1 to 5.

7. The method for preparing oligosaccharide gum gel according to claim 6, characterized in that, The alcohol precipitation time is 12-24 hours.

Citation Information

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