LU500957B1 - Method for preparing functional microcapsule from xanthan gum assisted porous starch - Google Patents
Method for preparing functional microcapsule from xanthan gum assisted porous starch Download PDFInfo
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
- A23L29/212—Starch; Modified starch; Starch derivatives, e.g. esters or ethers
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/269—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of microbial origin, e.g. xanthan or dextran
- A23L29/27—Xanthan not combined with other microbial gums
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
- A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5089—Processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
- A61J3/00—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms
- A61J3/07—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms into the form of capsules or similar small containers for oral use
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Polymers & Plastics (AREA)
- Animal Behavior & Ethology (AREA)
- Food Science & Technology (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Dispersion Chemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Organic Chemistry (AREA)
- Nutrition Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Preparation (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The present invention discloses a method for preparing a functional microcapsule from a xanthan gum assisted porous starch, including: S1, carrying out ultrasonic-enzymatic hydrolysis treatment on a rice starch, to obtain a porous starch; S2, suspending a certain quantity of solid xanthan gum in distilled water for homogenization for a period of time, then adding an enzymatically-hydrolyzed porous rice starch, and homogenizing same to form a uniform emulsion; and S3, adding quercetin into the emulsion, homogenizing a mixture, then moderately stirring the same for 12 h under dark conditions, and freeze drying all the mixture. According to the present invention, the xanthan gum in different proportions is used to prepare a porous starch-xanthan gum microcapsule wall material, so as to embed a functional component. Compared with a traditional porous starch, a loading capacity and an embedding rate of the porous starch microcapsule wall material prepared with the assistance of the xanthan gum are significantly increased, and stability of the functional component can be obviously improved.
Description
[0001] The present invention relates to a method, and in particular to a method for preparing a functional microcapsule from a xanthan gum assisted porous starch.
[0002] Being hollow, the porous starch (PS) particle can adsorb the target substance through the physical action, and store the target substance in micropores of the particle, thereby protecting and sustainedly releasing the target substance. Since the PS has a low cost, high availability, wide applicability, biodegradability, and biocompatibility, it is a highly popular wall material. Moreover, as a microcapsule wall material, the PS can reduce a cost of an encapsulated product.
[0003] The PS has been widely applied to embed the substances which are prone to be oxidized and decomposed in light, including vitamins, chlorogenic acid, cod liver oil, etc. However, the microcapsule with a single PS wall material generally has a low loading capacity, instability, etc. Currently, numerous studies have shown that the composite use of two or more wall materials is conducive to improvement in the loading capacity, the stability, etc. The xanthan gum (XG) is relatively long rigid anionic polysaccharide produced through microbial fermentation. It is also non-adsorptive polysaccharide with high apparent viscosity, a high shear thinning property, and a strong thickening capacity.
[0004] The present invention provides a method for preparing a functional microcapsule from a xanthan gum (XG) assisted porous starch (PS), so as to overcome the deficiencies in the art described above.
[0005] In order to solve the technical problems described above, the present invention 1 uses the following technical solution: a method for preparing a functional microcapsule from a XG assisted PS includes:
[0006] S1, carrying out ultrasonic-enzymatic pretreatment on a rice starch;
[0007] S2, suspending a certain quantity of solid XG in distilled water for homogenization for a period of time, then adding a porous rice starch subjected to ultrasonic-enzymatic treatment, and homogenizing same to form a uniform emulsion; and
[0008] S3, adding quercetin into the emulsion, homogenizing a mixture, then moderately stirring same for 12 h under dark conditions, freeze drying all the mixture, and grinding and sieving same to obtain the microcapsule embedded in a PS-XG composite wall material and containing the functional component.
[0009] Preferably, an ultrasonic-enzymatic process of preparing a PS in S1 includes: weighing a proper quantity of rice starch, adding same into a citric acid-sodium citrate buffer solution to prepare starch milk with a mass ratio concentration of 20-30%, ultrasonically treating same for 25 min at 450 W, and then adding 0.1 mL-0.2 mL of a-amylase and glucoamylase (the a-amylase: the glucoamylase = 1:5, v/v); magnetically stirring a mixture in a constant-temperature water bath for 12-16 h (at 150 rpm, 40°C), and adding NaOH to stop a reaction; and centrifugating and washing a mixture three times, then drying same to a constant weight, and sieving the same to obtain the PS.
[0010] Preferably, a process of preparing a XG assisted PS emulsion in S2 includes: suspending 0.1, 0.02, 0.01, 0.005, and 0.004 g of solid XG in the distilled water, and homogenizing same for 2 min at a speed of 16000 r/min; and then adding 1.0 g of PS, and homogenizing same to form the uniform emulsion (PS/XG).
[0011] Preferably, S3 includes: adding certain quantities of three active substances (2 mg/mL) into a paste separately, a ratio of the total solid amount to water being 11.1% (w/v), homogenizing a mixture, then moderately stirring same for 12 h under dark conditions, and using a sample without XG as a control group (CG); pouring different PS/XG or PS mixtures containing quercetin into flasks, and freeze drying same for 48 h; and taking out dried samples, grinding same, then placing the same in brown glass bottles, and storing same in a refrigerator (4°C) for analysis.
[0012] The present invention uses the XG in different proportions to prepare a PS-XG microcapsule wall material, so as to embed a functional component. In order to study influences from wall materials with different proportions on an embedding rate and a 2 loading capacity of the functional component, morphological characteristics are represented through a scanning electron microscope (SEM), and stability and an antioxidant capacity of the capsule are evaluated through differential scanning calorimetry (DSC) and a 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging capacity. Compared with a traditional PS, the loading capacity and the embedding rate of the PS microcapsule wall material prepared with the assistance of the XG are significantly increased, and stability of the functional component may be obviously improved.
[0013] Fig. 1 shows apparent structures of a porous starch (PS), a PS-quercetin microcapsule, and a PS/xanthan gum (XG)-quercetin microcapsule in the embodiments of the present invention separately.
[0014] Fig. 2 shows 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging rates of control group (CG)-Q, PS/XG (200:1)-Q, PS/XG (100:1)-Q, PS/XG (50:1)-Q, PS/XG (10:1)-Q, and quercetin standard solutions with different concentrations.
[0015] The present invention will be further described in detail below with reference to the particular implementations.
[0016] Embodiment 1:
[0017] A method for preparing a functional microcapsule from a xanthan gum (XG) assisted porous starch (PS) includes:
[0018] S1, an ultrasonic-enzymatic process of preparing a PS including: weigh a proper quantity of rice starch, add same into a citric acid-sodium citrate buffer solution to prepare starch milk with a mass ratio concentration of 20%, ultrasonically treat same for 25 min at 450 W, and then add 0.1 mL of a-amylase and glucoamylase (the a-amylase: the glucoamylase = 1:5, v/v). Magnetically stir a mixture in a constant-temperature water bath for 12 h (at 150 rpm, 40°C), and add NaOH to stop a reaction. Centrifugate and wash a mixture three times, then dry same to a constant weight, and sieve the same to obtain the PS.
[0019] S2, a process of preparing a XG assisted PS emulsion including: suspend 0.1 g 3 of solid XG in distilled water, and homogenize same for 2 min at a speed of 16000 r/min; and then add 1.0 g of PS, and homogenize same to form a uniform emulsion (PS/XG).
[0020] S3, add a certain quantity of quercetin (2 mg/mL) into a paste, a ratio of the total solid amount to water being 11.1% (w/v), homogenize a mixture, then moderately stir same for 12 h under dark conditions, and use a sample without XG as a control group (CG). Pour a PS/XG or PS mixture containing quercetin into a flask, and freeze dry same for 48 h. Take out a dried sample, grind same, then place the same in a brown glass bottle, and store same in a refrigerator (4°C) for analysis, named as PS/XG (10:1)-Q.
[0021] Embodiment 2:
[0022] A method for preparing a functional microcapsule from a XG assisted PS includes:
[0023] S1, an ultrasonic-enzymatic process of preparing a PS including: weigh a proper quantity of rice starch, add same into a citric acid-sodium citrate buffer solution to prepare starch milk with a mass ratio concentration of 25%, ultrasonically treat same for 25 min at 450 W, and then add 0.15 mL of a-amylase and glucoamylase (the a-amylase: the glucoamylase = 1:5, v/v). Magnetically stir a mixture in a constant-temperature water bath for 14 h (at 150 rpm, 40°C), and add NaOH to stop a reaction. Centrifugate and wash a mixture three times, then dry same to a constant weight, and sieve the same to obtain the PS.
[0024] S2, a process of preparing a XG assisted PS emulsion including: suspend 0.02 g of solid XG in distilled water, and homogenize same for 2 min at a speed of 16000 r/min; and then add 1 g of PS, and homogenize same to form a uniform emulsion (PS/XG).
[0025] S3, add a certain quantity of quercetin (2 mg/mL) into a paste, a ratio of the total solid amount to water being 11.1% (w/v), homogenize a mixture, then moderately stir same for 14 h under dark conditions, and use a sample without XG as a control group (CG). Pour a PS/XG or PS mixture containing quercetin into a flask, and freeze dry same for 48 h. Take out a dried sample, grind same, then place the same in a brown glass bottle, and store same in a refrigerator (4°C) for analysis, named as PS/XG (50:1)-Q.
[0026] Embodiment 3:
[0027] A method for preparing a functional microcapsule from a XG assisted porous starch PS includes:
[0028] S1, an ultrasonic-enzymatic process of preparing a PS including: weigh a proper 4 quantity of rice starch, add same into a citric acid-sodium citrate buffer solution to prepare starch milk with a mass ratio concentration of 25%, ultrasonically treat same for 25 min at 450 W, and then add 0.15 mL of a-amylase and glucoamylase (the a-amylase: the glucoamylase = 1:5, v/v). Magnetically stir a mixture in a constant-temperature water bath for 14 h (at 150 rpm, 40°C), and add NaOH to stop a reaction. Centrifugate and wash a mixture three times, then dry same to a constant weight, and sieve the same to obtain the PS.
[0029] S2, a process of preparing a XG assisted PS emulsion including: suspend 0.01 g of solid XG in distilled water, and homogenize same for 2 min at a speed of 16000 r/min; and then add 1 g of PS, and homogenize same to form a uniform emulsion (PS/XG).
[0030] S3, add a certain quantity of quercetin (2 mg/mL) into a paste, a ratio of the total solid amount to water being 11.1% (w/v), homogenize a mixture, and then moderately stir same for 12 h under dark conditions. Pour a PS/XG or PS mixture containing quercetin into a flask, and freeze dry same for 48 h. Take out a dried sample, grind same, then place the same in a brown glass bottle, and store same in a refrigerator (4°C) for analysis, named as PS/XG (100:1)-Q.
[0031] Embodiment 4
[0032] A method for preparing a functional microcapsule from a XG assisted PS includes:
[0033] S1, an ultrasonic-enzymatic process of preparing a PS including: weigh a proper quantity of rice starch, add same into a citric acid-sodium citrate buffer solution to prepare starch milk with a mass ratio concentration of 30%, ultrasonically treat same for 25 min at 450 W, and then add 0.15 mL of a-amylase and glucoamylase (the o-amylase: the glucoamylase = 1:4, v/v). Magnetically stir a mixture in a constant-temperature water bath for 12 h (at 150 rpm, 40°C), and add NaOH to stop a reaction. Centrifugate and wash a mixture three times, then dry same to a constant weight, and sieve the same to obtain the PS.
[0034] S2, a process of preparing a XG assisted PS emulsion including: suspend 0.005 g of solid XG in distilled water, and homogenize same for 2 min at a speed of 16000 r/min; and then add 0.6 g of PS, and homogenize same to form a uniform emulsion (PS/XG).
[0035] S3, add a certain quantity of quercetin (0.5 mg/mL) into a paste, a ratio of the total solid amount to water being 11.1% (w/v), homogenize a mixture, and then moderately stir same for 12 h under dark conditions. Pour a PS/XG or PS mixture containing quercetin into a flask, and freeze dry same for 48 h. Take out a dried sample, grind same, then place the same in a brown glass bottle, and store same in a refrigerator (4°C) for analysis, named as PS/XG (200:1)-Q.
[0036] Control group:
[0037] The sample without XG 1s used as the CG and a PS wall material containing quercetin is named as CG-Q.
[0038] An embedding property of the prepared PS/XG composite wall material described above is analyzed:
[0039] 1. an influence from an addition amount of the XG on a loading capacity and an embedding rate of the microcapsule
[0040] Table 1 Loading capacity and embedding rate of PS/XG/-quercetin microcapsule Quercetin Sample _— mm —”—-— Loading capacity (ug/mg) Embedding rate (%) PS/XG-Q (10:1) 1.89+0.042 94.93+1.972 PS/XG-Q (50:1) 1.87+0.022 93.36+0.84° PS/XG-Q (100:1) 1.850.038 92.74+1.508 PS/XG-Q (200:1) 1.820.068 91.19+2.96° CG-Q 1.53+0.06b 76.74+3.13P
[0041] Note: different letters at the ends of the same column of data denote significant differences (p<0.05)
[0042] As shown in Table 1, the loading capacity of the microcapsule added with the XG 1s 1.20-1.35 times that of a microcapsule without XG and a loading capacity of a functional component 1s increased slightly with increase of a proportion of the XG The embedding rate may be increased significantly with addition of the XG but no significant difference is caused with the addition of the XG (p>0.05).
[0043] 2. An influence from the addition amount of the XG on thermostability of the microcapsule
[0044] Table 2 Thermostability of PS/XG/-quercetin microcapsule (differential scanning calorimetry, DSC) sme | —— Queen 6
PS/XG-Q (10:1) 65.65+0.37¢ 69.05+0.80" PS/XG-Q (50:1) 63.73+0.45° 67.94+0.46" PS/XG-Q (100:1) 61.25+0.90° 66.32+0.65" PS/XG-Q (200:1) 61.39+0.47e 66.49+0.17" CG-Q 59.45+0.27° 64.54+0,29h Q 313.04+1.297 319.66+0.42i
[0045] Note: different letters at the ends of the same column of data denote significant differences (p<0.05)
[0046] As can be seen from the table, a sharp endothermic peak of a melting point, obtained through scanning of the DSC, of the quercetin is 319.66°C. When the quercetin is embedded, results show that their endothermic peaks are eliminated, and only a peak value of an endothermic peak of one which is not significantly different from the wall material is found, which indicates that an inclusion compound is formed between the functional component and the wall material, instead of a simple physical mixture, or being deemed as an indication of non-crystallization of the functional component.
[0047] 3. An influence from the addition amount of the XG on an antioxidant capacity of the microcapsule
[0048] As can be seen from Fig. 2, the microcapsule added with the XG has a higher radical scavenging rate, and the radical scavenging rate is increased with increase of the addition amount of the XG 2,2-diphenyl-1-picrylhydrazyl (DPPH) scavenging capacities of the quercetin (0.01 mg/mL), PS/XG-Q microcapsules, and CG-Q are 8.58%, 10.97%,
10.71%, 10.64%, and 10.31% (PS/XG=10:1, 50:1, 100:1, 200:1), and 8.58%, respectively. Radical scavenging rates of a 1 mg/mL raw quercetin solution and a 2 mg/mL raw quercetin solution are 41.84% and 81.39%, respectively. Results also show that the quercetin has an extremely high radical scavenging capacity, owing to a resonance stabilization semi-quinone radical structure, which is formed after the quercetin reacts with a radical through a phenolic hydroxyl group, thus stopping a chain reaction. In addition, antioxidant activity of a PS/XG-Q particle is slightly higher than that of raw quercetin with a concentration of 0.01 mg/mL. This also shows that antioxidant activity of the PS/XG-Q microcapsule and a CG-Q microcapsule is closely related to a loading capacity of the quercetin.
[0049] The implementations described above are not intended to limit the present 7 invention, and the present invention is not merely limited to the examples described above.
The variations, modifications, additions or substitutions which are made by those skilled in the art within the scope of the technical solution of the present invention all fall within the scope of protection of the present invention. 8
Claims (3)
1. A method for preparing a functional microcapsule from a xanthan gum (XG) assisted porous starch (PS), comprising: S1, carrying out ultrasonic-enzymatic pretreatment on a rice starch; S2: suspending solid XG in distilled water for homogenization, then adding a porous rice starch subjected to ultrasonic-enzymatic treatment, and homogenizing same to form a uniform emulsion; and S3, adding a functional component into the emulsion, homogenizing a mixture, then moderately stirring same for 12 h under dark conditions, freeze drying all the mixture, and grinding and sieving same to obtain the microcapsule embedded in a PS-XG composite wall material and containing the functional component.
2. The method according to claim 1, wherein an ultrasonic-enzymatic process of preparing a PS in S1 comprises: weighing a proper quantity of rice starch, adding same into a citric acid-sodium citrate buffer solution to prepare starch milk with a mass ratio concentration of 20-30%, ultrasonically treating same for 25 min at 450 W, and then adding
0.1 mL-0.2 mL of a-amylase and glucoamylase (the a-amylase: the glucoamylase = 1:5, v/v); magnetically stirring a mixture in a constant-temperature water bath for 12-16 h (at 150 rpm, 40°C), and adding NaOH to stop a reaction; and centrifugating and washing a mixture three times, then drying same to a constant weight, and sieving the same to obtain the PS.
3. The method according to claim 1, wherein a process of preparing a XG assisted PS emulsion in S2 comprises: suspending 0.004-0.1 g of solid XG in the distilled water, and homogenizing same for 2 min at a speed of 16000 r/min; and then adding 1.0 g of PS, and homogenizing same to form the uniform emulsion (PS/XG).
9
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