Method for preparing pectin composite fiber microsphere powder based on high-voltage pulse combined fluidized bed process and product thereof

Abstract

The invention provides a method for preparing pectin composite fiber microsphere powder based on a high-voltage pulse combined fluidized bed process and a product thereof, and relates to the technical field of fluidized bed spray drying. The method comprises the following steps: carrying out superfine grinding on composite fibers to obtain composite fiber powder; wherein the composite fibers comprise low-fat pectin, oat fibers, flaxseed fibers and guar fibers; dispersing and homogenizing the composite fiber powder and water at a high speed to obtain a suspension; and performing high-voltage pulse treatment on the suspension, and spraying the treated suspension on the surface of a carrier through a fluidized bed spray drying process to obtain the pectin composite fiber microsphere powder. According to the method, molecular chains of the pectin-containing composite fiber powder can be punctured through high-voltage pulse current, so that branched chains of the pectin-containing composite fiber powder are promoted to be opened, and the contact probability between the molecular chains is conveniently increased; through a fluidized bed spray drying process, the solubility and the dissolution rate of the composite fiber microsphere powder are improved, and the caking phenomenon is reduced.

Description

Technical Field

[0001] The invention relates to the technical field of fluidized bed spray drying, and in particular to a method for preparing pectin composite fiber microsphere powder based on a high-voltage pulse combined with a fluidized bed process and a product thereof. Background Art

[0002] Pectin is a natural linear macromolecular heteropolysaccharide with a complex structure widely distributed in plants in nature. According to the proportion of methyl ester groups in pectin molecules, pectin can be divided into high-ester pectin (esterification degree higher than 50%) and low-ester pectin (esterification degree lower than 50%). High-ester pectin usually forms gel under high sugar and high acid conditions, while low-ester pectin needs to add divalent metal ions (usually calcium ions) under low sugar conditions to form an "egg box" model with free carboxyl groups after deesterification to form a mesh gel structure. In this egg box model, the galacturonic acid sequence involved in the gel adopts a double-folded "Z" configuration, and the calcium ions and carboxyl groups are integrated on the inner side of the two pectin chains and further spirally aggregate to form a gel.

[0003] CN102553499A discloses a method for preparing microcapsules based on gelation of low-ester pectin and calcium ions and its application, the steps of which are as follows: (1) preparing a low-ester pectin solution: using 1 / 4 of the amount of water used in the entire preparation process to prepare a low-ester pectin solution containing 2-12% by mass; (2) preparing a CaCl2 solution: using 3 / 4 of the amount of water used in the entire preparation process to prepare a CaCl2 solution containing 0.01-0.08% by mass; (3) preparing a low-ester pectin-calcium ion solution: while stirring the low-ester pectin solution, slowly adding the CaCl2 solution thereto, and continuing to stir to form a low-ester pectin-calcium ion solution; (4) mixing with a core material: adding the core material to the low-ester pectin-calcium ion solution while stirring, and continuing to stir until the mixture is in a uniform state; (5) drying and gelling to form particles: spray drying the low-ester pectin-calcium ion-core material mixture, and the low-ester pectin and calcium ions are gelled as the water evaporates to form a microcapsule product with an organic combination of wall material components.

[0004] CN119215799A discloses a method for preparing controllably dissolvable microspheres based on sodium alginate and pectin, comprising: obtaining a sodium alginate solution and a pectin solution, mixing the sodium alginate solution and the pectin solution based on a first preset ratio, and using a preset stirring device to stir and mix them uniformly to obtain a mixed gel solution, mixing a pre-constructed calcium chloride aqueous solution and anhydrous ethanol based on a second preset ratio, and stirring and mixing them uniformly by a stirring device to obtain a crosslinker solution, dripping the mixed gel solution into the crosslinker solution by a preset dripping method, and obtaining mixed gel beads in the crosslinker solution, and washing the mixed microgel beads to obtain controllably dissolvable microspheres.

[0005] CN113893791A discloses a method for preparing betanin-Physalis chinensis pectin gel, the method comprising: (1) extracting Physalis chinensis seed pectin, dissolving it in distilled water, stirring overnight at 40-60°C to form 1-5% pectin solutions; (2) adding 1-3% betanin to the pectin solution, stirring at room temperature for 10-20 minutes to form a betanin-Physalis chinensis seed pectin complex; (3) placing the betanin-Physalis chinensis seed pectin complex at 4°C for 10-15 hours to form a gel, and storing it at room temperature; wherein, in step (2), after adding betanin, a calcium chloride solution is added and the pH value is adjusted, wherein the concentration of the calcium chloride solution is 1.0 g / L; and the pH value is adjusted to 4.

[0006] As mentioned above, the low-fat pectin in the above patents needs to be in a calcium ion environment to form a gel. In addition, when ordinary pectin first contacts water, it is very easy to undergo hydration, that is, water can only penetrate the surface of the pectin powder to a limited extent, locally transforming the glassy area into a rubbery state, and then expanding to form a sticky surface gel, which will cause the pectin powder to adhere to each other and form lumps. The lumps can only be broken under a high shear rate. Under normal circumstances, the dissolution of pectin requires mixing with three times the amount of diluent such as sucrose and then adding it to water.

[0007] Therefore, it is urgent to develop a product that can be directly dissolved in water and quickly form a gel in gastric acid without other conditions such as low sugar or divalent metal ions to meet diverse food needs.

[0008] In view of this, the present invention is proposed. Summary of the invention

[0009] One of the purposes of the present invention is to provide a method for preparing pectin composite fiber microsphere powder based on high-voltage pulse combined with fluidized bed process. The present invention can pierce the molecular chain of the composite fiber powder containing pectin through high-voltage pulse current, prompting its branch chain to open, thereby increasing the contact probability between molecular chains; through the fluidized bed spray drying process, the solubility and dissolution rate of the composite fiber microsphere powder are improved, and the agglomeration phenomenon is reduced.

[0010] The second object of the present invention is to provide a pectin composite fiber microsphere powder, which is prepared by the above-mentioned preparation method. After being dissolved in water again, the pectin composite fiber microsphere powder can quickly form a gel by self-assembly in an acidic environment, especially under gastric acid conditions, without the need for calcium ions as bridge points for gel formation.

[0011] The third object of the present invention is to provide a pectin composite fiber gel, which is prepared by combining the above-mentioned pectin composite fiber microsphere powder and gastric acid.

[0012] The fourth object of the present invention is to provide a method for preparing a pectin composite fiber gel, the preparation method comprising: dissolving the pectin composite fiber microsphere powder in water to obtain a microsphere powder solution; mixing the microsphere powder solution with simulated gastric fluid to form the composite fiber gel.

[0013] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are particularly adopted: In a first aspect, the present invention provides a method for preparing pectin composite fiber microsphere powder based on a high-voltage pulse combined with a fluidized bed process, the method comprising the following steps: The composite fiber is ultrafinely ground to obtain composite fiber powder; wherein the composite fiber includes low-fat pectin, oat fiber, flaxseed fiber and guar fiber; the ultrafine grinding pressure is 2-6 MPa, and the air flow velocity is 200-285 m / s; The composite fiber powder and water are dispersed and homogenized at high speed to obtain a suspension; wherein the rotation speed of the high-speed dispersion and homogenization is 15000-25000 r / min; The suspension is subjected to high-voltage pulse treatment, and then the treated suspension is sprayed on the surface of the carrier through a fluidized bed spray drying process to obtain pectin composite fiber microsphere powder; wherein the process parameters of the high-voltage pulse treatment include: a pulse frequency of 1-2 kHz, a pulse width of 10-50 μs, a flow rate of 10-20 L / h, an electric field strength of 10-50 kV / cm, and a pulse treatment time of 100-500 μs; the process parameters of the fluidized bed spray drying process include: a spray mode of top spraying, an air inlet temperature of 80-100°C, a material temperature of 55-75°C, a fan frequency of 20-50 Hz, an atomization pressure of 0.1-0.3 Mpa, and a liquid feed flow rate of the suspension of 20-80 g / min.

[0014] Preferably, the composite fiber comprises the following components by mass percentage: 50-70% low-fat pectin, 5-20% oat fiber, 5-20% flaxseed fiber and 5-20% guar bean fiber.

[0015] Preferably, the degree of esterification of the low-fat pectin is 20-40%.

[0016] Preferably, the molecular weight of the low-fat pectin is 10,000-20,000 g / mol.

[0017] Preferably, the ultrafine grinding is carried out in an airflow ultrafine grinding machine.

[0018] Preferably, the ultrafine grinding time is 1 to 3 hours.

[0019] Preferably, the particle size of the composite fiber powder is 10-50 μm.

[0020] Preferably, the mass ratio of the composite fiber powder to water is 1:(10-20).

[0021] Preferably, the process parameters of the high-speed dispersion and homogenization include: a single homogenization time of 30 s to 2 min, a homogenization number of 1 to 5 times, and an interval time of 10 to 40 s.

[0022] Preferably, the carrier comprises resistant dextrin.

[0023] Preferably, the mass ratio of the carrier to the suspension is (3-4):1.

[0024] In a second aspect, the present invention provides a pectin composite fiber microsphere powder, which is prepared by the method for preparing pectin composite fiber microsphere powder based on high-voltage pulse combined with fluidized bed process as described in the first aspect.

[0025] In a third aspect, the present invention provides a pectin composite fiber gel, wherein the pectin composite fiber gel is prepared by combining the pectin composite fiber microsphere powder as described in the second aspect and gastric acid.

[0026] In a fourth aspect, the present invention provides a method for preparing the pectin composite fiber gel according to the third aspect, the preparation method comprising: Dissolving the pectin composite fiber microsphere powder in water to obtain a microsphere powder solution; The microsphere powder solution and simulated gastric fluid are mixed to form the composite fiber gel.

[0027] Preferably, the mass ratio of the pectin composite fiber microsphere powder to water is 1:(100-200).

[0028] Preferably, the mass ratio of the pectin composite fiber microsphere powder to the simulated gastric fluid is 1:(40-60).

[0029] Preferably, the time for forming the composite fiber gel is ≤60 s.

[0030] Preferably, the composite fiber gel is formed at a multiple of ≥90 times.

[0031] Compared with the prior art, the present invention has the following beneficial effects: (1) The high-voltage pulse current formed by the pulse electric field in the present invention can pierce the molecular chains of pectin and composite fibers, causing their branches to open, thereby increasing the contact probability between the molecular chains. After being dissolved in water again, it can quickly form a gel through self-assembly under gastric acid conditions, without the need for calcium ions as bridge points for gel formation.

[0032] (2) In the present invention, the pectin composite fiber microsphere powder is prepared by fluidized bed spray drying. The powder is spherical, has a small contact area with each other, can be quickly dissolved in water, reduces agglomeration, and improves application efficiency.

[0033] (3) The pectin composite fiber microsphere powder prepared by high-pressure pulse combined with fluidized bed technology in the present invention dissolves in water and quickly forms a gel when encountering gastric acid in the stomach, while wrapping carbohydrates such as starch and delaying the latter's absorption, thereby reducing the rapid increase in blood sugar after a meal. DETAILED DESCRIPTION

[0034] Unless otherwise defined herein, scientific and technical terms used in conjunction with the present invention shall have the meanings commonly understood by those of ordinary skill in the art. The meaning and scope of the terms should be clear, however, in the case of any potential ambiguity, the definitions provided herein take precedence over any dictionary or external definitions. In this application, unless otherwise stated, the use of "or" means "and / or". In addition, the use of the term "including" and other forms is non-limiting.

[0035] It should be noted that specific details are described in the following description to facilitate a full understanding of the present invention. However, the present invention can be implemented in a variety of other ways different from those described herein, and those skilled in the art can make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0036] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0037] In a first aspect, the present invention provides a method for preparing pectin composite fiber microsphere powder based on a high-voltage pulse combined with a fluidized bed process, the method comprising the following steps: The composite fiber is ultra-finely ground to obtain composite fiber powder; wherein the composite fiber comprises low-fat pectin, oat fiber, flax seed fiber and guar bean fiber; The composite fiber powder and water are dispersed and homogenized at high speed to obtain a suspension; The suspension is subjected to high-pressure pulse treatment, and then the treated suspension is sprayed on the surface of the carrier through a fluidized bed spray drying process to obtain pectin composite fiber microsphere powder.

[0038] In the present invention, pectin is selected and mixed with oat fiber, flax seed fiber and guar bean fiber and then ultrafinely ground. Then, the mixture is placed in a high-speed homogenizer, purified water is added, stirred and dissolved to form a suspension, and then the molecular branches of the four fibers (glue) are broken open by high-voltage pulse electric field technology. After spray drying, pectin composite fiber powder is formed.

[0039] Among them, the high-voltage pulse current formed by the pulse electric field in the present invention can pierce the molecular chains of pectin and composite fibers, prompting the branch chains to open, so as to increase the contact probability between the molecular chains. After being redissolved, under acidic conditions, especially under gastric acid conditions, the positive and negative groups in the pectin composite fibers are self-assembled and entangled to form a mesh structure, quickly forming a gel, replacing the egg-box structure formed by low-fat pectin gel and calcium ions, and no calcium ions are needed as bridge points for gel formation.

[0040] Among them, the pectin composite fiber microsphere powder is prepared by fluidized bed spray drying in the present invention. The powder is spherical, has a small contact area with each other, can be quickly dissolved in water, reduces agglomeration, and improves application efficiency.

[0041] As an optional embodiment, the composite fiber comprises the following components by mass percentage: 50-70% low-fat pectin, 5-20% oat fiber, 5-20% flaxseed fiber and 5-20% guar bean fiber.

[0042] As an optional embodiment, based on the total mass of the composite fiber as 100%, the content of low-fat pectin is 50-70%, for example, it can be 50%, 52%, 54%, 55%, 56%, 58%, 60%, 62%, 64%, 65%, 66%, 68%, 70%, etc.

[0043] As an optional embodiment, based on the total mass of the composite fiber as 100%, the content of oat fiber is 5-20%, for example, it can be 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, etc.

[0044] As an optional embodiment, based on the total mass of the composite fiber as 100%, the content of flaxseed fiber is 5-20%, for example, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, etc.

[0045] As an optional embodiment, based on the total mass of the composite fiber as 100%, the content of guar bean fiber is 5-20%, for example, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, etc.

[0046] As an optional embodiment, the degree of esterification of the low-fat pectin is 20-40%, for example, it can be 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, etc.

[0047] As an optional embodiment, the molecular weight of the low-fat pectin is 10,000-20,000 g / mol, for example, 10,000 g / mol, 12,000 g / mol, 14,000 g / mol, 15,000 g / mol, 16,000 g / mol, 18,000 g / mol, 20,000 g / mol, etc.

[0048] As an optional embodiment, the ultrafine grinding is carried out in an airflow ultrafine grinding machine.

[0049] As an optional embodiment, the process parameters of the ultrafine grinding include: a grinding pressure of 2-6 MPa, an air flow velocity of 200-285 m / s, and a grinding time of 1-3 h.

[0050] As an optional embodiment, the crushing pressure is 2~6 MPa, for example, it can be 2 MPa, 2.5 MPa, 3 MPa, 3.5 MPa, 4 MPa, 4.5 MPa, 5 MPa, 5.5 MPa, 6 MPa, etc.

[0051] As an optional embodiment, the air flow velocity is 200~285 m / s, for example, it can be 200 m / s, 210 m / s, 220 m / s, 230 m / s, 240 m / s, 250 m / s, 260 m / s, 280 m / s, 285 m / s, etc.

[0052] As an optional embodiment, the crushing time is 1 to 3 h, for example, it can be 1 h, 1.2 h, 1.4 h, 1.5 h, 1.6 h, 1.8 h, 2 h, 2.2 h, 2.4 h, 2.5 h, 2.6 h, 2.8 h, 3 h, etc.

[0053] As an optional embodiment, the particle size of the composite fiber powder is 10~50 μm, for example, it can be 10 μm, 12 μm, 14 μm, 16 μm, 18 μm, 20 μm, 22 μm, 24 μm, 26 μm, 28 μm, 30 μm, 32 μm, 34 μm, 36 μm, 38 μm, 40 μm, 42 μm, 44 μm, 46 μm, 48 μm, 50 μm, etc.

[0054] As an optional embodiment, the mass ratio of the composite fiber powder to water is 1:(10-20), for example, it can be 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, 1:16, 1:17, 1:18, 1:19, 1:20, etc.

[0055] As an optional embodiment, the water includes purified water.

[0056] As an optional implementation, the process parameters of the high-speed dispersion and homogenization include: a homogenization speed of 15000-25000 r / min, a homogenization time of 30 s-2 min, a homogenization number of 1-5 times, and an interval time of 10-40 s.

[0057] As an optional embodiment, the rotation speed of the high-speed dispersion and homogenization is 15000~25000 r / min, for example, it can be 15000 r / min, 16000 r / min, 17000 r / min, 18000 r / min, 19000 r / min, 20000 r / min, 21000 r / min, 22000 r / min, 23000 r / min, 24000 r / min, 25000 r / min, etc.

[0058] As an optional implementation, the homogenization time is 30 s to 2 min, for example, it can be 30 s, 40 s, 50 s, 1 min, 1.2 min, 1.4 min, 1.6 min, 1.8 min, 2 min, etc.

[0059] As an optional implementation, the homogenization times are 1 to 5 times, for example, 1 time, 2 times, 3 times, 4 times, or 5 times.

[0060] As an optional implementation, the interval time is 10-40 s, for example, it can be 10 s, 15 s, 20 s, 25 s, 30 s, 35 s, 40 s, etc.

[0061] As an optional embodiment, the process parameters of the high voltage pulse treatment include: The pulse frequency is 1~2 kHz, the pulse width is 10~50 μs, the flow rate is 10~20 L / h, the electric field strength is 10~50 kV / cm, and the pulse treatment time is 100~500 μs.

[0062] As an optional implementation, the pulse frequency is 1-2 kHz, for example, it can be 1 kHz, 1.2 kHz, 1.4 kHz, 1.5 kHz, 1.6 kHz, 1.8 kHz, 2 kHz, etc.

[0063] As an optional implementation, the pulse width is 10~50 μs, for example, it can be 10 μs, 12 μs, 14 μs, 15 μs, 16 μs, 18 μs, 20 μs, 22 μs, 24 μs, 26 μs, 28 μs, 30 μs, 32 μs, 34 μs, 35 μs, 36 μs, 38 μs, 40 μs, 42 μs, 44 μs, 45 μs, 46 μs, 48 ​​μs, 50 μs, etc.

[0064] As an optional embodiment, the flow rate is 10-20 L / h, for example, it can be 10 L / h, 11 L / h, 12 L / h, 13 L / h, 14 L / h, 15 L / h, 16 L / h, 17 L / h, 18 L / h, 19 L / h, 20 L / h, etc.

[0065] As an optional embodiment, the electric field strength is 10~50 kV / cm, for example, it can be 10 kV / cm, 12 kV / cm, 14 kV / cm, 16 kV / cm, 18 kV / cm, 20 kV / cm, 22 kV / cm, 24 kV / cm, 26 kV / cm, 28 kV / cm, 30 kV / cm, 32 kV / cm, 34 kV / cm, 36 kV / cm, 38 kV / cm, 40 kV / cm, 42 kV / cm, 44 kV / cm, 46 kV / cm, 48 kV / cm, 50 kV / cm, etc.

[0066] As an optional embodiment, the pulse processing time is 100~500 μs, for example, it can be 100 μs, 120 μs, 140 μs, 160 μs, 180 μs, 200 μs, 220 μs, 240 μs, 260 μs, 280 μs, 300 μs, 320 μs, 340 μs, 360 μs, 380 μs, 400 μs, 420 μs, 440 μs, 460 μs, 480 μs, 500 μs, etc.

[0067] As an optional embodiment, the process parameters of the fluidized bed spray drying process include: The spraying method is top spraying, the inlet air temperature is 80~100℃, the material temperature is 55~75℃, the fan frequency is 20~50Hz, the atomization pressure is 0.1~0.3 Mpa, and the liquid inlet flow rate of the suspension is 20~80 g / min.

[0068] As an optional implementation, the spraying method is top spraying.

[0069] As an optional embodiment, the inlet air temperature is 80~100℃, for example, it can be 80℃, 82℃, 84℃, 85℃, 86℃, 88℃, 90℃, 92℃, 94℃, 96℃, 98℃, 100℃, etc.

[0070] As an optional embodiment, the material temperature is 55-75°C, for example, it can be 55°C, 56°C, 58°C, 60°C, 62°C, 64°C, 66°C, 68°C, 70°C, 72°C, 74°C, 75°C, etc.

[0071] As an optional embodiment, the fan frequency is 20~50 Hz, for example, it can be 20 Hz, 22 Hz, 24 Hz, 25 Hz, 26 Hz, 28 Hz, 30 Hz, 32 Hz, 34 Hz, 35 Hz, 36 Hz, 38 Hz, 40 Hz, 42 Hz, 44 Hz, 45Hz, 46 Hz, 48 Hz, 50 Hz, etc.

[0072] As an optional embodiment, the atomization pressure is 0.1~0.3 Mpa, for example, it can be 0.1 Mpa, 0.12 Mpa, 0.14 Mpa, 0.15 Mpa, 0.16 Mpa, 0.18 Mpa, 0.2 Mpa, 0.22 Mpa, 0.24 Mpa, 0.25 Mpa, 0.26 Mpa, 0.28 Mpa, 0.3 Mpa, etc.

[0073] As an optional embodiment, the liquid feed flow rate of the suspension is 20-80 g / min, for example, it can be 20 g / min, 25 g / min, 30 g / min, 35 g / min, 40 g / min, 45 g / min, 50 g / min, 55 g / min, 60 g / min, 65 g / min, 70 g / min, 75 g / min, 80 g / min, etc.

[0074] As an optional embodiment, the carrier comprises resistant dextrin.

[0075] In the present invention, resistant dextrin with good water solubility is used as a carrier, and pectin composite fiber microsphere powder is prepared by fluidized bed spray drying. The powder is spherical, and the contact area between each other is small, which further improves the dissolution rate and solubility in water, effectively avoids agglomeration, and more significantly improves the application efficiency. In addition, resistant dextrin is a low-molecular water-soluble dietary fiber, has the effect of resisting digestive enzymes, can accelerate gastrointestinal motility, can maintain the stability of blood sugar after meals, and can also help improve blood sugar levels in daily life.

[0076] As an optional embodiment, the mass ratio of the carrier to the suspension is (3~4):1, for example, it can be 3:1, 3.1:1, 3.2:1, 3.3:1, 3.4:1, 3.5:1, 3.6:1, 3.7:1, 3.8:1, 3.9:1, 4:1, etc.

[0077] In a second aspect, the present invention provides a pectin composite fiber microsphere powder, which is prepared by the method for preparing pectin composite fiber microsphere powder based on high-voltage pulse combined with fluidized bed process as described in the first aspect.

[0078] In a third aspect, the present invention provides a pectin composite fiber gel, wherein the pectin composite fiber gel is prepared by combining the pectin composite fiber microsphere powder as described in the second aspect and gastric acid.

[0079] In the present invention, the pectin composite fiber microsphere powder is dissolved in water and quickly forms gel when encountering gastric acid in the stomach, while wrapping carbohydrates such as starch and delaying the absorption of the latter, thereby reducing the rapid increase of blood sugar after a meal.

[0080] In a fourth aspect, the present invention provides a method for preparing the pectin composite fiber gel according to the third aspect, the preparation method comprising: Dissolving the pectin composite fiber microsphere powder in water to obtain a microsphere powder solution; The microsphere powder solution and simulated gastric fluid are mixed to form the composite fiber gel.

[0081] As an optional embodiment, the mass ratio of the pectin composite fiber microsphere powder to water is 1:(100-200), for example, it can be 1:100, 1:120, 1:140, 1:150, 1:160, 1:180, 1:200, etc.

[0082] As an optional embodiment, the mass ratio of the pectin composite fiber microsphere powder to the simulated gastric fluid is 1:(40~60), for example, it can be 1:40, 1:42, 1:44, 1:45, 1:46, 1:48, 1:50, 1:52, 1:54, 1:55, 1:56, 1:58, 1:60, etc.

[0083] As an optional embodiment, the simulated gastric fluid is prepared according to the method in Chinese Pharmacopoeia.

[0084] The time for forming the composite fiber gel is ≤60 s, for example, it can be 60 s, 55 s, 50 s, 45 s, 40 s, 35 s, 30 s, 25 s, 20 s, 15 s, 10 s, etc.

[0085] The multiple of the composite fiber gel is ≥90 times, for example, it can be 90 times, 91 times, 92 times, 93 times, 94 times, 95 times, 96 times, 97 times, 99 times, 100 times. (The multiple of the composite fiber gel refers to the weight of the gel formed.) The present invention is further described below by way of examples. Unless otherwise specified, the materials in the examples are prepared according to existing methods or directly purchased from the market.

[0086] Example 1 This embodiment provides a method for preparing composite fiber microsphere powder, the preparation method comprising the following steps: S1. Ultrafine grinding: 50 parts of low-fat pectin (esterification degree of 20%, molecular weight of 10000 g / mol), 20 parts of oat fiber, 20 parts of flaxseed fiber and 10 parts of guar bean fiber were put into an airflow ultrafine grinder with a crushing pressure of 2 MPa, an airflow velocity of 200 m / s and a crushing time of 1 h to obtain composite fiber powder; the composite fiber powder was passed through a multi-layer sieve to test the material particle size, and the particle size was 45-50 μm.

[0087] S2, high-speed dispersion and homogenization: 100 parts of the composite fiber powder obtained from S1 were added to 2000 parts of purified water, and homogenized and stirred using a high-speed dispersing homogenizer at a speed of 15000 r / min, a single homogenization time of 1 min, and homogenization was performed twice with an interval of 30 s to obtain a suspension 1.

[0088] S3, high voltage pulse processing: The suspension 1 obtained by S2 is placed in the processing chamber of a high-voltage pulse treatment device for high-voltage pulse treatment to maintain a stable flow of the liquid. The pulse frequency is 1 kHz, the pulse width is 10 μs, the flow rate is 10 L / h, the electric field strength is 10 kV / cm, and the pulse treatment time is 500 μs to obtain a suspension 2.

[0089] S4, fluidized bed spray drying: 300 parts of resistant dextrin are placed in a fluidized bed, and then 100 parts of suspension 2 obtained in S3 are atomized and sprayed onto the surface of the resistant dextrin. The spraying method is: top spraying, air inlet temperature is 80°C, material temperature is 60±5°C, fan frequency is 30 Hz, atomization pressure is 0.2Mpa, and the liquid inlet flow rate of suspension 2 is 60 g / min. After drying, the pectin composite fiber microsphere powder is obtained.

[0090] Example 2 This embodiment provides a method for preparing composite fiber microsphere powder, the preparation method comprising the following steps: S1. Ultrafine grinding: 70 parts of low-fat pectin (esterification degree of 26%, molecular weight of 15000 g / mol), 5 parts of oat fiber, 20 parts of flaxseed fiber, and 5 parts of guar bean fiber were put into an airflow ultrafine grinder with a crushing pressure of 6 MPa, an airflow velocity of 285 m / s, and a crushing time of 3 h to obtain composite fiber powder; the composite fiber powder was passed through a multi-layer sieve to test the material particle size, and the particle size was 10-15 μm.

[0091] S2, high-speed dispersion and homogenization: 100 parts of the composite fiber powder obtained from S1 were added to 1000 parts of purified water, and homogenized and stirred using a high-speed dispersing homogenizer at a speed of 20000 r / min, a single homogenization time of 1 min, and homogenized 3 times with an interval of 30 s to obtain a suspension 1.

[0092] S3, high voltage pulse processing: The suspension 1 obtained by S2 is placed in the processing chamber of a high-voltage pulse treatment device for high-voltage pulse treatment to maintain a stable flow of the liquid. The pulse frequency is 1 kHz, the pulse width is 10 μs, the flow rate is 10 L / h, the electric field strength is 10 kV / cm, and the pulse treatment time is 500 μs to obtain a suspension 2.

[0093] S4, fluidized bed spray drying: 300 parts of resistant dextrin are placed in a fluidized bed, and then 100 parts of suspension 2 obtained in S3 are atomized and sprayed onto the surface of the resistant dextrin. The spraying method is: top spraying, air inlet temperature is 100°C, material temperature is 72.5±2.5°C, fan frequency is 50 Hz, atomization pressure is 0.2 Mpa, and the liquid inlet flow rate of suspension 2 is 80 g / min. After drying, the pectin composite fiber microsphere powder is obtained.

[0094] Example 3 This embodiment provides a method for preparing composite fiber microsphere powder, the preparation method comprising the following steps: S1. Ultrafine grinding: 70 parts of low-fat pectin (esterification degree of 30%, molecular weight of 18000 g / mol), 5 parts of oat fiber, 5 parts of flaxseed fiber, and 20 parts of guar bean fiber were put into an airflow ultrafine grinder with a crushing pressure of 4 MPa, an airflow velocity of 240 m / s, and a crushing time of 2 h to obtain composite fiber powder; the composite fiber powder was passed through a multi-layer sieve to test the material particle size, and the particle size was 22~26 μm.

[0095] S2, high-speed dispersion and homogenization: 100 parts of the composite fiber powder obtained from S1 were added to 1000 parts of purified water, and homogenized and stirred using a high-speed dispersing homogenizer at a speed of 25000 r / min, a single homogenization time of 1 min, and homogenized 3 times with an interval of 30 s to obtain a suspension 1.

[0096] S3, high voltage pulse processing: The suspension 1 obtained by S2 is placed in the processing chamber of a high-voltage pulse treatment device for high-voltage pulse treatment to maintain a stable flow of the liquid. The pulse frequency is 2 kHz, the pulse width is 50 μs, the flow rate is 20 L / h, the electric field strength is 50 kV / cm, and the pulse treatment time is 100 μs to obtain a suspension 2.

[0097] S4, fluidized bed spray drying: 400 parts of resistant dextrin are placed in a fluidized bed, and then 100 parts of suspension 2 obtained in S3 are atomized and sprayed onto the surface of the resistant dextrin. The spraying method is: top spraying, inlet air temperature is 80°C, material temperature is 67.5±2.5°C, fan frequency is 20 Hz, atomization pressure is 0.3 Mpa, and the liquid inlet flow rate of suspension 2 is 20 g / min. After drying, the pectin composite fiber microsphere powder is obtained.

[0098] Example 4 This embodiment provides a method for preparing a composite fiber microsphere powder, which is different from Embodiment 2 only in that, in S1: the content of low-fat pectin is 40 parts, the content of oat fiber is 25 parts, the content of flaxseed fiber is 25 parts, and the content of guar bean fiber is 10 parts, and the other settings are consistent with Embodiment 2.

[0099] Example 5 This embodiment provides a method for preparing a composite fiber microsphere powder, which is different from Embodiment 2 only in that, in S1: the content of low-fat pectin is 80 parts, the content of oat fiber is 8 parts, the content of flaxseed fiber is 6 parts, and the content of guar bean fiber is 6 parts, and the other settings are consistent with Embodiment 2.

[0100] Example 6 This embodiment provides a method for preparing composite fiber microsphere powder, which is different from Embodiment 2 only in that, in S4: the resistant dextrin is replaced with maltodextrin of equal weight proportion, and other settings are consistent with Embodiment 1.

[0101] Comparative Example 1 This comparative example provides a method for preparing composite fiber microsphere powder, which is different from Example 2 only in that the ultrafine grinding process of S1 is not performed, and other settings are consistent with Example 2.

[0102] Comparative Example 2 This comparative example provides a method for preparing a composite fiber microsphere powder, which differs from Example 2 only in that, in S1: a roller mill is used for pulverization, and the powder is passed through a sieve to obtain a composite fiber powder with a particle size of 150-160 μm. Other settings are consistent with Example 2.

[0103] Comparative Example 3 This comparative example provides a method for preparing composite fiber microsphere powder, which is different from Example 2 only in that high-speed dispersing and homogenizing of S2 is not performed, and other settings are consistent with Example 2.

[0104] Comparative Example 4 This comparative example provides a method for preparing a composite fiber microsphere powder, which differs from Example 2 only in that, in S2: a magnetic stirrer is used for stirring, the stirring speed is 500 r / min, the stirring time is 2 h, and a suspension 1 is obtained, and the other settings are consistent with Example 2.

[0105] Comparative Example 5 This comparative example provides a method for preparing composite fiber microsphere powder, which is different from Example 2 only in that the high-voltage pulse process of S3 is not performed, and other settings are consistent with Example 2.

[0106] Comparative Example 6 This comparative example provides a method for preparing a composite fiber microsphere powder, which differs from Example 2 only in that, in S3: after the suspension obtained in S2 is poured into a sealed container, the container is placed in an ultrasonic device for ultrasonic treatment, the ultrasonic power is 600 W, and the time is 30 min. The other settings are consistent with Example 2.

[0107] Comparative Example 7 This comparative example provides a method for preparing composite fiber microsphere powder, which is different from Example 2 only in that the low-fat pectin in S1 is replaced by an equal weight of high-fat pectin, the degree of esterification is 62%, and other settings are consistent with Example 2.

[0108] Comparative Example 8 This comparative example provides a method for preparing a composite fiber microsphere powder, which differs from Example 2 only in that, in S4: there is no spray drying process, 100 parts of suspension 2 are placed in a constant temperature forced air drying oven, dried at 100°C, crushed through a 40-mesh sieve, and then mixed with 300 parts of resistant dextrin to obtain pectin composite fiber powder.

[0109] Comparative Example 9 This comparative example provides a method for preparing a composite fiber microsphere powder, which is different from Example 2 only in that, in S1: the crushing pressure is 8 MPa, the air flow velocity is 300 m / s, the crushing time is 30 min, and the material particle size is tested by multi-layer sieve after crushing, and the particle size is 61-65 μm. The other settings are consistent with Example 2.

[0110] Comparative Example 10 This comparative example provides a method for preparing a composite fiber microsphere powder, which is different from Example 2 only in that, in S1: the crushing pressure is 1 MPa, the air flow velocity is 180 m / s, the crushing time is 5 h, and the material particle size is tested by multi-layer sieve after crushing, and the particle size is 90-96 μm. The other settings are consistent with Example 2.

[0111] Comparative Example 11 This comparative example provides a method for preparing composite fiber microsphere powder, which is different from Example 2 only in that, in S2: the rotation speed is 5000 r / min, the homogenization time is 5 min, and the other settings are consistent with Example 2.

[0112] Comparative Example 12 This comparative example provides a method for preparing composite fiber microsphere powder, which is different from Example 2 only in that, in S2: the rotation speed is 13000 r / min, the homogenization time is 30 s, and the other settings are consistent with Example 2.

[0113] Comparative Example 13 This comparative example provides a method for preparing a composite fiber microsphere powder, which is different from Example 2 only in that, in S3: the pulse frequency is 0.5 kHz, the pulse width is 5 μs, the flow rate is 30 L / h, the electric field strength is 5 kV / cm, the pulse treatment time is 600 μs, and the other settings are consistent with Example 2.

[0114] Comparative Example 14 This comparative example provides a method for preparing a composite fiber microsphere powder, which is different from Example 2 only in that, in S3: the pulse frequency is 3 kHz, the pulse width is 60 μs, the flow rate is 5 L / h, the electric field strength is 60 kV / cm, the pulse treatment time is 60 μs, and the other settings are consistent with Example 2.

[0115] Comparative Example 15 This comparative example provides a method for preparing a composite fiber microsphere powder, which is different from Example 2 only in that, in S4: the inlet air temperature is 120°C, the material temperature is 80±5°C, the fan frequency is 10 Hz, the atomization pressure is 0.05 Mpa, the suspension liquid feed flow rate is 90 g / min, and the other settings are consistent with Example 2.

[0116] Comparative Example 16 This comparative example provides a method for preparing a composite fiber microsphere powder, which is different from Example 2 only in that, in S4: the inlet air temperature is 70°C, the material temperature is 50±5°C, the fan frequency is 60 Hz, the atomization pressure is 0.5 Mpa, the suspension liquid feed flow rate is 10 g / min, and the other settings are consistent with Example 1.

[0117] Test Example 1 Solubility test Test samples: the composite fiber microsphere powder provided in Examples 1 to 6 and the composite fiber microsphere powder provided in Comparative Examples 1 to 16.

[0118] Test method: Take 1 g of sample and add it into a beaker containing 200 mL of purified water at 60°C. Place the beaker on a constant temperature magnetic stirrer, set the heating temperature to 60°C and the speed to 300 r / min, observe the dissolution and record the complete dissolution time.

[0119] The specific test results are shown in Table 1: Table 1

[0120] It can be seen from the test data in Table 1 that the dissolution of the pectin composite fiber microsphere powder prepared by the present invention based on high-voltage pulse combined with fluidized bed process shows that there is no agglomeration at all, and the dissolution time is within 170 s; Comparative Example 8 does not use the fluidized bed process, and agglomeration occurs during dissolution, resulting in a longer dissolution time. This fully illustrates that the pectin composite fiber microsphere powder prepared by fluidized bed spray drying can effectively reduce the agglomeration phenomenon during pectin dissolution, and has better solubility.

[0121] Test Example 2 In vitro simulated gastric gel test Test samples: the composite fiber microsphere powder provided in Examples 1 to 6 and the composite fiber microsphere powder provided in Comparative Examples 1 to 16.

[0122] Test method: (a) Weigh 1 g of sample, add it into a beaker containing 150 mL of purified water, and stir rapidly until it is completely dissolved; (b) Add 50 mL of pharmacopoeial gastric juice to a beaker, then add 150 mL of dissolved sample, stir rapidly for 5-10 seconds, place in a 37±1℃ water bath for 30 minutes, then pour through an 80-mesh sieve and drain for 10 minutes. Weigh the gel and sieve, record as M2; the weight of the 80-mesh sieve, record as M1; (c) Gel multiple calculation formula: X=(M2-M1) / 1; Where X represents the gel multiple, dimensionless; M1 represents the weight of the sieve after drying, unit is g; M2 represents the total weight of the gel and sieve, unit is g; Among them, artificial gastric juice was prepared according to the 2010 edition of the Chinese Pharmacopoeia, and the method was as follows: 16.4 mL of dilute hydrochloric acid was added to artificial gastric juice, about 800 mL of water and 10 g of pepsin were added, and after shaking, water was added to dilute it to 1000 mL.

[0123] The specific test results are shown in Table 2: Table 2

[0124] It can be seen from the test data in Table 2 that the gel multiple of the pectin composite fiber gel prepared by the present invention based on high-voltage pulse combined with fluidized bed process is ≥65 times; wherein, Examples 1 to 3 are preferred schemes, and the gel multiple of the gel is ≥125 times. The gel multiples of Examples 1 to 3 are relatively high, indicating that the molecular chains of the composite fibers are opened to varying degrees, and self-assemble and entangle to form a mesh gel in gastric acid through the action of positive and negative groups. The higher the gel multiple, the higher the degree of opening of the molecular chains. The gel multiple of Example 6 is still maintained at a relatively high level, indicating that maltodextrin and resistant dextrin have little effect on its gel properties as carriers. Comparative Examples 1 to 4 and Comparative Examples 9 to 16, due to the use of non-range process parameters, some molecular chains are opened, and partial gels are formed under the action of gastric acid, resulting in a lower gel multiple. Comparative Examples 5 and 6 have the lowest gel multiples, because the lack of high-voltage pulse electric field action, the molecular chains are almost not opened, and a small amount of gel is formed under the action of gastric acid. Comparative Example 7 did not form a gel because high-fat pectin was used and could not form a gel with acid in a sugar-free environment, so no gel was formed.

[0125] This fully demonstrates that the high-voltage pulse current formed by the pulse electric field in the present invention can pierce the molecular chains of pectin and composite fibers, prompting their branch chains to open, thereby increasing the contact probability between molecular chains. After being dissolved in water again, a gel can be quickly formed by self-assembly under gastric acid conditions.

[0126] Test Example 3 Post-meal blood sugar level test Test samples: the composite fiber microsphere powder provided in Examples 1 to 6 and the composite fiber microsphere powder provided in Comparative Examples 1 to 16.

[0127] Test method: Twenty healthy adults were selected from each group, including 10 men and 10 women, aged 25-40 years old, with a BMI of 18.8-23.9 kg / m 2 , no history of diabetes (or impaired glucose tolerance), no other metabolic diseases, digestive system diseases, endocrine system diseases and mental illnesses, etc.; no history of allergy and intolerance to the tested food, normal oral glucose tolerance test, regular diet, no recent gastrointestinal diseases and taking any medications, and qualified physical examination. Before the experiment, the subjects were trained and signed informed consent. Stop eating and drinking after 22:00 the night before the experiment, and test the blood sugar fluctuation after breakfast.

[0128] Control group: consumed 202 mL of water 15 min before breakfast, and then consumed reference food white bread normally; Experimental group: consumed 2 g of each embodiment and comparative example sample within 15 min before breakfast (2 g of sample was dissolved in 200 mL of water), and then consumed reference food white bread normally; with time as the abscissa and blood glucose value at each time point-fasting blood glucose value as the ordinate, a blood glucose response curve was prepared, and the area under the curve (IAUC) above the fasting blood glucose level was calculated, and the inhibition rate (%) = (reference food IAUC-embodiment IAUC) / reference food IAUC × 100%.

[0129] Among them, the blood sugar test uses a Roche blood sugar meter, and the specific operation of measuring fingertip blood sugar is as follows: (1) Fingertip blood was collected, the first drop was discarded, and fasting blood glucose was measured twice with an interval of 5 min and recorded; (2) The control group consumed 202 mL of water; the experimental group consumed the example sample and the comparative example sample (2 g of the sample was dissolved in 200 mL of water) (3) 15 min later, the control group and the experimental group consumed white bread (calculated as 50 g of carbohydrate intake) within 5 min; blood glucose was measured and recorded (15 min, 30 min, 45 min, 60 min, 90 min, 120 min after the meal).

[0130] The specific test results are shown in Table 3: Table 3

[0131] It can be seen from the test data in Table 3 that after eating the pectin composite fiber microsphere powder prepared by the present invention based on high-voltage pulse combined with fluidized bed technology, the blood sugar suppression rate is more than 33%; among them, Examples 1 to 3 are preferred schemes, and after using the pectin composite fiber microsphere powder prepared by Examples 1 to 3, the blood sugar suppression rate can reach more than 62%.

[0132] The blood sugar suppression rate of Examples 1 to 3 is relatively high because the pectin composite fiber solution forms a gel in the gastric juice while wrapping most of the chyme, delaying the gastrointestinal tract's absorption and conversion of carbohydrates. Although Example 6 has a high gel multiple, the blood sugar suppression rate is low because maltodextrin is a carbohydrate that can cause blood sugar to rise, and resistant dextrin is a dietary fiber that does not cause blood sugar to rise in the body. Therefore, using resistant dextrin as a carrier can more effectively suppress the rise in postprandial blood sugar. The blood sugar suppression rate of Comparative Examples 1 to 16 is relatively low because its fiber solution has a low gel multiple in gastric acid, wraps less chyme, and has a high gastrointestinal absorption of carbohydrates. The data of Comparative Examples 1 to 16 show that the higher the gel multiple, the more chyme is wrapped, and the higher the blood sugar suppression rate.

[0133] This shows that the pectin composite fiber microsphere powder of the present invention dissolves in water, and quickly forms a gel when encountering gastric acid in the stomach, while wrapping carbohydrates such as starch and delaying the latter's absorption, thereby playing a role in reducing the rapid increase of blood sugar after a meal.

[0134] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing pectin composite fiber microsphere powder based on high-voltage pulse combined with fluidized bed process, characterized in that: The method comprises the following steps: The composite fiber is ultrafinely ground to obtain composite fiber powder; wherein the composite fiber comprises low-fat pectin, oat fiber, flaxseed fiber and guar fiber; the ultrafine grinding pressure is 2-6 MPa, and the air flow velocity is 200-285 m / s; The composite fiber powder and water are dispersed and homogenized at high speed to obtain a suspension; wherein the rotation speed of the high-speed dispersion and homogenization is 15000-25000 r / min; The suspension is subjected to high-voltage pulse treatment, and then the treated suspension is sprayed on the surface of the carrier through a fluidized bed spray drying process to obtain pectin composite fiber microsphere powder; wherein the process parameters of the high-voltage pulse treatment include: a pulse frequency of 1-2 kHz, a pulse width of 10-50 μs, a flow rate of 10-20 L / h, an electric field strength of 10-50 kV / cm, and a pulse treatment time of 100-500 μs; the process parameters of the fluidized bed spray drying process include: a spray mode of top spraying, an air inlet temperature of 80-100°C, a material temperature of 55-75°C, a fan frequency of 20-50 Hz, an atomization pressure of 0.1-0.3 Mpa, and a liquid feed flow rate of the suspension of 20-80 g / min.

2. The method for preparing pectin composite fiber microsphere powder based on high-voltage pulse combined with fluidized bed process according to claim 1, characterized in that: The composite fiber comprises the following components by weight percentage: 50-70% low-fat pectin, 5-20% oat fiber, 5-20% flaxseed fiber and 5-20% guar bean fiber.

3. The method for preparing pectin composite fiber microsphere powder based on high-voltage pulse combined with fluidized bed process according to claim 1 or 2, characterized in that: The esterification degree of the low-fat pectin is 20-40%; And / or, the molecular weight of the low-fat pectin is 10000-20000 g / mol.

4. The method for preparing pectin composite fiber microsphere powder based on high-voltage pulse combined with fluidized bed process according to claim 1, characterized in that: The ultrafine grinding is carried out in an airflow ultrafine grinding machine; And / or, the ultrafine grinding time is 1 to 3 hours; And / or, the particle size of the composite fiber powder is 10-50 μm.

5. The method for preparing pectin composite fiber microsphere powder based on high-voltage pulse combined with fluidized bed process according to claim 1, characterized in that: The mass ratio of the composite fiber powder to water is 1:(10-20); And / or, the process parameters of the high-speed dispersion and homogenization include: a single homogenization time of 30 s to 2 min, a homogenization number of 1 to 5 times, and an interval time of 10 to 40 s.

6. The method for preparing pectin composite fiber microsphere powder based on high-voltage pulse combined with fluidized bed process according to claim 1, characterized in that: The carrier includes resistant dextrin; And / or, the mass ratio of the carrier to the suspension is (3~4):

1.

7. A pectin composite fiber microsphere powder, characterized in that: The pectin composite fiber microsphere powder is prepared by the method for preparing pectin composite fiber microsphere powder based on high-voltage pulse combined with fluidized bed process according to any one of claims 1 to 6.

8. A pectin composite fiber gel, characterized in that: The pectin composite fiber gel is prepared by combining the pectin composite fiber microsphere powder according to claim 7 and gastric acid.

9. A method for preparing the pectin composite fiber gel according to claim 8, characterized in that: The preparation method comprises: Dissolving the pectin composite fiber microsphere powder in water to obtain a microsphere powder solution; The microsphere powder solution and simulated gastric fluid are mixed to form the composite fiber gel.

10. The method for preparing pectin composite fiber gel according to claim 9, characterized in that: The mass ratio of the pectin composite fiber microsphere powder to water is 1:(100-200); And / or, the mass ratio of the pectin composite fiber microsphere powder to the simulated gastric fluid is 1:(40-60); and / or, the time for forming the composite fiber gel is ≤ 60 s; And / or, the multiple of forming the composite fiber gel is ≥90 times.

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