Insoluble solid particle suspension system and preparation method thereof

By controlling the particle size of insoluble calcium supplements and preparing specific combination components, and using gradient cooling and high-speed shear mixing processes, the problem of difficulty in stable suspension and dispersion of insoluble solid particles in water in the prior art is solved, and the preparation of a stable and non-layered insoluble solid particles is achieved.

CN119655447APending Publication Date: 2025-03-21GUANGZHOU PROCEPT BIOTECH
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Patent Information

Application Number
CN202411958167.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-30
Publication Date
2025-03-21

AI Technical Summary

Technical Problem

The existing insoluble solid particle suspension system is difficult to achieve stable suspension dispersion in water, and the preparation process is complex, with individual oil leakage and slight stratification.

Method used

By controlling the particle size of insoluble calcium supplements between 2000-2500 mesh, combined with the ratio of thickener, mixed suspension agent and sugar alcohol, a stable, non-layered insoluble solid particles suspension system was prepared using the process of gradient cooling and high-speed shearing.

Benefits of technology

The stable suspension of insoluble calcium supplements in water is achieved, precipitation and stratification are avoided, and the stability of the suspension system and the simplicity of preparation are improved.

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Abstract

The invention provides an insoluble solid particle suspension system which comprises the following raw materials in parts by weight: 10-30 parts of an insoluble calcium supplement, 2-4 parts of a thickening agent, 0.5-2.5 parts of sugar alcohol, 3-7 parts of a mixed suspending aid, 0.3-0.8 part of a functional nutritional raw material, 0.1-0.5 part of a flavoring agent, 1-3 parts of a sweetening agent and 50-70 parts of deionized water, the insoluble calcium supplement is one or a mixture of seaweed calcium, milk mineral salt or calcium citrate; the particle size of the insoluble calcium supplement is controlled to be 2000-2500 meshes; the thickening agent is one or a mixture of xanthan gum, chitosan or pectin; the sugar alcohol is one or a mixture of xylitol or erythritol. A stable and non-layering insoluble solid particle suspension system is obtained by controlling the size of the insoluble calcium supplement, the formula of the suspension system and a preparation process.
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Description

Technical Field

[0001] The invention belongs to the field of food, and specifically relates to an insoluble solid particle suspension system and a preparation method thereof. Background Art

[0002] Suspensions of Insoluble Solid Particles refer to a dispersion system formed by dispersing solid particles insoluble in a solvent (usually water) in a solvent. This system is widely used in many fields such as pharmaceuticals, chemicals, and food.

[0003] The insoluble solid particle suspension system usually consists of the following parts: solid particles: particles insoluble in solvents, which can be drugs, pigments, fillers, etc.; solvents: usually water, but can also be organic solvents or other liquids; suspending agents: used to increase the stability of the system and prevent particle sedimentation.

[0004] Patent CN109007934A discloses an ultrafine suspension system that improves product stability by reducing the particle size of powder materials and increasing the mass ratio of powder phase to oil phase, but individual oil leakage and slight stratification still occur, and the process of preparing ultrafine powder is complicated and requires high equipment; CN114158720A discloses a suspension with high solid content and a preparation method thereof, wherein the suspension comprises 52-75% of solid active ingredients, 10-45% of oil dispersant, 0.5-5% of solubilizer, 0.1-5% of surfactant and 0.1-3% of flow aid, and the preparation method thereof adopts a grinding method to form a stable suspension of the feed liquid. However, the patent mainly solves the suspension dispersion of solid components in oil dispersants, and cannot solve the stable suspension dispersion of solid components in water. Summary of the invention

[0005] The purpose of the present invention is to provide an insoluble solid particle suspension system and a preparation method thereof. By controlling the size of an insoluble calcium supplement, a suspension system formula and a preparation process, a stable, non-stratified insoluble solid particle suspension system is obtained.

[0006] In order to achieve the above object, the present invention provides the following technical solutions: An insoluble solid particle suspension system, the raw materials of which include the following components in parts by weight: 10-30 parts of an insoluble calcium supplement, 2-4 parts of a thickener, 0.5-2.5 parts of a sugar alcohol, 3-7 parts of a mixed suspending agent, 0.3-0.8 parts of a functional nutrient raw material, 0.1-0.5 parts of a flavoring agent, 1-3 parts of a sweetener and 50-70 parts of deionized water.

[0007] Furthermore, the insoluble calcium supplement is one or a mixture of seaweed calcium, milk mineral salt or calcium citrate.

[0008] Furthermore, the particle size of the insoluble calcium supplement is controlled within the range of 2000-2500 meshes.

[0009] Furthermore, the thickener is one or a mixture of xanthan gum, chitosan or pectin.

[0010] Furthermore, the sugar alcohol is one or a mixture of xylitol or erythritol.

[0011] Furthermore, the mixed suspending agent is a mixture of soybean lecithin and glyceryl monostearate in a mass ratio of 1:2-4.

[0012] Furthermore, the functional nutritional raw material is one or a mixture of vitamin D, vitamin K, L-lysine, colostrum basic protein, casein phosphopeptide, γ-aminobutyric acid, and galacto-oligosaccharide.

[0013] Furthermore, the flavoring agent is one or a mixture of fruit and vegetable juice, fruit and vegetable powder, acidulant, and food flavoring.

[0014] Furthermore, according to the insoluble solid particle suspension system of claim 1, it is characterized in that the sweetener is one or a mixture of steviol glycoside and mogroside.

[0015] The preparation method of the above-mentioned insoluble solid particle suspension system comprises the following steps: S1: 10-30 parts of an insoluble calcium supplement, 2-4 parts of a thickener and 3-7 parts of a mixed suspending agent are mixed, and heated at a temperature of 90-120° C. and a rate of 2000-4000 r / min for 35-55 min under a nitrogen environment to obtain a mixed solution A; S2: Cool the mixed solution A in step S1 to 75-85° C., add 0.5-2.5 parts of sugar alcohol and 50-70 parts of deionized water, and stir at a rate of 3000-5000 r / min for 10-20 min under a nitrogen environment to obtain a mixed solution B; S3: Cooling the mixed solution B in step S2 to 60-70° C., adding 0.3-0.8 portions of functional nutrient raw materials, stirring at a rate of 2500-3500 r / min for 15-25 min under a nitrogen environment, and homogenizing at a pressure setting of 50-80 bar to obtain a mixed solution C; S4: Cooling the mixed solution C in step S3 to 30-40° C., adding 0.1-0.5 parts of flavoring agent and 1-3 parts of sweetener, stirring and reacting at a rate of 6000-8000 r / min for 40-60 minutes, and obtaining the insoluble solid particle suspension system.

[0016] Compared with the prior art, the advantages and beneficial effects of the present invention are: The invention firstly compound an insoluble calcium supplement, a thickener and a mixed suspending agent, and simultaneously heats the mixture in an inert gas environment in combination with gradient cooling and step-by-step feeding to improve the stability of the suspension system; the particle size of the insoluble calcium supplement is controlled to be below 2000-2500 meshes, and then high-speed shear mixing is combined, and an excellent sedimentation rate is ensured by using specific combination components, so that the insoluble calcium supplement is not easy to precipitate and does not form lumps, thereby forming a stable, non-stratified insoluble solid particle suspension system. DETAILED DESCRIPTION

[0017] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. 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.

[0018] The raw materials used in the present invention are as follows: Seaweed calcium was obtained from Qingdao Miaopinyuan Co., Ltd., item number 909784; xanthan gum was obtained from Jiangsu Weizhirun Biotechnology Co., Ltd., item number 3336; soybean lecithin was obtained from Guangzhou Haisha Biological Co., Ltd., item number 23033103; glyceryl monostearate was obtained from Kerry Kerry Ingredients Trading (Shanghai) Co., Ltd., item number 4Z23940A; xylitol was obtained from Zhejiang Huakang Pharmaceutical Co., Ltd., item number XZ23033001; vitamin D was obtained from Shanghai Yuanye Biotechnology Co., Ltd., item number S80764; fruit and vegetable juice was obtained from Guangzhou Tianjia Biotechnology Co., Ltd., item number 3728 ; Stevioside is from Shandong Haigen Biotechnology Co., Ltd., item number 20230316; chitosan is from Shandong Haiyihua Biotechnology Co., Ltd., item number 51; erythritol is from Shaanxi Panier Biotechnology Co., Ltd., item number 604; casein phosphopeptide is from Shanghai Yuanye Biotechnology Co., Ltd., item number S25818; food flavor is from Guangzhou Hengyu Spice Co., Ltd., item number hy-14355; mogroside is from Zhangjiajie Jiurui Biotechnology Co., Ltd., item number 119; γ-aminobutyric acid is from Nantong Licheng Biotechnology Co., Ltd., item number γ20230503.

[0019] Example 1 This embodiment provides a method for preparing an insoluble solid particle suspension system, comprising the following steps: S1: 10g of seaweed calcium with a particle size of 2000-2500 mesh, 2g of xanthan gum and 3g of a mixed suspending agent (a mixture of soybean lecithin and glyceryl monostearate in a mass ratio of 1:2) were mixed, and heated at 90°C and a speed of 2000r / min for 35min under a nitrogen environment to obtain a mixed solution A; S2: Cool the mixed solution A in step S1 to 75° C., add 0.5 g of xylitol and 50 g of deionized water, and stir at a rate of 3000 r / min for 10 min under a nitrogen environment to obtain a mixed solution B; S3: Cool the mixed solution B in step S2 to 60° C., add 0.3 g of vitamin D, stir at a rate of 2500 r / min for 15 min under a nitrogen environment, and homogenize at a pressure of 50 bar to obtain a mixed solution C; S4: Cool the mixed solution C in step S3 to 30° C., add 0.1 g of fruit and vegetable juice and 1 g of stevioside, and stir at a rate of 6000 r / min for 40 min to obtain the insoluble solid particle suspension system.

[0020] Example 2 This embodiment provides a method for preparing an insoluble solid particle suspension system, comprising the following steps: S1: Mix 30g of calcium citrate with a particle size of 2000-2500 mesh, 4g of chitosan and 7g of a mixed suspending agent (a mixture of soybean lecithin and glyceryl monostearate in a mass ratio of 1:4), and heat at 120°C and a speed of 4000r / min for 55min under a nitrogen environment to obtain a mixed solution A; S2: Cool the mixed solution A in step S1 to 85° C., add 2.5 g of erythritol and 70 g of deionized water, and stir at a rate of 5000 r / min for 20 min under a nitrogen environment to obtain a mixed solution B; S3: Cool the mixed solution B in step S2 to 70° C., add 0.8 g of casein phosphopeptide, stir at a rate of 3500 r / min for 25 min under a nitrogen environment, and homogenize at a pressure of 80 bar to obtain a mixed solution C; S4: Cool the mixed solution C in step S3 to 40° C., add 0.5 g of food flavor and 3 g of mogroside, and stir at a rate of 8000 r / min for 60 min to obtain the insoluble solid particle suspension system.

[0021] Example 3 This embodiment provides a method for preparing an insoluble solid particle suspension system, comprising the following steps: S1: Mix 20g of seaweed calcium with a particle size of 2000-2500 mesh, 3g of pectin and 5g of a mixed suspending agent (a mixture of soybean lecithin and glyceryl monostearate in a mass ratio of 1:3), and heat at 110°C and a speed of 3500r / min for 50min under a nitrogen environment to obtain a mixed solution A; S2: Cool the mixed solution A in step S1 to 80° C., add 2 g of erythritol and 60 g of deionized water, and stir at a rate of 4000 r / min for 15 min under a nitrogen environment to obtain a mixed solution B; S3: Cool the mixed solution B in step S2 to 65° C., add 0.5 g of γ-aminobutyric acid, stir at a rate of 3000 r / min for 22 min under a nitrogen environment, and homogenize at a pressure of 65 bar to obtain a mixed solution C; S4: Cool the mixed solution C in step S3 to 35° C., add 0.3 g of fruit and vegetable powder and 2 g of mogroside, and stir at a rate of 7000 r / min for 50 min to obtain the insoluble solid particle suspension system.

[0022] Example 4 This embodiment provides a method for preparing an insoluble solid particle suspension system, comprising the following steps: S1: 12g of milk mineral salt with a particle size of 2000-2500 mesh, 3g of chitosan and 6g of a mixed suspending agent (a mixture of soybean lecithin and glyceryl monostearate in a mass ratio of 1:3) were mixed, and heated at 100°C and a speed of 3000r / min for 40min under a nitrogen environment to obtain a mixed solution A; S2: Cool the mixed solution A in step S1 to 80° C., add 1.5 g of xylitol and 55 g of deionized water, and stir at a rate of 3500 r / min for 15 min under a nitrogen environment to obtain a mixed solution B; S3: Cooling the mixed solution B in step S2 to 63° C., adding 0.5 g of colostrum alkaline protein, stirring at a rate of 2800 r / min for 18 min under a nitrogen environment, and homogenizing at a pressure setting of 65 bar to obtain a mixed solution C; S4: Cool the mixed solution C in step S3 to 33° C., add 0.3 g of acidulant and 1.5 g of mogroside, and stir at a rate of 6500 r / min for 45 min to obtain the insoluble solid particle suspension system.

[0023] Example 5 This embodiment provides a method for preparing an insoluble solid particle suspension system, comprising the following steps: S1: Mix 25g of seaweed calcium with a particle size of 2000-2500 mesh, 3g of chitosan and 6g of a mixed suspending agent (a mixture of soybean lecithin and glyceryl monostearate in a mass ratio of 1:4), and heat at 115°C and a speed of 3500r / min for 52min under a nitrogen environment to obtain a mixed solution A; S2: Cool the mixed solution A in step S1 to 83° C., add 2.2 g of xylitol and 67 g of deionized water, and stir at a rate of 4800 r / min for 16 min under a nitrogen environment to obtain a mixed solution B; S3: Cool the mixed solution B in step S2 to 66° C., add 0.6 g of galacto-oligosaccharide, stir at a rate of 3200 r / min for 22 min under a nitrogen environment, and homogenize at a pressure of 75 bar to obtain a mixed solution C; S4: Cool the mixed solution C in step S3 to 37° C., add 0.4 g of fruit and vegetable juice and 2.5 g of stevioside, and stir at a rate of 7500 r / min for 55 min to obtain the insoluble solid particle suspension system.

[0024] Comparative Example 1 The difference between this comparative example and Example 3 is that the mixing suspending agent is missing in step S1, and the other steps are the same.

[0025] Comparative Example 2 The difference between this comparative example and Example 3 is that pectin is missing in step S1, and the other steps are the same.

[0026] Comparative Example 3 The difference between this comparative example and Example 3 is that step S2 and step S3 are missing, that is, no gradient cooling is performed, and 2 g of erythritol and 0.5 g of γ-aminobutyric acid are directly added and mixed in step S4, and the other steps are the same.

[0027] Performance Test: Appearance evaluation: The prepared suspension system is sterilized at 90°C for 1 hour and then cooled to room temperature to evaluate the severity of its stratification. The evaluation indicators are as follows: Observe the appearance with the naked eye. If there is no obvious stratification on the liquid surface, it means there is no stratification. Centrifugation evaluation: Take the sterilized sample and place it in a centrifuge tube and centrifuge it at 25°C and 4000rpm for 10 minutes. Then, aspirate the supernatant with a pipette, test the quality, and obtain the water output. Water output rate = (water output / sample amount) 100%, " / " in each table indicates water yield, which means no stratification and no water yield. Sterilized samples were added to the sample tube and tested using a rotary viscometer. The instrument was leveled and the SP-3 rotor was used to measure the sample viscosity at 25°C. The results are as follows: Table 1

[0028] From the above performance test results, it can be seen that Examples 1-5 have excellent performance in appearance, viscosity, etc., and the insoluble calcium supplement is suspended stably in the system. In particular, the comprehensive performance of Example 3 is the most outstanding. However, since Comparative Examples 1-3 do not adopt the necessary technical solutions, their corresponding performance tests are significantly worse than those of the Examples. The above experimental results further prove the importance of the technical solutions defined in the present invention for its technical effects.

[0029] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. An insoluble solid particle suspension system, characterized in that: The raw materials include the following components in parts by weight: 10-30 parts of insoluble calcium supplement, 2-4 parts of thickener, 0.5-2.5 parts of sugar alcohol, 3-7 parts of mixed suspending agent, 0.3-0.8 parts of functional nutrient raw materials, 0.1-0.5 parts of flavoring agent, 1-3 parts of sweetener and 50-70 parts of deionized water.

2. An insoluble solid particle suspension system according to claim 1, characterized in that: The insoluble calcium supplement is one or a mixture of seaweed calcium, milk mineral salt or calcium citrate.

3. An insoluble solid particle suspension system according to claim 2, characterized in that: The particle size of the insoluble calcium supplement is controlled at 2000-2500 meshes.

4. The insoluble solid particle suspension system according to claim 1, characterized in that: The thickener is one or a mixture of xanthan gum, chitosan or pectin.

5. The insoluble solid particle suspension system according to claim 1, characterized in that: The sugar alcohol is one or a mixture of xylitol or erythritol.

6. The insoluble solid particle suspension system according to claim 1, characterized in that: The mixed suspending agent is a mixture of soybean lecithin and glyceryl monostearate in a mass ratio of 1:2-4.

7. The insoluble solid particle suspension system according to claim 1, characterized in that: The functional nutritional raw material is one or a mixture of vitamin D, vitamin K, L-lysine, colostrum basic protein, casein phosphopeptide, gamma-aminobutyric acid, and galacto-oligosaccharide.

8. The insoluble solid particle suspension system according to claim 1, characterized in that: The flavoring agent is one or a mixture of fruit and vegetable juice, fruit and vegetable powder, acidulant, and food flavor.

9. The insoluble solid particle suspension system according to claim 1, characterized in that: The sweetener is one of stevioside and mogroside or a mixture thereof.

10. A method for preparing an insoluble solid particle suspension system, characterized in that: The steps include: S1: 10-30 parts of an insoluble calcium supplement, 2-4 parts of a thickener and 3-7 parts of a mixed suspending agent are mixed, and heated at a temperature of 90-120° C. and a rate of 2000-4000 r / min for 35-55 min under a nitrogen environment to obtain a mixed solution A; S2: Cool the mixed solution A in step S1 to 75-85° C., add 0.5-2.5 parts of sugar alcohol and 50-70 parts of deionized water, and stir at a rate of 3000-5000 r / min for 10-20 min under a nitrogen environment to obtain a mixed solution B; S3: Cooling the mixed solution B in step S2 to 60-70° C., adding 0.3-0.8 portions of functional nutrient raw materials, stirring at a rate of 2500-3500 r / min for 15-25 min under a nitrogen environment, and homogenizing at a pressure setting of 50-80 bar to obtain a mixed solution C; S4: Cooling the mixed solution C in step S3 to 30-40° C., adding 0.1-0.5 parts of flavoring agent and 1-3 parts of sweetener, stirring and reacting at a rate of 6000-8000 r / min for 40-60 minutes, and obtaining the insoluble solid particle suspension system.

Citation Information

Patent Citations

  • Ultrafine suspension system

    CN109007934A

  • High-solid-content suspension and preparation method thereof

    CN114158720A