Glucosamine chondroitin bone collagen composition for improving bone and joint functions and preparation method of glucosamine chondroitin bone collagen composition

Abstract

The invention belongs to the technical field of health-care food, and particularly relates to a glucosamine chondroitin bone collagen composition for improving bone and joint functions and a preparation method of the glucosamine chondroitin bone collagen composition. The glucosamine chondroitin collagen composition is characterized by being prepared from the following raw materials in parts by weight: 160 to 200 parts of calcium carbonate, 150 to 200 parts of D-glucosamine hydrochloride, 40 to 50 parts of chondroitin sulfate, 30 to 50 parts of bone collagen powder, 5 to 10 parts of hydroxypropyl methyl cellulose, 10 to 20 parts of sodium carboxymethyl starch and 2 to 8 parts of magnesium stearate. By reasonably controlling the ratio of the D-glucosamine hydrochloride to the chondroitin sulfate and the ratio of the calcium carbonate to the bone collagen powder, a better effect of increasing the bone mineral density is achieved. By reasonably controlling the content of the auxiliary materials, the product has better hardness, disintegration time limit and friability.

Description

Technical Field

[0001] The invention belongs to the technical field of health food, and particularly relates to a glucosamine chondroitin collagen composition for improving bone and joint function and a preparation method thereof. Background Art

[0002] In recent years, the development of functional compositions that promote the health of athletes and use nutritional means to delay the onset of fatigue and promote fatigue recovery has become a research hotspot in disciplines such as sports, medicine, and food. Existing compositions that promote the health of athletes mainly contain ingredients such as complex polysaccharides, unsaturated fatty acids, branched-chain amino acids, or active ingredients. They generally have the disadvantages of unreasonable formulations, insufficient nutrition, poor human absorption, low nutrient utilization, and insignificant effects in increasing bone density and relieving physical fatigue. There are also Chinese herbal compositions on the market that promote the health of athletes. However, such compositions cannot supplement the protein and energy needs during and after exercise, nor can they effectively promote the recovery of bones and joints.

[0003] Glucosamine promotes cartilage synthesis and chondrocyte growth, increases bone calcium uptake, stimulates mucopolysaccharide biosynthesis, increases synovial fluid viscosity, and alleviates pain. Chondroitin sulfate can reverse cartilage damage and increase synovial fluid. Chondroitin inhibits cyclooxygenase-2, alleviating joint inflammation; it reduces fibrin clot formation and promotes blood circulation in the subchondral bone. Chondroitin and glucosamine work synergistically, further enhancing the improvement effect. Combined use also increases safety and prevents adverse reactions.

[0004] For example, Chinese patent CN108619493A discloses a capsule for increasing bone density. The capsule is made of calcium carbonate, D-glucosamine hydrochloride, chondroitin sulfate, collagen powder, vitamin K2, microcrystalline cellulose, and magnesium stearate. The invention also discloses a method for preparing the capsule for increasing bone density. The capsule for increasing bone density of the invention combines the various functions of calcium carbonate, D-glucosamine hydrochloride, chondroitin sulfate, collagen powder, and vitamin K2, is suitable for middle-aged and elderly people, and can increase the bone density of the user. However, the effect of the invention on increasing bone density still needs to be improved, and the bioavailability of the capsule is not ideal.

[0005] For example, Liu Lei mentioned in "Study on the Bone Density Increasing Function of Glucosamine Chondroitin Tablets" Food Industry, 2022, 43(09): 143-145 that glucosamine chondroitin tablets prepared with D-glucosamine hydrochloride, sodium chondroitin sulfate, calcium carbonate, fish collagen and casein phosphopeptide as the main raw materials were used as the research object. According to the evaluation method and judgment standard of the bone density increasing function in the "Technical Specifications for Inspection and Evaluation of Health Foods", the study found that glucosamine chondroitin tablets can significantly increase the calcium content and bone density of rat femurs. However, the selection of unknown excipients for glucosamine chondroitin tablets provided in the document cannot fully exert the effect of the active ingredients.

[0006] Therefore, there is an urgent need to study a glucosamine chondroitin collagen composition with high bioavailability that can increase bone density and a preparation method thereof. Summary of the Invention

[0007] Based on the shortcomings of the prior art, the present invention aims to provide a glucosamine chondroitin collagen composition for improving bone and joint function and a preparation method thereof. The glucosamine chondroitin collagen composition provided by the present invention can significantly increase bone density.

[0008] To achieve the above object, the present invention adopts the following technical solutions: On the one hand, the present invention provides a glucosamine chondroitin collagen composition, which includes the following raw materials, by weight: 160-200 parts of calcium carbonate, 150-200 parts of D-glucosamine hydrochloride, 40-50 parts of chondroitin sulfate, 30-50 parts of bone collagen powder, 5-10 parts of hydroxypropyl methylcellulose, 10-20 parts of sodium carboxymethyl starch and 2-8 parts of magnesium stearate.

[0009] Preferably, the mass ratio of D-glucosamine hydrochloride to chondroitin sulfate is 3-5:1, more preferably 4:1.

[0010] Preferably, the mass ratio of calcium carbonate to collagen powder is 4-6:1, more preferably 4.5:1.

[0011] Preferably, the glucosamine chondroitin collagen composition comprises the following raw materials: 180 parts of calcium carbonate, 180 parts of D-glucosamine hydrochloride, 45 parts of chondroitin sulfate, 40 parts of bone collagen powder, 8 parts of hydroxypropyl methylcellulose, 10 parts of sodium carboxymethyl starch and 5 parts of magnesium stearate.

[0012] On the other hand, the present invention also provides a method for preparing the above-mentioned glucosamine chondroitin collagen composition, comprising the following steps: (1) Weigh the formulated amount of calcium carbonate, D-glucosamine hydrochloride, chondroitin sulfate and collagen powder, mix them evenly, add the formulated amount of hydroxypropyl methylcellulose, mix, dry, grind and sieve to obtain a mixture; (2) Weighing the formulated amount of sodium carboxymethyl starch and magnesium stearate and mixing them with the mixture obtained in step (1) to obtain the product.

[0013] Preferably, the drying temperature in step (1) is 40-50° C., and the drying time is 10-20 min.

[0014] More preferably, the drying temperature in step (1) is 45° C. and the drying time is 15 minutes.

[0015] Preferably, the mesh size of the sieving in step (1) is 30-50 mesh, more preferably 40 mesh.

[0016] Finally, the present invention also provides the use of the glucosamine chondroitin collagen composition in the preparation of body-building products.

[0017] Preferably, the product is a health food.

[0018] Preferably, the dosage form of the product is tablets, capsules, granules or oral liquid.

[0019] The present invention also provides a glucosamine chondroitin collagen tablet, the preparation method of which comprises the following steps: (1) Weigh the formulated amount of calcium carbonate, D-glucosamine hydrochloride, chondroitin sulfate, collagen powder and hydroxypropyl methylcellulose, mix them, and granulate the mixture; (2) Drying after granulation; (3) After drying, add the formulated amount of magnesium stearate and sodium carboxymethyl starch for tableting and coating.

[0020] Preferably, the granulation in step (1) is wet granulation, and the specific operation is: adding a wetting agent to the mixture in step (1), the wetting agent is ethanol with a volume fraction of 60-80%, and the specific process conditions of the wet granulation are: premixing stirring at 120-130 rpm, shearing at 1000-1200 rpm, mixing for 5-10 minutes; the spray pressure is 0.1-0.4 MPa, the peristaltic pump speed is 5-10 Hz, stirring at 120-130 rpm, shearing at 1000-1200 rpm, the total liquid addition time is 5-15 minutes, and granulation is performed for 1-2 minutes after the liquid addition is completed.

[0021] More preferably, the specific operation of the granulation in step (1) is: adding a wetting agent to the mixture in step (1), wherein the wetting agent is ethanol with a volume fraction of 70%, and the specific process conditions of the wet granulation are: The premix was stirred at 125 rpm, sheared at 1100 rpm, mixed for 5 min, the spray pressure was 0.3 MPa, the peristaltic pump speed was 7 Hz, stirred at 125 rpm, sheared at 1100 rpm, the total liquid addition time was 10 min, and granulated for 1 min after the liquid addition was completed.

[0022] Preferably, the drying in step (2) is performed by fluidized bed drying, and the specific operation is as follows: the inlet air temperature is set to 60-70°C, the material temperature is set to 35-45°C, and the moisture content is controlled to 1-3%.

[0023] More preferably, the specific operation of drying in step (2) is: the inlet air temperature is set to 65°C, the material temperature is set to 40°C, and the moisture content is controlled to 2%.

[0024] Preferably, the specific operation of tableting in step (3) is: tableting is performed using a high-speed rotary tablet press with an average hardness of 50-70N and a tableting speed of 3-6w / h.

[0025] More preferably, the specific operation of tableting in step (3) is: tableting is performed using a high-speed rotary tablet press with an average hardness of 60N and a tableting speed of 5w / h.

[0026] Preferably, the specific operation of coating in step (3) is as follows: controlling the air inlet temperature to 60-70°C, the pot speed to 5-10rpm, the atomization pressure to 0.1-0.5MPa, the fan pressure to 0.1-0.5MPa, the peristaltic pump speed to 15-30rpm, the tablet surface temperature to 35-40°C, and the weight gain to 1-3%, to obtain glucosamine chondroitin collagen tablets.

[0027] More preferably, the specific operation of coating in step (3) is as follows: controlling the air inlet temperature to 65°C, the pot speed to 8 rpm, the atomization pressure to 0.3 MPa, the fan pressure to 0.3 MPa, the peristaltic pump speed to 25 rpm, the tablet surface temperature to 35°C, and the weight gain to 2%, to obtain glucosamine chondroitin collagen tablets.

[0028] Compared with the prior art, the present invention has the following beneficial effects: (1) The present invention has a better effect of increasing bone density by rationally controlling the ratio of D-glucosamine hydrochloride and chondroitin sulfate and the ratio of calcium carbonate and collagen powder.

[0029] (2) The present invention reasonably controls the content of excipients to make the product have better hardness, disintegration time and friability. DETAILED DESCRIPTION

[0030] The technical solution of the present invention is described clearly and completely below with specific embodiments. Obviously, the embodiments described are only some embodiments of the present invention, rather than all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work are within the scope of protection of the present invention. Unless otherwise specified, the materials and reagents used are commercially available reagents and materials.

[0031] Example 1 A Glucosamine Chondroitin Collagen Composition The preparation comprises the following raw materials in parts by weight: 180 parts of calcium carbonate, 180 parts of D-glucosamine hydrochloride, 45 parts of chondroitin sulfate, 40 parts of collagen powder, 8 parts of hydroxypropyl methylcellulose, 10 parts of sodium carboxymethyl starch and 5 parts of magnesium stearate.

[0032] Example 2 A Glucosamine Chondroitin Collagen Composition The preparation comprises the following raw materials in parts by weight: 160 parts of calcium carbonate, 150 parts of D-glucosamine hydrochloride, 40 parts of chondroitin sulfate, 30 parts of collagen powder, 5 parts of hydroxypropyl methylcellulose, 10 parts of sodium carboxymethyl starch and 2 parts of magnesium stearate.

[0033] Example 3 A Glucosamine Chondroitin Collagen Composition The preparation comprises the following raw materials in parts by weight: 200 parts of calcium carbonate, 200 parts of D-glucosamine hydrochloride, 50 parts of chondroitin sulfate, 50 parts of collagen powder, 10 parts of hydroxypropyl methylcellulose, 20 parts of sodium carboxymethyl starch and 8 parts of magnesium stearate.

[0034] Comparative Example 1 The difference from Example 1 is that the ratio of the components is not within the scope of protection of the present invention, namely: 80 parts of calcium carbonate, 150 parts of D-glucosamine hydrochloride, 120 parts of chondroitin sulfate, 80 parts of collagen powder, 15 parts of hydroxypropyl methylcellulose, 8 parts of sodium carboxymethyl starch and 15 parts of magnesium stearate.

[0035] The above Examples 1-3 and Comparative Example 1 were prepared as follows: (1) Weigh the formulated amount of calcium carbonate, D-glucosamine hydrochloride, chondroitin sulfate and collagen powder and mix them evenly. Add the formulated amount of hydroxypropyl methylcellulose and mix them. Dry at 45°C for 15 minutes, grind and sieve through 40 mesh to obtain a mixture. (2) Weighing the formulated amount of sodium carboxymethyl starch and magnesium stearate and mixing them with the mixture obtained in step (1) to obtain the product.

[0036] Comparative Example 2 The difference from Example 1 is that 40 parts of collagen powder are replaced by 40 parts of calcium carbonate, namely: 220 parts of calcium carbonate, 180 parts of D-glucosamine hydrochloride, 45 parts of chondroitin sulfate, 8 parts of hydroxypropyl methylcellulose, 10 parts of sodium carboxymethyl starch and 5 parts of magnesium stearate.

[0037] Prepare as follows: (1) Weigh the formulated amount of calcium carbonate, D-glucosamine hydrochloride and chondroitin sulfate and mix them evenly. Add the formulated amount of hydroxypropyl methylcellulose and mix them. Dry at 45°C for 15 minutes, grind and sieve through 40 mesh to obtain a mixture. (2) Weighing the formulated amount of sodium carboxymethyl starch and magnesium stearate and mixing them with the mixture obtained in step (1) to obtain the product.

[0038] Comparative Example 3 The difference from Example 1 is that 8 parts of hydroxypropyl methylcellulose and 10 parts of sodium carboxymethyl starch are replaced by 18 parts of microcrystalline cellulose.

[0039] Prepare as follows: (1) Weigh the formulated amount of calcium carbonate, D-glucosamine hydrochloride and chondroitin sulfate and mix them evenly. Add the formulated amount of microcrystalline cellulose and mix them. Dry at 45°C for 15 minutes, grind and sieve through 40 mesh to obtain a mixture. (2) Weigh the formulated amount of magnesium stearate and mix it with the mixture obtained in step (1) to obtain the product.

[0040] Application Example 1-4: A Glucosamine Chondroitin Collagen Tablet The formulations of Examples 1-3 and Comparative Example 1 were prepared as follows: (1) Calcium carbonate, D-glucosamine hydrochloride, chondroitin sulfate, collagen powder and hydroxypropyl methylcellulose in a formula amount are granulated by wet granulation. The wet granulation adopts 90 parts by weight of a wetting agent, which is 70% by volume of ethanol. The specific operating conditions of the wet granulation are as follows: The premix was stirred at 125 rpm, sheared at 1100 rpm, mixed for 5 min, the spray pressure was 0.3 MPa, the peristaltic pump speed was 7 Hz, stirred at 125 rpm, sheared at 1100 rpm, the total addition time was 10 min, and granulated for 1 min after the addition was completed; (2) After wet granulation, fluidized bed drying was performed. The specific operating conditions of fluidized bed drying were as follows: inlet air temperature was set at 65°C, material temperature was set at 40°C, and moisture content was controlled at 2%. (3) Add the formulated amount of sodium carboxymethyl starch and magnesium stearate, compress the tablets and coat the tablets. The specific steps of compressing the tablets and coating the tablets are as follows: Tablet pressing: Use high-speed rotary tablet press, average hardness 60N, tablet pressing speed 5w / h; Coating: Control the inlet air temperature to 65°C, the pot speed to 8 rpm, the atomization pressure to 0.3 MPa, the fan pressure to 0.3 MPa, the peristaltic pump speed to 25 rpm, the tablet temperature to 35°C, and the weight gain to 2% to obtain the corresponding glucosamine chondroitin collagen tablets (Application Example 1 is a tablet prepared from the composition of Example 1, Application Example 2 is a tablet prepared from the composition of Example 2, Application Example 3 is a tablet prepared from the composition of Example 3, and Application Example 4 is a tablet prepared from the composition of Comparative Example 1).

[0041] Application Example 5: A Glucosamine Chondroitin Collagen Tablet The formula of Comparative Example 2 was prepared as follows: (1) Calcium carbonate, D-glucosamine hydrochloride, chondroitin sulfate and hydroxypropyl methylcellulose in a formulated amount are granulated by a wet granulation method. The wet granulation method uses 90 parts by weight of a wetting agent, which is 70% by volume ethanol. The specific operating conditions of the wet granulation method are as follows: The premix was stirred at 125 rpm, sheared at 1100 rpm, mixed for 5 min, the spray pressure was 0.3 MPa, the peristaltic pump speed was 7 Hz, stirred at 125 rpm, sheared at 1100 rpm, the total addition time was 10 min, and granulated for 1 min after the addition was completed; (2) After wet granulation, fluidized bed drying was performed. The specific operating conditions of fluidized bed drying were as follows: inlet air temperature was set at 65°C, material temperature was set at 40°C, and moisture content was controlled at 2%. (3) Add the formulated amount of sodium carboxymethyl starch and magnesium stearate, compress the tablets and coat the tablets. The specific steps of compressing the tablets and coating the tablets are as follows: Tablet pressing: Use high-speed rotary tablet press, average hardness 60N, tablet pressing speed 5w / h; Coating: Control the inlet air temperature to 65°C, the pot speed to 8 rpm, the atomization pressure to 0.3 MPa, the fan pressure to 0.3 MPa, the peristaltic pump speed to 25 rpm, the tablet surface temperature to 35°C, and the weight gain to 2% to obtain tablets prepared from the composition of Comparative Example 2.

[0042] Application Example 6: A Glucosamine Chondroitin Collagen Tablet The formula of Comparative Example 3 was prepared as follows: (1) Calcium carbonate, D-glucosamine hydrochloride, chondroitin sulfate, collagen powder and microcrystalline cellulose in the formulated amount were granulated by wet granulation. The wet granulation used 90 parts by weight of a wetting agent, which was 70% by volume of ethanol. The specific operating conditions of the wet granulation were as follows: The premix was stirred at 125 rpm, sheared at 1100 rpm, mixed for 5 min, the spray pressure was 0.3 MPa, the peristaltic pump speed was 7 Hz, stirred at 125 rpm, sheared at 1100 rpm, the total addition time was 10 min, and granulated for 1 min after the addition was completed; (2) After wet granulation, fluidized bed drying was performed. The specific operating conditions of fluidized bed drying were as follows: inlet air temperature was set at 65°C, material temperature was set at 40°C, and moisture content was controlled at 2%. (3) Add the formulated amount of magnesium stearate, compress the tablets and coat the tablets. The specific steps of compressing the tablets and coating the tablets are as follows: Tablet pressing: Use high-speed rotary tablet press, average hardness 60N, tablet pressing speed 5w / h; Coating: Control the inlet air temperature to 65°C, the pot speed to 8 rpm, the atomization pressure to 0.3 MPa, the fan pressure to 0.3 MPa, the peristaltic pump speed to 25 rpm, the tablet surface temperature to 35°C, and the weight gain to 2% to obtain tablets prepared from the composition of Comparative Example 3.

[0043] Effect experiment (1) Quality evaluation The tablet weight of the tablets prepared in Control Application Example 1-6 was 1.0±0.05 g, and the disintegration time, hardness and friability of the tablets and the commercially available Kangenbei brand glucosamine chondroitin calcium tablets were tested respectively.

[0044] 1. Disintegration time detection Set the temperature of the disintegration instrument to 37°C. After the temperature stabilizes, take 6 pieces of the prepared glucosamine chondroitin collagen tablets and place them in the hanging basket of the disintegration instrument. Then place the hanging basket in the beaker of pure water in the disintegration instrument. Start disintegration and record the time for complete disintegration. The time taken for the glucosamine chondroitin collagen tablet to completely disintegrate is the disintegration time limit.

[0045] 2. Hardness test Take 6 pieces of the prepared glucosamine chondroitin collagen tablets and place them between the two pressure plates of the hardness tester. Slowly apply pressure along the diameter direction of the tablet. The pressure (N) when the tablet is just broken is the hardness.

[0046] 3. Friability test Take 10 glucosamine chondroitin collagen tablets respectively, blow off the powder on the tablets with a hair dryer, accurately weigh the mass m1, and place them in a fragility tester. Let them collide and rub against each other in the rotating drum. Take them out after 4 minutes, and blow off the powder on the tablets with a hair dryer again. Accurately weigh m2. The friability formula is as follows: Friability (%) = [(m1-m2) / m1)] × 100% The results are shown in Table 1 below.

[0047] Table 1

[0048] Note: *p<0.05 compared with Application Example 1.

[0049] As can be seen from the data in Table 1, changing the ratio and type of excipients can significantly reduce tablet hardness and increase tablet disintegration time and friability. This shows that choosing the right excipients and their ratio is crucial for tablet quality evaluation.

[0050] (2) Animal experiments After 7 days of acclimatization to a basal diet, SPF male SD rats were randomly divided according to body weight into a blank control group, a model group, Example 1-3 groups, and Comparative Example 1-3 groups, with 10 rats in each group. During the experiment, all groups except the blank control group were fed a low-calcium diet (purchased from Beijing Ke'ao Xieli Feed Co., Ltd.). The compositions prepared in Examples 1-3 and Comparative Example 1-3 were administered orally at a dose of 2.0 g / kg. The blank control group and the model group were administered orally with an equal amount of distilled water once daily for 90 consecutive days. Body weight was measured weekly, and the dose adjusted based on body weight.

[0051] After the experiment, the rats were killed, and the left femur was removed and baked in a 105°C oven until constant weight was measured. The bone weight was then measured using a DPX-L dual-energy X-ray absorptiometry system to scan the entire left femur and determine the bone density (g / cm 2 The results are shown in Table 2.

[0052] Table 2

[0053] Note: Compared with Example 1, *p<0.05.

[0054] As can be seen from the data in Table 2, changing the ratio of calcium carbonate, D-glucosamine hydrochloride, chondroitin sulfate, and collagen powder or lacking one of the components will affect the effect of the composition in improving bone density. Only when the components of the present invention are used and the ratio is within the scope of the present invention can the ideal effect be achieved.

[0055] The above detailed description is a specific description of one feasible embodiment of the present invention. This embodiment is not intended to limit the patent scope of the present invention. Any equivalent implementation or modification that does not depart from the present invention should be included in the scope of the technical solution of the present invention.

Claims

1. A glucosamine chondroitin collagen composition for improving bone and joint function, characterized in that: The preparation comprises the following raw materials in parts by weight: 160-200 parts of calcium carbonate, 150-200 parts of D-glucosamine hydrochloride, 40-50 parts of chondroitin sulfate, 30-50 parts of collagen powder, 5-10 parts of hydroxypropyl methylcellulose, 10-20 parts of sodium carboxymethyl starch and 2-8 parts of magnesium stearate.

2. The glucosamine chondroitin collagen composition according to claim 1, characterized in that The mass ratio of the D-glucosamine hydrochloride to chondroitin sulfate is 3-5:

1.

3. The glucosamine chondroitin collagen composition according to claim 1, characterized in that The mass ratio of the calcium carbonate to the collagen powder is 4-6:

1.

4. The glucosamine chondroitin collagen composition according to claim 1, characterized in that The preparation comprises the following raw materials in parts by weight: 180 parts of calcium carbonate, 180 parts of D-glucosamine hydrochloride, 45 parts of chondroitin sulfate, 40 parts of collagen powder, 8 parts of hydroxypropyl methylcellulose, 10 parts of sodium carboxymethyl starch and 5 parts of magnesium stearate.

5. The method for preparing the glucosamine chondroitin collagen composition according to any one of claims 1 to 4, characterized in that: The following steps are involved: (1) Weigh the formulated amount of calcium carbonate, D-glucosamine hydrochloride, chondroitin sulfate and collagen powder, mix them evenly, add the formulated amount of hydroxypropyl methylcellulose, mix, dry, grind and sieve to obtain a mixture; (2) Weighing the formulated amount of sodium carboxymethyl starch and magnesium stearate and mixing them with the mixture obtained in step (1) to obtain the product.

6. Use of the glucosamine chondroitin collagen composition according to any one of claims 1 to 4 or the glucosamine chondroitin collagen composition prepared by the preparation method according to claim 5 in the preparation of a body-building product.

7. The use according to claim 6, characterized in that The product is a health food.

8. The use according to claim 6, characterized in that The dosage form of the product is tablet, capsule, granule or oral solution.

9. A glucosamine chondroitin collagen tablet, characterized in that: The invention comprises the glucosamine chondroitin collagen composition according to any one of claims 1 to 4 or the glucosamine chondroitin collagen composition prepared by the preparation method according to claim 5.

10. The tablet according to claim 9, characterized in that The preparation method of the tablet comprises the following steps: (1) Weigh the formulated amount of calcium carbonate, D-glucosamine hydrochloride, chondroitin sulfate, collagen powder and hydroxypropyl methylcellulose, mix them, and granulate the mixture; (2) Drying after granulation; (3) After drying, add the formulated amount of magnesium stearate and sodium carboxymethyl starch for tableting and coating.

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