Microcrystalline cellulose as a tablet excipient, its preparation method and use

CN119101172BActive Publication Date: 2026-09-11QILU UNIVERSITY OF TECHNOLOGY (SHANDONG ACADEMY OF SCIENCES)
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Patent Information

Application Number
CN202411257159.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-09-09
Publication Date
2026-09-11
Estimated Expiration
2044-09-09

AI Technical Summary

Technical Problem

发明人发现,现有微晶纤维素的制备工艺获得的微晶纤维素用于片剂辅料时,获得的片剂硬度不佳,而且脆碎度较高,甚至大于1%;而片剂硬度的提升一般会导致崩解时间的延长

Benefits of technology

[0022]This invention first improves the uniformity of short fibers through sieving, then pretreats the short fibers using ultrasound at a specific power, which improves the fiber's water retention value and specific surface area, increases the accessibility of chemical reagents to the short fibers during acid hydrolysis, and significantly affects the final microcrystalline cellulose particle size and crystallinity. Subsequently, the fibers are acid-hydrolyzed to prepare microcrystalline cellulose. The obtained microcrystalline cellulose has a small particle size, with a median diameter (D50) of less than 40 μm, and high crystallinity, exceeding 75%. When the microcrystalline cellulose prepared by this invention is directly compressed into ibuprofen tablets, the ibuprofen tablets exhibit low friability (less than 0.6%) and high hardness (greater than 60 N), while the disintegration time is less than 1300 s and the dissolution rate is greater than 50%, showing good application prospects.

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Abstract

The application discloses microcrystalline cellulose used as a tablet excipient and a preparation method and application thereof, and belongs to the technical field of microcrystalline cellulose preparation. The preparation method comprises the following steps: dispersing dissolving pulp in water, defibrating, screening and drying to obtain short fibers; dispersing the short fibers in water and performing ultrasonic treatment, wherein the ultrasonic frequency is 20-30 kHz, the ultrasonic power is 350-650 W, and the ultrasonic treatment time is 3-10 min; performing acid hydrolysis on the short fibers after the ultrasonic treatment, then filtering, washing the filter residue and drying, and thus the microcrystalline cellulose is obtained. The microcrystalline cellulose obtained by the application has small particle size and high crystallinity; when the microcrystalline cellulose obtained by the preparation method is directly used for tablet compression to prepare ibuprofen tablets, the ibuprofen tablets exhibit low friability, high hardness, short disintegration time and high dissolution rate, and have a good application prospect.
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Description

Technical Field

[0001] This invention relates to the field of microcrystalline cellulose preparation technology, and in particular to a microcrystalline cellulose used as a tablet excipient, its preparation method, and its application. Background Technology

[0002] The information disclosed in the background section of this invention is intended only to enhance the understanding of the overall background of the invention and is not necessarily to be construed as an admission or in any way implying that such information constitutes prior art known to those skilled in the art.

[0003] Microcrystalline cellulose is a cellulose derivative obtained by hydrolyzing cellulose. As a natural polymer material, it is widely used as an excipient in the preparation of drug tablets. It mainly acts as a filler, and can also play a role in lubrication, flow aid, disintegration and adhesion. It can reduce the friction between drug particles, improve the flowability of drug particles, and facilitate tablet formation.

[0004] For tablets, not only is a suitable disintegration time necessary, but also high hardness and low friability are required to prevent damage during transportation and use, ensuring the quality and stability of the drug. However, current methods often focus on optimizing the tablet forming process, lacking research on controlling the properties of the excipients themselves. The inventors discovered that when microcrystalline cellulose prepared using existing processes is used as a tablet excipient, the resulting tablets have poor hardness and high friability, even exceeding 1%; and increasing tablet hardness generally leads to a prolonged disintegration time.

[0005] Therefore, how to provide a method for preparing microcrystalline cellulose so that the prepared microcrystalline cellulose can produce tablets with high hardness and low brittleness, as well as short disintegration time when used as a tablet excipient is an urgent problem to be solved. Summary of the Invention

[0006] In view of this, the present invention provides a microcrystalline cellulose for use as a tablet excipient, a method for its preparation, and its application. When the microcrystalline cellulose provided by the present invention is used as an excipient to prepare tablets, it can make the tablets have high hardness and low brittleness, while having a short disintegration time.

[0007] In a first aspect, the present invention provides a method for preparing microcrystalline cellulose for use as a tablet excipient, comprising the following steps:

[0008] The dissolving pulp is dispersed in water, then loosened, sieved, and dried to obtain short fibers;

[0009] Short fibers were dispersed in water and subjected to ultrasonic treatment at a frequency of 20–30 kHz, an ultrasonic power of 350–650 W, and a treatment time of 3–10 min.

[0010] The short fibers after ultrasonic treatment are acid-hydrolyzed, then filtered, the filter residue is washed and dried to obtain the final product.

[0011] Preferably, the α-cellulose content of the dissolving pulp is above 95%; and the mesh size of the short fibers is 50 to 100 mesh.

[0012] Preferably, in the step of dispersing short fibers in water and performing ultrasonic treatment, the mass fraction of the short fibers is 0.5 to 2 wt%.

[0013] Preferably, the temperature of the ultrasonic treatment is 0 to 5°C.

[0014] Preferably, the acid hydrolysis step specifically involves placing the short fibers in an inorganic acid solution and stirring and hydrolyzing at 80–90°C for 50–70 minutes.

[0015] Furthermore, the inorganic acid is selected from hydrochloric acid, sulfuric acid, or nitric acid, and the concentration of the inorganic acid solution is 3-5 wt%.

[0016] Furthermore, the ratio of the short fiber to the inorganic acid solution is 1g:(20-40)mL; the stirring speed is 100-500rpm.

[0017] Preferably, in the step of washing and drying the filter residue, the filter residue is washed with hot water at 95-100°C, and the drying method is freeze drying.

[0018] Secondly, the present invention provides a microcrystalline cellulose for use as a tablet excipient, obtained by the above-described preparation method.

[0019] Thirdly, the present invention provides the application of the microcrystalline cellulose used as a tablet excipient in the preparation of ibuprofen tablets, wherein the ibuprofen tablets, by mass percentage, mainly comprise: 32-38% microcrystalline cellulose used as a tablet excipient, 15-25% ibuprofen, 1-3% magnesium stearate, 2-4% talc, 1-3% steviol glycoside, 2-4% corn starch, and the balance being lactose;

[0020] The preparation method of the ibuprofen tablets is as follows: grind and mix the components thoroughly according to the proportion, and compress them into tablets using the direct compression method.

[0021] Compared with the prior art, the present invention has achieved the following beneficial effects:

[0022] This invention first improves the uniformity of short fibers through sieving, then pretreats the short fibers using ultrasound at a specific power, which improves the fiber's water retention value and specific surface area, increases the accessibility of chemical reagents to the short fibers during acid hydrolysis, and significantly affects the final microcrystalline cellulose particle size and crystallinity. Subsequently, the fibers are acid-hydrolyzed to prepare microcrystalline cellulose. The obtained microcrystalline cellulose has a small particle size, with a median diameter (D50) of less than 40 μm, and high crystallinity, exceeding 75%. When the microcrystalline cellulose prepared by this invention is directly compressed into ibuprofen tablets, the ibuprofen tablets exhibit low friability (less than 0.6%) and high hardness (greater than 60 N), while the disintegration time is less than 1300 s and the dissolution rate is greater than 50%, showing good application prospects. Detailed Implementation

[0023] It should be noted that the following detailed descriptions are exemplary and intended to provide further illustration of the invention. Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.

[0024] This invention provides a method for preparing microcrystalline cellulose for use as a tablet excipient, comprising the following steps:

[0025] The dissolving pulp is dispersed in water, then loosened, sieved, and dried to obtain short fibers;

[0026] Short fibers were dispersed in water and subjected to ultrasonic treatment at a frequency of 20–30 kHz, an ultrasonic power of 350–650 W, and a treatment time of 3–10 min.

[0027] The short fibers after ultrasonic treatment are acid-hydrolyzed, then filtered, the filter residue is washed and dried to obtain the final product.

[0028] This invention uses dissolving pulp as a raw material for preparing microcrystalline cellulose. It has high fiber whiteness, uniform molecular weight, low ash content, and good reactivity, making it suitable for preparing microcrystalline cellulose. This invention does not impose special restrictions on the specific source of the dissolving pulp; commonly used dissolving pulps in the art can be used. Preferably, the α-cellulose content of the dissolving pulp in this invention is above 95%, which is more conducive to the preparation of microcrystalline cellulose.

[0029] This invention does not impose special limitations on the processes of delamination, sieving, and drying; commonly used methods in the art for delamination, sieving, and drying can be employed. These steps yield short fibers with uniform particle size, which is beneficial for subsequent reactions and the final properties of the microcrystalline cellulose. In this invention, the mesh size of the short fibers is preferably 50-100 mesh.

[0030] In this invention, in the step of dispersing short fibers in water for ultrasonic treatment, the mass fraction of the short fibers is 0.5–2 wt%. A suitable concentration allows for sufficient dispersion of the short fibers, which is beneficial for absorbing the energy released by ultrasonic waves.

[0031] In this invention, the temperature of the ultrasonic treatment is 0–5°C. Controlling the temperature within this range can prevent the ultrasonic waves from causing excessively high temperatures that could adversely affect the fibers themselves.

[0032] This invention preferably uses an ultrasonic probe to provide ultrasound, which can generate a significant cavitation effect. The ultrasonic power of this invention is further preferably 350–550 W, more preferably 430–470 W; the ultrasonic treatment time is further preferably 4–6 min. Ultrasonic power has a significant impact on the final properties of the microcrystalline cellulose. If the ultrasonic power is too low, its effect on improving the final properties of the microcrystalline cellulose is not significant; if the ultrasonic power is too high, it will cause some damage to the structure of the microcrystalline cellulose, thus affecting its subsequent performance. Therefore, a suitable ultrasonic treatment power can give the microcrystalline cellulose suitable morphology, particle size, and crystallinity, thereby improving the hardness and dissolution rate of tablets when used as a filler excipient, reducing friability, and shortening disintegration time.

[0033] The ultrasonic process of the present invention is carried out before acid hydrolysis, which can effectively avoid corrosion of ultrasonic equipment. On the other hand, the short fibers treated by ultrasound have better reaction accessibility and can improve the reaction degree of the acid hydrolysis process.

[0034] In this invention, the acid hydrolysis step specifically involves placing the short fibers in an inorganic acid solution and stirring at 80–90°C for 50–70 minutes. The inorganic acid is selected from hydrochloric acid, sulfuric acid, or nitric acid, with hydrochloric acid being preferred in this invention. The concentration of the inorganic acid solution is 3–5 wt%, more preferably 4 wt%.

[0035] In this invention, the ratio of the short fiber to the inorganic acid solution is 1g:(20-40)mL; the stirring speed is 100-500rpm, more preferably 100-300rpm.

[0036] In the step of washing and drying the filter residue described in this invention, the filter residue is washed with hot water at 95-100°C, and the drying method is freeze-drying. This invention does not impose any special limitations on the method of washing the filter residue with hot water or the specific steps of freeze-drying; steps commonly used in the art can be employed.

[0037] The present invention also provides a microcrystalline cellulose for use as a tablet excipient, obtained by the above preparation method, having a degree of polymerization of 160-180, a median diameter (D50) of 35-40 μm, and a crystallinity of 75.5-77%.

[0038] The present invention also provides the application of the above-mentioned microcrystalline cellulose used as a tablet excipient in the preparation of ibuprofen tablets, wherein the ibuprofen tablets, by mass percentage, mainly comprise: 32-38% microcrystalline cellulose used as a tablet excipient, 15-25% ibuprofen, 1-3% magnesium stearate, 2-4% talc, 1-3% steviol glycoside, 2-4% corn starch, and the balance being lactose;

[0039] The preparation method of the ibuprofen tablets is as follows: grind and mix the components thoroughly according to the proportion, and compress them into tablets using the direct compression method.

[0040] In this invention, the pressure of the tablet is 8-12 MPa, more preferably 10 MPa.

[0041] The prepared ibuprofen tablets have a hardness greater than 60 N, a disintegration time less than 1300 s, a friability of less than 0.6%, and a dissolution rate greater than 50%.

[0042] The technical solution of the present invention will be further described below with reference to specific embodiments.

[0043] Example 1

[0044] This embodiment provides a method for preparing microcrystalline cellulose.

[0045] (1) Weigh 500g of dried coniferous wood dissolving pulp board, tear it into pieces and disperse it in water. After soaking for 24 hours, the pulp is loosened and the fibers are sieved using a Pall sieve to obtain 50-100 mesh short fibers.

[0046] (2) The short fibers obtained in step (1) were spun dry and transferred to a sealed bag to balance the moisture content. The short fibers were then characterized as follows: average fiber length was 0.690 mm, average fiber width was 31.3 μm, crystallinity was 72.63%, water retention value was 0.9109 g / g, and specific surface area was 4.1911 m². 2 / g.

[0047] (3) Weigh 3.0 g (oven-dry) of the short fibers obtained in step (2), place them in a 500 mL jacketed beaker, add a certain amount of deionized water to make the short fiber mass fraction 1 wt%, and place them in an ultrasonic cell disruptor for reaction. An external intelligent energy-saving constant temperature bath was connected, the ultrasonic frequency was fixed at 25 kHz, the treatment temperature at 0℃, the reaction time at 5 min, and the ultrasonic power at 360 W. After ultrasonic treatment, the moisture content was balanced, and characterization analysis was performed. After ultrasonic pretreatment, the water retention value of the short fibers was 1.1743 g / g, and the specific surface area was 6.1532 m². 2 / g.

[0048] (4) Weigh 2.0 g (oven dry) of the short fibers obtained in step (3) and place them in a reaction vessel. Add hydrochloric acid and deionized water to the reaction vessel, wherein the amount of hydrochloric acid is 4 wt% and the solid-liquid ratio is 1 g: 30 mL. The reaction is carried out in a heat-collecting constant temperature magnetic stirrer at a reaction temperature of 85 °C for 60 min.

[0049] (5) The reaction mixture obtained in step (4) was rapidly cooled, filtered with a G4 sand core funnel, and the solid hydrolysis product was thoroughly washed with hot water until neutral. The obtained solid hydrolysis product was freeze-dried for 48 hours to obtain microcrystalline cellulose.

[0050] Results: The degree of polymerization of the obtained microcrystalline cellulose was 181, the D50 was 39.0 μm, and the crystallinity was 75.97%.

[0051] Example 2

[0052] This embodiment provides a method for preparing microcrystalline cellulose.

[0053] (1) Weigh 500g of dried coniferous wood dissolving pulp board, tear it into pieces and disperse it in water. After soaking for 24 hours, the pulp is loosened and the fibers are sieved using a Pall sieve to obtain 50-100 mesh short fibers.

[0054] (2) The short fibers obtained in step (1) were spun dry and transferred to a sealed bag to balance the moisture content. The short fibers were then characterized as follows: average fiber length was 0.690 mm, average fiber width was 31.3 μm, crystallinity was 72.63%, water retention value was 0.9109 g / g, and specific surface area was 4.1911 m². 2 / g.

[0055] (3) Weigh 3.0 g (oven-dry) of the short fibers obtained in step (2), place them in a 500 mL jacketed beaker, add a certain amount of deionized water to make the short fiber mass fraction 1 wt%, and place them in an ultrasonic cell disruptor for reaction. An external intelligent energy-saving constant temperature bath was connected, the ultrasonic frequency was fixed at 25 kHz, the treatment temperature at 0℃, the reaction time at 5 min, and the ultrasonic power at 450 W. After ultrasonic treatment, the moisture content was balanced, and the fibers were characterized and analyzed. After ultrasonic pretreatment, the water retention value of the short fibers was 1.2549 g / g, and the specific surface area was 6.9369 m². 2 / g.

[0056] (4) Weigh 2.0 g (oven dry) of the short fibers obtained in step (3) and place them in a reaction vessel. Add hydrochloric acid and deionized water to the reaction vessel, wherein the amount of hydrochloric acid is 4 wt% and the solid-liquid ratio is 1 g: 30 mL. The reaction is carried out in a heat-collecting constant temperature magnetic stirrer at a reaction temperature of 85 °C for 60 min.

[0057] (5) The reaction mixture obtained in step (4) was rapidly cooled, filtered with a G4 sand core funnel, and the solid hydrolysis product was thoroughly washed with hot water until neutral. The obtained solid hydrolysis product was freeze-dried for 48 hours to obtain microcrystalline cellulose.

[0058] Example 3

[0059] This embodiment provides a method for preparing microcrystalline cellulose.

[0060] (1) Weigh 500g of dried coniferous wood dissolving pulp board, tear it into pieces and disperse it in water. After soaking for 24 hours, the pulp is loosened and the fibers are sieved using a Pall sieve to obtain 50-100 mesh short fibers.

[0061] (2) The short fibers obtained in step (1) were spun dry and transferred to a sealed bag to balance the moisture content. The short fibers were then characterized as follows: average fiber length was 0.690 mm, average fiber width was 31.3 μm, crystallinity was 72.63%, water retention value was 0.9109 g / g, and specific surface area was 4.1911 m². 2 / g.

[0062] (3) Weigh 3.0 g (oven-dry) of the short fibers obtained in step (2), place them in a 500 mL jacketed beaker, add a certain amount of deionized water to make the short fiber mass fraction 1 wt%, and place them in an ultrasonic cell disruptor for reaction. An external intelligent energy-saving constant temperature bath was connected, the ultrasonic frequency was fixed at 25 kHz, the treatment temperature at 0℃, the reaction time at 5 min, and the ultrasonic power at 540 W. After ultrasonic treatment, the moisture content was balanced, and the fibers were characterized and analyzed. After ultrasonic pretreatment, the water retention value of the short fibers was 1.3686 g / g, and the specific surface area was 7.9751 m². 2 / g.

[0063] (4) Weigh 2.0 g (oven dry) of the short fibers obtained in step (3) and place them in a reaction vessel. Add hydrochloric acid and deionized water to the reaction vessel, wherein the amount of hydrochloric acid is 4 wt% and the solid-liquid ratio is 1 g: 30 mL. The reaction is carried out in a heat-collecting constant temperature magnetic stirrer at a reaction temperature of 85 °C for 60 min.

[0064] (5) The reaction mixture obtained in step (4) was rapidly cooled, filtered with a G4 sand core funnel, and the solid hydrolysis product was thoroughly washed with hot water until neutral. The obtained solid hydrolysis product was freeze-dried for 48 hours to obtain microcrystalline cellulose.

[0065] Example 4

[0066] This embodiment provides a method for preparing microcrystalline cellulose.

[0067] (1) Weigh 500g of dried coniferous wood dissolving pulp board, tear it into pieces and disperse it in water. After soaking for 24 hours, the pulp is loosened and the fibers are sieved using a Pall sieve to obtain 50-100 mesh short fibers.

[0068] (2) The short fibers obtained in step (1) were spun dry and transferred to a sealed bag to balance the moisture content. The short fibers were then characterized as follows: average fiber length was 0.690 mm, average fiber width was 31.3 μm, crystallinity was 72.63%, water retention value was 0.9109 g / g, and specific surface area was 4.1911 m². 2 / g.

[0069] (3) Weigh 3.0 g (oven-dry) of the short fibers obtained in step (2), place them in a 500 mL jacketed beaker, add a certain amount of deionized water to make the short fiber mass fraction 1 wt%, and place them in an ultrasonic cell disruptor for reaction. An external intelligent energy-saving constant temperature bath was connected, the ultrasonic frequency was fixed at 25 kHz, the treatment temperature at 0℃, the reaction time at 5 min, and the ultrasonic power at 630 W. After ultrasonic treatment, the moisture content was balanced, and the cells were characterized and analyzed. After ultrasonic pretreatment, the water retention value of the short fibers was 1.3742 g / g, and the specific surface area was 8.6879 m². 2 / g.

[0070] (4) Weigh 2.0 g (oven dry) of the short fibers obtained in step (3) and place them in a reaction vessel. Add hydrochloric acid and deionized water to the reaction vessel, wherein the amount of hydrochloric acid is 4 wt% and the solid-liquid ratio is 1 g: 30 mL. The reaction is carried out in a heat-collecting constant temperature magnetic stirrer at a reaction temperature of 85 °C for 60 min.

[0071] (5) The reaction mixture obtained in step (4) was rapidly cooled, filtered with a G4 sand core funnel, and the solid hydrolysis product was thoroughly washed with hot water until neutral. The obtained solid hydrolysis product was freeze-dried for 48 hours to obtain microcrystalline cellulose.

[0072] Comparative Example 1

[0073] Compared to Example 1, this comparative example did not undergo ultrasonic treatment. The specific steps are as follows:

[0074] (1) Weigh 500g of dried coniferous wood dissolving pulp board, tear it into pieces and disperse it in water. After soaking for 24 hours, the pulp is loosened and the fibers are sieved using a Pall sieve to obtain 50-100 mesh short fibers.

[0075] (2) The short fibers obtained in step (1) were spun dry and transferred to a sealed bag to balance the moisture content. The short fibers were then characterized as follows: average fiber length was 0.690 mm, average fiber width was 31.3 μm, crystallinity was 72.63%, water retention value was 0.9109 g / g, and specific surface area was 4.1911 m². 2 / g.

[0076] (3) Weigh 2.0 g (oven dry) of the short fibers obtained in step (2) and place them in a reaction vessel. Add hydrochloric acid and deionized water to the reaction vessel, wherein the amount of hydrochloric acid is 4 wt% and the solid-liquid ratio is 1 g: 30 mL. The reaction is carried out in a heat-collecting constant temperature magnetic stirrer at a reaction temperature of 85 °C for 60 min.

[0077] (5) The reaction mixture obtained in step (4) was rapidly cooled, filtered with a G4 sand core funnel, and the solid hydrolysis product was thoroughly washed with hot water until neutral. The obtained solid hydrolysis product was freeze-dried for 48 hours to obtain microcrystalline cellulose.

[0078] Comparative Example 2

[0079] Compared to Example 1, the ultrasonic power of this comparative example is 180W.

[0080] Comparative Example 3

[0081] Compared to Example 1, the ultrasonic power of this comparative example is 270W.

[0082] Application examples

[0083] Using microcrystalline cellulose from Examples 1-4 and Comparative Examples 1-3 as pharmaceutical excipients, ibuprofen tablets were prepared according to the following formulation: by mass fraction, microcrystalline cellulose 35%, lactose 35%, ibuprofen 20%, magnesium stearate 2%, talc 3%, steviol 2%, and corn starch 3%; the preparation method was as follows: all components were thoroughly ground and mixed, and tablets were compressed using the direct compression method at a compression pressure of 10 MPa, with the tablet weight controlled at 200 mg.

[0084] The properties of the microcrystalline cellulose of Examples 1-4 and Comparative Examples 1-3, as well as the prepared ibuprofen tablets, were determined, and the results are shown in Table 1.

[0085] Table 1 Performance data of microcrystalline cellulose and ibuprofen tablets

[0086]

[0087] As shown in Table 1, without ultrasonic treatment, the crystallinity of microcrystalline cellulose is 73.25%, the particle size D50 is 42.9 μm, the resulting tablets have a hardness below 50 N, a long disintegration time of 1473 s, high friability, and a dissolution rate of only 48.75%. Lower ultrasonic treatment power (below 300 W) has less impact on the properties of microcrystalline cellulose and tablets. When the ultrasonic treatment power reaches above 360 ​​W, the particle size D50 of microcrystalline cellulose is below 40 μm, the crystallinity reaches above 75.5%, and the tablet hardness remains above 60 N, the friability is below 0.6%, and the disintegration time is within 1260 s. When the ultrasonic treatment power is 450 W, the prepared microcrystalline cellulose has the highest crystallinity, the lowest tablet friability (below 0.5%), the highest hardness (above 70 N), and a short disintegration time. As the ultrasonic power continued to increase, the particle size and degree of polymerization of microcrystalline cellulose continued to decrease, but the crystallinity also decreased, resulting in a decrease in the hardness of the tablets and an increase in brittleness.

[0088] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for preparing microcrystalline cellulose for use as a tablet excipient, characterized in that, Includes the following steps: The dissolving pulp is dispersed in water, then loosened, sieved, and dried to obtain short fibers; the α-cellulose content of the dissolving pulp is above 95%; and the mesh size of the short fibers is 50-100 mesh. Short fibers were dispersed in water and subjected to ultrasonic treatment. The mass fraction of the short fibers was 0.5~2wt%, the ultrasonic frequency was 20~30kHz, the ultrasonic power was 430~470W, and the ultrasonic treatment time was 3~10min. The short fibers after ultrasonic treatment are acid-hydrolyzed, then filtered, the filter residue is washed and dried to obtain the final product. The acid hydrolysis step specifically involves placing the short fibers in an inorganic acid solution and stirring at 80-90°C for 50-70 minutes. The concentration of the inorganic acid solution is 3-5 wt%. The microcrystalline cellulose obtained by the above preparation method has a degree of polymerization of 160~180, a median diameter D50 of 35~40μm, and a crystallinity of 75.5~77%.

2. The preparation method according to claim 1, characterized in that, The temperature for ultrasonic treatment is 0~5℃.

3. The preparation method according to claim 1, characterized in that, The inorganic acid is selected from hydrochloric acid, sulfuric acid, or nitric acid.

4. The preparation method according to claim 1, characterized in that, The ratio of the short fiber to the inorganic acid solution is 1g:(20~40)mL; the stirring speed is 100~500rpm.

5. The preparation method according to claim 1, characterized in that, In the step of washing and drying the filter residue, hot water at 95~100℃ is used to wash the filter residue, and the drying method is freeze drying.

6. A microcrystalline cellulose for use as a tablet excipient, characterized in that, Obtained by the preparation method according to any one of claims 1 to 5.

7. The use of microcrystalline cellulose as a tablet excipient as described in claim 6 in the preparation of ibuprofen tablets, characterized in that, The ibuprofen tablets, by weight percentage, mainly comprise: 32-38% microcrystalline cellulose used as tablet excipients, 15-25% ibuprofen, 1-3% magnesium stearate, 2-4% talc, 1-3% steviol glycoside, 2-4% corn starch, with the remainder being lactose. The preparation method of the ibuprofen tablets is as follows: grind and mix the components thoroughly according to the proportion, and compress them into tablets using the direct compression method.

Citation Information

Patent Citations

  • Method for preparing microcrystalline cellulose from short fibers, microcrystalline cellulose and application of microcrystalline cellulose

    CN117285656A