Sunflower disc holocellulose, preparation method and application of sunflower disc holocellulose as disintegrating agent

Abstract

The invention discloses sunflower disc holocellulose, a preparation method and application of the sunflower disc holocellulose as a disintegrating agent, and belongs to the technical field of pharmaceutic adjuvants. The preparation method comprises the following steps: crushing sunflower heads, sieving, degreasing to obtain sunflower head powder, mixing the sunflower head powder with an alkali solution, and extracting; and bleaching the washed and dried filter residues, washing, drying, and modifying with a biological enzyme to obtain the sunflower disc holocellulose disintegrating agent. The disintegrant is prepared from agricultural wastes as raw materials through alkali extraction, bleaching, enzyme modification and other processes, the sunflower disc holocellulose is used as an efficient pharmaceutical adjuvant disintegrant, rapid disintegration of tablets such as orally disintegrating tablets and the like can be achieved, the disintegration effect can be equivalent to that of commercially available efficient disintegrants, and high-value utilization of the agricultural wastes is achieved. The prepared disintegrating agent is high in water absorption performance, good in expansion performance, good in biocompatibility and environment-friendly, and has important practical significance for fully utilizing biomass resources and solving the problem of medicine auxiliary material sources.

Description

Technical Field

[0001] The invention belongs to the technical field of pharmaceutical excipients, and particularly relates to a novel and highly efficient sunflower disk holocellulose, a preparation method and an application of the sunflower disk holocellulose as a disintegrant. Background Art

[0002] Sunflower, a commercially cultivated plant in the Asteraceae family, is one of the world's four most widely used oilseed crops for oil production. During the annual harvest season, many people discard or incinerate the sunflower heads after removing the seeds, ignoring their rich lignocellulose resources. This waste of resources and environmental pollution results.

[0003] Lignocellulose is nature's most abundant renewable resource, primarily composed of cellulose, hemicellulose, and lignin. According to research reports, approximately 181.5 billion tons of lignocellulose are produced annually globally, while only 8.2 billion tons are utilized, representing a significant waste of resources. my country, a major agricultural producer, possesses abundant lignocellulose reserves, yet utilization remains low. Extracting cellulose from lignocellulose plant matrices can mitigate environmental concerns and promote sustainable economic and social development.

[0004] Holocellulose is extracted from natural plant lignocellulose through a delignification process. It is a mixture of cellulose and hemicellulose. Because the product retains a large portion of the hemicellulose, it exhibits excellent water-swelling properties. Recent studies have shown that cellulose and hemicellulose materials extracted from various plants have great potential for application in the food and pharmaceutical industries. However, no reports have been found on holocellulose from sunflower discs.

[0005] Chinese patent CN101810269B provides a method for preparing highland barley dietary microcrystalline fiber. The highland barley dietary microcrystalline fiber extracted by this method can be used as a pharmaceutical disintegrant, but there is no modification step to further improve its physical and chemical properties. Chinese patent CN118005446A provides a method for preparing a fertilizer disintegrant from rice straw. This method further prepares rice straw holocellulose into sodium carboxymethyl cellulose. The process is complex, has certain equipment requirements, and has a high preparation cost. "Effect of rice straw holocellulose on the disintegration performance of aspirin tablets" (Li Shuangfeng et al., Journal of Chemical Industry and Engineering, 2019, 70(11): 4420-4427.) extracted rice straw holocellulose, but compared with commercially available microcrystalline cellulose, the performance improvement was limited. Summary of the Invention

[0006] In view of this, the object of the present invention is to provide a novel and highly efficient sunflower holocellulose, a preparation method and an application thereof as a disintegrant.

[0007] The present invention crushes, sieves, and defattes sunflower disks to obtain sunflower disk powder, and mixes the sunflower disk powder with an alkaline solution for extraction; takes the washed and dried filter residue for bleaching treatment, and after washing and drying, it is modified by biological enzymes to obtain the product sunflower disk holocellulose disintegrant. The present application adopts agricultural waste as raw material and is prepared through processes such as alkali extraction, bleaching, and enzyme modification. By using sunflower disk holocellulose as a high-efficiency pharmaceutical excipient disintegrant, it can achieve rapid disintegration of tablets such as orally disintegrating tablets, and the disintegration effect can be comparable to that of commercially available high-efficiency disintegrants, so that agricultural waste is utilized in a high-value manner. The prepared disintegrant has high water absorption performance, good expansion performance, good biocompatibility, and is environmentally friendly, and has important practical significance for making full use of biomass resources and solving the problem of the source of pharmaceutical excipients.

[0008] The method for preparing sunflower disk holocellulose of the present invention comprises the following steps:

[0009] (1) pre-treating sunflower discs to obtain sunflower disc powder;

[0010] (2) placing the sunflower disk powder obtained in step (1) in an alkaline solution for alkaline extraction, filtering the resulting filter residue, washing it with deionized water until it is neutral, and drying it to obtain an alkaline extraction product;

[0011] (3) placing the alkali extraction product obtained in step (2) in a bleaching aqueous solution for bleaching reaction, filtering the resulting filter residue and washing it with deionized water at 50 to 70° C. until it is neutral, then washing it with anhydrous ethanol and acetone for 3 to 5 times respectively, and drying it to obtain a bleached product;

[0012] (4) The bleached product obtained in step (3) is prepared into an acidic solution, and then a biological enzyme is added to perform an enzyme modification reaction under sealed heating and stirring. After the enzyme is inactivated, the filter is filtered, and the obtained filter residue is washed with deionized water until neutral, and then washed with 75% by mass ethanol and anhydrous ethanol for 3 to 5 times respectively, and dried to obtain the sunflower disk holocellulose.

[0013] Preferably, the pretreatment method in step (1) is as follows: fresh sunflower discs are deseeded, air-dried, and crushed into powder that can pass through a 20-40 mesh standard sieve; the obtained powder is soaked in petroleum ether for 10-12 hours for defatting, with the ratio of powder mass to petroleum ether volume being 1 g: 5-15 mL; after defatting, vacuum filtration is performed, and the sunflower disc powder is obtained after drying;

[0014] Preferably, the alkaline solution in step (2) is one of a NaOH aqueous solution and a KOH aqueous solution;

[0015] Preferably, during the alkaline solution extraction process in step (2), the material-liquid ratio of sunflower disc powder to alkaline solution is 1 g: 15-25 mL, the mass concentration of the alkaline solution is 1-5%; the extraction temperature is 50-70° C., and the extraction time is 30-90 min;

[0016] Preferably, the bleaching reaction in step (3) is carried out under sealed heating and stirring, and the bleaching method is one of acidic sodium chlorite bleaching method and alkaline hydrogen peroxide bleaching method;

[0017] Preferably, the mass concentration of the sodium chlorite aqueous solution in the acidic sodium chlorite bleaching method is 10-20 g / L, and the reaction pH condition is 4-5;

[0018] Preferably, the mass fraction of the hydrogen peroxide aqueous solution in the alkaline hydrogen peroxide bleaching method is 3-5%, and the reaction pH condition is 9-10;

[0019] Preferably, in the bleaching treatment of step (3), the solid-liquid ratio of the alkali extraction product to the bleaching aqueous solution is 1 g: 10-25 mL, the bleaching temperature is 70-100° C., and the bleaching time is 60-120 min;

[0020] Preferably, the enzyme modification reaction in step (4) is carried out under sealed heating and stirring;

[0021] Preferably, in step (4), the bleaching product is prepared into an acidic solution by mixing the bleaching product with a citric acid-sodium citrate buffer solution having a pH of 4 to 5, and the material-liquid ratio of the bleaching product to the citric acid-sodium citrate buffer solution is 1 g: 10 to 20 mL;

[0022] Preferably, the biological enzyme used in step (4) is at least one of cellulase and xylanase;

[0023] Preferably, when the cellulase and xylanase are used in combination, the mass ratio of the cellulase to the xylanase is 1:1-4;

[0024] Preferably, the total amount of the biological enzyme added in step (4) is 1.0-5.0% of the mass of the bleached product, the modification temperature is 40-60° C., and the modification time is 30-90 min;

[0025] Preferably, in step (4), the enzyme is inactivated in a boiling water bath at 100° C. for 4 to 6 minutes;

[0026] Preferably, the drying method in step (2) is hot air drying or vacuum drying, and the drying method in steps (3) and (4) is vacuum drying; the drying temperature in steps (1) to (4) is 40 to 80°C;

[0027] The sunflower disk holocellulose described in the present invention is prepared by the above method.

[0028] The sunflower disk holocellulose of the present invention can be used as a disintegrant, in particular as a tablet disintegrant.

[0029] Preferably, the tablet is a dispersible tablet or an orally disintegrating tablet.

[0030] More preferably, the tablet contains pharmaceutically acceptable excipients.

[0031] Compared with the prior art, the present invention has the following beneficial effects:

[0032] The present invention subjects agricultural waste sunflower discs to alkali extraction, bleaching, and bio-enzyme modification treatment to obtain a novel and highly efficient sunflower disc holocellulose. The above-mentioned enzyme modification process of sunflower disc holocellulose further improves the physical and chemical properties of the holocellulose and improves the disintegration effect on tablets. The present invention uses sunflower discs as raw materials, has low cost, expands new avenues for the resource utilization of sunflower discs, and provides a new natural source for pharmaceutical excipients. At the same time, the preparation process provided by the present invention is simple to operate, has low equipment requirements, is green and environmentally friendly, is easy to industrialize, and has industrial application prospects. Experimental results show that the sunflower disc holocellulose obtained by the present invention has good disintegration performance and can be a novel and highly efficient pharmaceutical disintegrant. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 This is a diagram showing the water holding capacity of sunflower holocellulose obtained by different extraction methods and the raw material;

[0034] Figure 2 The swelling force results of sunflower holocellulose obtained by different extraction methods and the raw material are shown in the figure;

[0035] Figure 3 The figure shows the water absorption performance test results of sunflower holocellulose prepared in Example 1 and four commonly used disintegrants;

[0036] Figure 4 This is a graph showing the swelling performance test results of the sunflower disk holocellulose prepared in Example 1 and four commonly used disintegrants;

[0037] Figure 5 The figure shows the disintegration time test results of orally disintegrating tablets with different disintegrants;

[0038] Figure 6 This is a diagram showing the disintegration process of orally disintegrating tablets using sunflower seed holocellulose as a disintegrant;

[0039] Figure 7 This is a diagram of the disintegration process of orally disintegrating tablets using low-substituted hydroxypropyl cellulose as a disintegrant;

[0040] Figure 8 This is a diagram of the disintegration process of orally disintegrating tablets using cross-linked polyvinyl pyrrolidone as a disintegrant;

[0041] Figure 9This is a diagram of the disintegration process of orally disintegrating tablets with microcrystalline cellulose as a disintegrant;

[0042] Figure 10 This is a diagram of the disintegration process of orally disintegrating tablets using corn starch as a disintegrant. DETAILED DESCRIPTION

[0043] The following describes in detail the method for extracting sunflower disc holocellulose and the application of sunflower disc holocellulose in the field of pharmaceutical excipients provided by the present invention in conjunction with the examples, but they should not be construed as limiting the scope of protection of the present invention.

[0044] Example 1

[0045] A method for extracting sunflower disk holocellulose, comprising the following steps:

[0046] (1) Grinding: fresh sunflower discs were harvested, deseeded, air-dried, and ground into powder that passed through a 40-mesh standard sieve. The obtained powder was soaked in petroleum ether for 12 h for defatting, with the ratio of powder mass to petroleum ether volume being 1 g:10 mL. After defatting, the powder was vacuum filtered and then dried in an oven at 45°C to obtain sunflower disc powder.

[0047] (2) Alkali extraction: The sunflower disk powder obtained in step (1) was placed in a sodium hydroxide aqueous solution with a mass concentration of 3.2% and mixed for alkaline extraction, with a liquid-to-solid ratio of 19.7 mL:1 g, an extraction time of 54 min, and an extraction temperature of 58° C. The filter residue obtained after filtration was washed with deionized water until neutral, and dried in a vacuum oven at 60° C. to constant weight to obtain an alkaline extract of sunflower disk insoluble dietary fiber with a yield of 45.71%;

[0048] (3) Bleaching: The above alkaline extract was mixed with an acidic sodium chlorite aqueous solution (the mass concentration of the sodium chlorite aqueous solution was 10 g / L, and the pH was adjusted to 4.5 using glacial acetic acid) at a liquid-to-solid ratio of 20 mL:1 g. The mixture was sealed and heated with stirring for reaction. The bleaching time was 90 min and the bleaching temperature was 75°C. The filter residue obtained after filtration was washed with deionized water at 60°C until neutral, and then washed with anhydrous ethanol and acetone three times respectively. Finally, it was dried in a vacuum drying oven at 50°C to constant weight to obtain a bleached product.

[0049] (4) Enzyme modification: The bleached product was mixed with a citric acid-sodium citrate buffer solution having a pH of 4.7 at a liquid-to-solid ratio of 10 mL:1 g; cellulase and xylanase were then added at 1.0% and 3.0% of the mass of the bleached product, respectively, and the modified reaction was carried out under sealed heating and stirring. The modification time was 60 min and the modification temperature was 50°C. After the modification reaction was completed, the product was immediately transferred to a boiling water bath at 100°C to inactivate the enzyme for 5 min. The filter residue obtained after filtration was washed with deionized water until neutral, and then washed three times with 75% ethanol and anhydrous ethanol, respectively. Finally, the product was dried in a vacuum drying oven at 50°C to constant weight to obtain the sunflower disc holocellulose with a yield of 40.58%.

[0050] Example 2

[0051] A method for extracting sunflower disk holocellulose, comprising the following steps:

[0052] (1) Grinding: fresh sunflower discs were harvested, deseeded, air-dried, and ground into powder that passed through a 40-mesh standard sieve. The obtained powder was soaked in petroleum ether for 12 h for defatting, with the ratio of powder mass to petroleum ether volume being 1 g:10 mL. After defatting, the powder was vacuum filtered and then dried in an oven at 45°C to obtain sunflower disc powder.

[0053] (2) Alkali extraction: The sunflower disk powder obtained in step (1) was placed in a sodium hydroxide aqueous solution with a mass concentration of 3.2% and mixed for alkaline extraction, with a liquid-to-solid ratio of 20 mL:1 g, an extraction time of 60 min, and an extraction temperature of 60° C. The filter residue obtained after filtration was washed with deionized water until neutral, and dried in a vacuum oven at 60° C. to constant weight to obtain an alkaline extract of sunflower disk insoluble dietary fiber, with a yield of 45.26%;

[0054] (3) Bleaching: The above alkaline extract was mixed with a 3% by mass aqueous solution of hydrogen peroxide (adjusted to pH 9.0 with a 6% by mass aqueous solution of sodium hydroxide) at a liquid-to-solid ratio of 10 mL:1 g. The mixture was sealed and heated with stirring for a bleaching time of 90 min at a bleaching temperature of 90°C. The filter residue obtained after filtration was washed with deionized water at 60°C until neutral, then washed three times with anhydrous ethanol and acetone, respectively, and finally dried in a vacuum drying oven at 50°C to constant weight to obtain a bleached product.

[0055] (4) Enzyme modification: The bleached product was mixed with a citric acid-sodium citrate buffer solution having a pH of 4.7 at a liquid-to-solid ratio of 10 mL:1 g. Cellulase and xylanase were added at 1.0% and 1.0% of the mass of the bleached product, respectively. The mixture was sealed, heated, and stirred for reaction. The modification time was 60 min and the modification temperature was 50°C. After the reaction was completed, the mixture was immediately transferred to a boiling water bath at 100°C to inactivate the enzyme for 5 min. The residue obtained after filtration was washed with deionized water until neutral, and then washed three times with 75% ethanol and anhydrous ethanol, respectively. Finally, the mixture was dried in a vacuum drying oven at 50°C to constant weight to obtain the sunflower disc holocellulose with a yield of 39.77%.

[0056] Example 3

[0057] A method for extracting sunflower disk holocellulose, comprising the following steps:

[0058] (1) Grinding: fresh sunflower discs were harvested, deseeded, air-dried, and ground into powder that passed through a 40-mesh standard sieve. The obtained powder was soaked in petroleum ether for 12 h for defatting, with the ratio of powder mass to petroleum ether volume being 1 g:10 mL. After defatting, the powder was vacuum filtered and then dried in an oven at 45°C to obtain sunflower disc powder.

[0059] (2) Alkali extraction: The sunflower disk powder obtained in step (1) was placed in a sodium hydroxide aqueous solution with a mass concentration of 3.0% and mixed for alkaline extraction, with a liquid-to-solid ratio of 20 mL:1 g, an extraction time of 60 min, and an extraction temperature of 60° C. The filter residue obtained after filtration was washed with deionized water until neutral, and dried in a vacuum oven at 60° C. to constant weight to obtain an alkaline extract of sunflower disk insoluble dietary fiber, with a yield of 44.58%;

[0060] (3) Bleaching: The above alkaline extract was mixed with an acidic sodium chlorite aqueous solution (the mass concentration of the sodium chlorite aqueous solution was 10 g / L, and the pH was adjusted to 4.5 using glacial acetic acid) at a liquid-to-solid ratio of 20 mL:1 g. The mixture was sealed and heated with stirring for reaction. The bleaching time was 90 min and the bleaching temperature was 75°C. The filter residue obtained after filtration was washed with deionized water at 60°C until neutral, and then washed with anhydrous ethanol and acetone three times respectively. The bleached product, sunflower disc holocellulose, was obtained.

[0061] (4) Enzyme modification: The bleached product was mixed with a citric acid-sodium citrate buffer solution having a pH of 4.7 at a liquid-to-solid ratio of 10 mL:1 g, and then cellulase was added at 1% of the mass of the bleached product. The mixture was sealed, heated, and stirred for reaction. The reaction time was 60 min and the reaction temperature was 50°C. After the reaction was completed, the mixture was immediately transferred to a boiling water bath at 100°C for 5 min to inactivate the enzyme. The filter residue obtained after wave filtration was washed with deionized water until neutral, and then washed with 75% ethanol and anhydrous ethanol three times respectively. The mixture was dried in a vacuum drying oven at 50°C to constant weight to obtain the sunflower disc holocellulose with a yield of 40.03%.

[0062] Test Example 1

[0063] Effects of different extraction methods on the physicochemical properties of sunflower disk holocellulose:

[0064] The specific method is:

[0065] Determination of water holding capacity: Weigh 1.000 g of sample and place in a 50 mL centrifuge tube. Add 25 mL of deionized water, shake to mix, and hydrate at room temperature for 24 hours. Centrifuge at 4000 rpm for 15 minutes, discard the supernatant, and carefully wipe the centrifuge tube dry with filter paper. Calculate the water holding capacity as follows:

[0066]

[0067] Where: m0 is the dry weight of the fiber (1.000 g); m1 is the total mass of the centrifuge tube and the sample before water absorption (g); m2 is the total mass of the centrifuge tube and the sample after water absorption (g).

[0068] Determination of expansion force: Weigh 0.250 g of sample, place in a 25 mL expansion tube, read the scale V1, add 20 mL of deionized water, shake and mix, let stand at room temperature for 24 hours, read the scale V2 corresponding to the sample after water absorption. The expansion force calculation formula is as follows:

[0069]

[0070] Where: V1 is the initial volume of the sample (mL); V2 is the volume of the sample after water absorption and expansion (mL); m is the dry weight of the sample (0.250 g).

[0071] Test results: The present invention obtained several sunflower disk holocelluloses through different embodiments. Figure 1 and Figure 2 It can be seen that the product obtained by the acidic sodium chlorite bleaching process performed better than the alkaline hydrogen peroxide method, and the product obtained by the enzyme modification process using a combination of cellulase and ligninase was superior to that obtained by modification using only cellulase. Compared with the raw material, the water-holding capacity and swelling capacity of the sunflower disk holocellulose obtained in Example 1 increased by 134.27% and 183.74%, respectively.

[0072] Test Example 2

[0073] Determination of disintegration performance of sunflower disk holocellulose and four commonly used disintegrants:

[0074] The present invention tests the water absorption and swelling properties of the sunflower disk holocellulose prepared in Example 1 and four commonly used disintegrants. The disintegrants tested include corn starch, microcrystalline cellulose, low-substituted hydroxypropyl cellulose, and cross-linked polyvinyl pyrrolidone. The test method is as follows:

[0075] Water absorption performance: Test according to the water holding capacity determination method in Test Example 1.

[0076] Swelling performance study: Weigh 0.250 g of different disintegrant powders (passed through an 80-mesh sieve) and add them to a 25 mL expansion tube. Add 5 mL of liquid paraffin and 10 mL of deionized water, respectively. Shake to completely suspend the powder. Let stand at room temperature for 12 hours. Observe the volume of the disintegrant in different solvents. The swelling performance of the sample is characterized by the swelling ratio, which is calculated as follows:

[0077]

[0078] Where: V1 is the volume of disintegrant in liquid paraffin (mL); V2 is the expanded volume of disintegrant in water (mL).

[0079] Water absorption performance test results: Figure 3 As shown in the figure, the water absorption properties of different disintegrants vary significantly. The results show that sunflower holocellulose has the best water absorption capacity, far exceeding that of the other disintegrants. Furthermore, sunflower holocellulose absorbs 4.85 times more water than microcrystalline cellulose, indicating its excellent water absorption properties and its ability to absorb large amounts of water as a disintegrant to promote tablet disintegration.

[0080] Swelling performance test results: Swelling performance of different disintegrants Figure 4 The results showed that sunflower holocellulose had the best swelling property, slightly better than low-substituted hydroxypropyl cellulose, while starch and microcrystalline cellulose had average swelling properties, and the volume of cross-linked polyvinyl pyrrolidone was almost unchanged before and after the test.

[0081] Example 4

[0082] An application of sunflower disc holocellulose in preparing orally disintegrating tablets, comprising the following steps:

[0083] An orally disintegrating tablet comprising:

[0084] Aripiprazole 10g;

[0085] Mannitol 20.6g;

[0086] Lactose 20.6g;

[0087] Disintegrant 12g;

[0088] Aspartame 0.6g;

[0089] Silicon dioxide 0.6 g;

[0090] Magnesium stearate 0.6g.

[0091] The disintegrant is selected from any one of sunflower holocellulose, corn starch, microcrystalline cellulose, low-substituted hydroxypropyl cellulose, and cross-linked polyvinyl pyrrolidone.

[0092] Preparation method: The aripiprazole raw material is ultrafinely ground and passed through a 100-mesh sieve. The remaining excipients are passed through an 80-mesh sieve. The powder direct tableting method is used to mix the aripiprazole raw material with the remaining excipients in proportion in equal amounts. The tablets are compressed using a single-punch tablet press under the same pressure and filling amount. The punch die is a 6mm shallow concave punch. The tablet weight is 60 mg and the tablet specification is 5 mg.

[0093] Test Example 3

[0094] Determination of the disintegration time of different aripiprazole orally disintegrating tablets;

[0095] Using the titration method, a 25mL burette is filled to the zero mark with (37±0.5)°C water. During the test, the sample is placed on a 30-mesh sieve. The water droplet is approximately 2cm vertically from the sample surface at a controlled drip rate of 2mL / min. Timing begins when the water droplet strikes the orally disintegrating tablet and ends when no residue remains on the sieve.

[0096] Test results: Figure 5 As shown, the disintegration rates of different disintegrants are as follows: low-substituted hydroxypropyl cellulose > sunflower holocellulose > cross-linked polyvinyl pyrrolidone > microcrystalline cellulose > corn starch. The results indicate that sunflower holocellulose exhibits excellent disintegration properties, with an average in vitro disintegration time of 34.27 seconds, which is related to its good water absorption and swelling properties. At the same disintegrant dosage, the sunflower holocellulose prepared in the present invention exhibits a slightly better disintegration time than the highly efficient disintegrant cross-linked polyvinyl pyrrolidone, and better than the common disintegrants corn starch and microcrystalline cellulose.

[0097] Test Example 4

[0098] Determination of the disintegration process of different aripiprazole orally disintegrating tablets;

[0099] The specific method is:

[0100] Different orally disintegrating aripiprazole tablets prepared in Example 4 were placed in water at (37±0.5)° C., and the disintegration process was photographed using a digital camera (Nikon Z6II, Japan).

[0101] Test results: Figure 6 The disintegration process of tablets using sunflower disc holocellulose as a disintegrant was demonstrated: the tablets expanded rapidly within 5 seconds after contacting water, and then fully expanded within 15 seconds, with their own volume increasing significantly. In addition to external water absorption and expansion, due to the strong water absorption capacity of the material itself, water entered the tablet core through a strong capillary action, causing it to absorb water from the inside and expand and disintegrate. The simultaneous action of the internal and external factors enabled the tablets to quickly disintegrate within 30 seconds. When low-substituted hydroxypropyl cellulose was used as a disintegrant, the process was similar to that of sunflower disc holocellulose ( Figure 7 ); Compared with other disintegrants, cross-linked polyvinyl pyrrolidone does not show obvious wicking and swelling effects, but has better deformation recovery ability ( Figure 8 ), the disintegration rate is slightly slower than that of sunflower disc holocellulose; Figure 9 and Figure 10 As shown in the figure, the water absorption and swelling properties of microcrystalline holocellulose and corn starch are average, and their disintegration rates are slow.

[0102] It can be seen from the above examples that the sunflower disc holocellulose prepared by the present invention has good water absorption, swelling and disintegration properties when used as a high-efficiency pharmaceutical disintegrant, which is comparable to commonly used commercially available high-efficiency disintegrants; and the present invention uses sunflower discs as raw materials, which have a wide source, low cost, simple preparation process and are environmentally friendly, which not only broadens the natural source of pharmaceutical excipients, but also further realizes the high-value utilization of agricultural waste sunflower discs.

[0103] The above is only 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. A method for preparing sunflower disk holocellulose, comprising the following steps: (1) pre-treating sunflower discs to obtain sunflower disc powder; (2) placing the sunflower disk powder obtained in step (1) in an alkaline solution for alkaline extraction, filtering the resulting filter residue, washing it with deionized water until it is neutral, and drying it to obtain an alkaline extraction product; (3) placing the alkali extraction product obtained in step (2) in a bleaching aqueous solution for bleaching reaction, filtering the resulting filter residue and washing it with deionized water at 50 to 70° C. until it is neutral, then washing it with anhydrous ethanol and acetone for 3 to 5 times respectively, and drying it to obtain a bleached product; (4) The bleached product obtained in step (3) is prepared into an acidic solution, and then a biological enzyme is added to perform an enzyme modification reaction under sealed heating and stirring. After the enzyme is inactivated, the filter is filtered, and the obtained filter residue is washed with deionized water until neutral, and then washed with 75% by mass ethanol and anhydrous ethanol for 3 to 5 times respectively, and dried to obtain the sunflower disk holocellulose.

2. The method for preparing sunflower disk holocellulose according to claim 1, wherein: The pretreatment in step (1) is to remove the seeds from the fresh sunflower disks, air-dry them, and grind them into powder that can pass through a 20-40 mesh standard sieve; soak the obtained powder in petroleum ether for 10-12 hours for defatting, with the ratio of powder mass to petroleum ether volume being 1g:5-15mL; vacuum filter the powder after defatting, and then dry it to obtain sunflower disk powder.

3. The method for preparing sunflower disk holocellulose according to claim 1, wherein: The alkaline solution in step (2) is one of a NaOH aqueous solution and a KOH aqueous solution; the material-liquid ratio of sunflower disk powder to alkaline solution is 1g:15-25mL, and the mass concentration of the alkaline solution is 1-5%; the extraction temperature is 50-70°C, and the extraction time is 30-90min.

4. The method for preparing sunflower disk holocellulose according to claim 1, wherein: The bleaching reaction in step (3) is carried out under sealed, heated and stirred conditions, and the bleaching method is one of the acidic sodium chlorite bleaching method and the alkaline hydrogen peroxide bleaching method.

5. The method for preparing sunflower disk holocellulose according to claim 4, wherein: In the acidic sodium chlorite bleaching method, the mass concentration of the sodium chlorite aqueous solution is 10-20 g / L, and the reaction pH condition is 4-5; in the alkaline hydrogen peroxide bleaching method, the mass fraction of the hydrogen peroxide aqueous solution is 3-5%, and the reaction pH condition is 9-10.

6. The method for preparing sunflower disk holocellulose according to claim 1, wherein: In the bleaching treatment of step (3), the material-liquid ratio of the alkali extraction product to the bleaching aqueous solution is 1 g: 10-25 mL, the bleaching temperature is 70-100° C., and the bleaching time is 60-120 min.

7. The method for preparing sunflower disk holocellulose according to claim 1, wherein: The enzyme modification reaction in step (4) is carried out under sealed heating and stirring; the bleaching product is prepared into an acidic solution by mixing the bleaching product with a citric acid-sodium citrate buffer solution with a pH of 4 to 5, and the material-liquid ratio of the bleaching product to the citric acid-sodium citrate buffer solution is 1 g:10 to 20 mL.

8. The method for preparing sunflower disk holocellulose according to claim 1, wherein: The biological enzyme used in step (4) is at least one of cellulase and xylanase; when cellulase and xylanase are used in combination, the mass ratio of cellulase to xylanase is 1:1-4; the total amount of biological enzyme added is 1.0-5.0% of the mass of the bleached product, the modification temperature is 40-60°C, and the modification time is 30-90 minutes; the enzyme is inactivated in a boiling water bath at 100°C for 4-6 minutes.

9. A sunflower disk holocellulose, characterized by: The method is prepared by any one of claims 1 to 8.

10. Use of the sunflower disk holocellulose according to claim 9 as a disintegrant.

Images