CN116036015B - Microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product and preparation method thereof - Google Patents
Microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product and preparation method thereof Download PDFInfo
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- CN116036015B CN116036015B CN202211468350.1A CN202211468350A CN116036015B CN 116036015 B CN116036015 B CN 116036015B CN 202211468350 A CN202211468350 A CN 202211468350A CN 116036015 B CN116036015 B CN 116036015B
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- 239000001768 carboxy methyl cellulose Substances 0.000 title claims abstract description 104
- 229920002134 Carboxymethyl cellulose Polymers 0.000 title claims abstract description 96
- 239000008112 carboxymethyl-cellulose Substances 0.000 title claims abstract description 96
- 235000010948 carboxy methyl cellulose Nutrition 0.000 title claims abstract description 92
- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims abstract description 64
- 239000008108 microcrystalline cellulose Substances 0.000 claims abstract description 64
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims abstract description 64
- 229940016286 microcrystalline cellulose Drugs 0.000 claims abstract description 64
- -1 hydroxyethyl carboxymethyl Chemical group 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002002 slurry Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 238000001694 spray drying Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000008213 purified water Substances 0.000 claims abstract description 10
- 239000000725 suspension Substances 0.000 claims description 38
- 239000000463 material Substances 0.000 claims description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 229920001131 Pulp (paper) Polymers 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- 238000006467 substitution reaction Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 2
- 238000009472 formulation Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 8
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- 239000013049 sediment Substances 0.000 abstract description 4
- 238000007086 side reaction Methods 0.000 abstract description 3
- 238000005189 flocculation Methods 0.000 abstract description 2
- 230000016615 flocculation Effects 0.000 abstract description 2
- 230000036571 hydration Effects 0.000 abstract description 2
- 238000006703 hydration reaction Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 34
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 14
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 13
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- 239000002994 raw material Substances 0.000 description 12
- 239000012065 filter cake Substances 0.000 description 10
- 238000012545 processing Methods 0.000 description 9
- 239000000853 adhesive Substances 0.000 description 8
- 230000001070 adhesive effect Effects 0.000 description 8
- 238000011278 co-treatment Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 8
- 230000001276 controlling effect Effects 0.000 description 7
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 6
- 238000005086 pumping Methods 0.000 description 6
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 6
- 238000011056 performance test Methods 0.000 description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 4
- 229930006000 Sucrose Natural products 0.000 description 4
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 4
- QYIYFLOTGYLRGG-GPCCPHFNSA-N cefaclor Chemical compound C1([C@H](C(=O)N[C@@H]2C(N3C(=C(Cl)CS[C@@H]32)C(O)=O)=O)N)=CC=CC=C1 QYIYFLOTGYLRGG-GPCCPHFNSA-N 0.000 description 4
- 229960005361 cefaclor Drugs 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 239000005720 sucrose Substances 0.000 description 4
- 239000008186 active pharmaceutical agent Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000004537 pulping Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 229920003090 carboxymethyl hydroxyethyl cellulose Polymers 0.000 description 1
- 235000010980 cellulose Nutrition 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000008040 ionic compounds Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007935 oral tablet Substances 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000015067 sauces Nutrition 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/10—Dispersions; Emulsions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
- A61K47/38—Cellulose; Derivatives thereof
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention provides a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product and a preparation method thereof, wherein the co-processed product comprises 10-25% of hydroxyethyl carboxymethyl cellulose and 75-90% of microcrystalline cellulose, the viscosity of a 1% aqueous solution of the co-processed product is 40-5000 cp, the pH is 5-8, and the preparation method of the co-processed product comprises the following steps: mixing and stirring microcrystalline cellulose, purified water and hydroxyethyl carboxymethyl cellulose to obtain slurry; and carrying out spray drying treatment on the slurry to obtain the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product. The microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product provided by the invention has better chemical stability and chemical compatibility when being used together with other reagents, reduces the risk of forming sediment due to side reaction with other reagents, has higher hydration binding capacity and flocculation effect, and has stronger universality.
Description
Technical Field
The invention relates to the technical field related to medical foods, in particular to a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product and a preparation method thereof.
Background
The co-processed auxiliary materials are prepared by processing two or more auxiliary materials through specific physical processing technologies (such as spray drying, granulating and the like), and the novel auxiliary materials with specific functions and uniform appearance are produced through advantage complementation. The co-processing makes the composite auxiliary material physically modified in a special mode under the condition of not changing the chemical structure, and the fixed and uniform distribution is realized by closely connecting one auxiliary material with the other auxiliary material in submicron order, so that the defects of nonuniform mixing and nonuniform performance of the prior premix are overcome.
Microcrystalline cellulose is a linear polysaccharide substance bonded by beta-1, 4-glucosidic bond, is free-flowing superfine short rod-shaped or powdery porous particles with limited polymerization degree, is prepared by hydrolysis of natural cellulose by dilute acid, and is widely applied to the field of pharmaceutical preparations, and is widely used as a diluent and a binder of oral tablets and capsules. In the existing products, microcrystalline cellulose and other auxiliary materials are often processed and mixed to improve the performance of the microcrystalline cellulose and meet more application scenes, for example, patent document with the application number of CN201280048427.8 discloses a stabilizer composition, wherein the stabilizer composition comprises microcrystalline cellulose and water-soluble carboxymethyl cellulose with low viscosity and substitution degree of about 0.45-0.85; the patent document with the application number of CN201510590673.1 discloses a preparation process of modified microcrystalline cellulose, which comprises the following process steps: mixing and kneading the microcrystalline cellulose filter cake and 7LF sodium carboxymethyl cellulose accounting for 5.5-9.3% of the microcrystalline cellulose filter cake, carrying out high-pressure homogenization after high-shear treatment, and drying; or mixing the microcrystalline cellulose filter cake with 7LF sodium carboxymethyl cellulose accounting for 10 to 18.5 percent of the microcrystalline cellulose filter cake after high-shear treatment, kneading, homogenizing under high pressure and drying.
In the method, microcrystalline cellulose and sodium carboxymethyl cellulose are mixed to improve the performance of the microcrystalline cellulose, but in the application process, the existence of sodium carboxymethyl cellulose can cause incompatibility between the composition and some preparations, and the composition can generate byproducts such as precipitation, co-condensation and the like when being mixed with some preparations in certain scenes, so that the effect of the preparations is affected, and the application range of the composition is limited.
Disclosure of Invention
In order to solve the problems, the invention provides a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product and a preparation method thereof, and the co-processed product solves the problem that the application of the existing microcrystalline cellulose-sodium carboxymethyl cellulose composition is limited due to easy formation of precipitation with other reagents to a certain extent, and has wide application range and strong stability.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
The invention provides a preparation method of microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed matter, which comprises the following steps:
s1, mixing and stirring microcrystalline cellulose, purified water and hydroxyethyl carboxymethyl cellulose to obtain slurry;
S2, carrying out spray drying treatment on the slurry obtained in the step S2 to obtain microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed matter; the content of hydroxyethyl carboxymethyl cellulose in the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose is 10-25%, and the content of microcrystalline cellulose is not less than 75%.
In order to improve the performance of microcrystalline cellulose auxiliary materials, the existing product generally mixes microcrystalline cellulose and sodium carboxymethyl cellulose to form co-processed auxiliary materials, and the co-processed auxiliary materials are matched with other preparations for use. However, the inventors found that the co-processed excipients may form by-products such as precipitates and co-agglomerates in some application scenarios, which may affect the effect of the co-processed formulations. The inventor researches that sodium carboxymethyl cellulose in the co-processing auxiliary materials is an ionic compound, and when the co-processing auxiliary materials are used together with other preparations, chemical compatibility problems are easy to occur, so that side reactions are caused to form substances such as precipitation, and the effect of the preparations is affected, and therefore, in order to avoid the influence of pharmaceutical active ingredients, the selection range of matched preparations is limited when the co-processing auxiliary materials are used. In order to solve the problem, the inventor proposes that a nonionic compound is used as a modification additive to prepare microcrystalline cellulose co-processing auxiliary materials with wide application range and strong stability, and particularly, the nonionic compound is hydroxyethyl carboxymethyl cellulose, 10-25% of hydroxyethyl carboxymethyl cellulose and 75-90% of microcrystalline cellulose are added into purified water to be stirred to form slurry, and then the slurry is subjected to spray drying treatment, so that the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processing material is obtained, and the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processing material has good flowability, can form stable suspension in aqueous solution, is not easy to precipitate, has good compatibility between microcrystalline cellulose and hydroxyethyl carboxymethyl cellulose, has the effects of disintegration and suspension aid, and is particularly suitable for the production of dry suspension preparations.
In the present invention, unless otherwise noted, the percentages refer to percentages by mass.
Further, the preparation method of the microcrystalline cellulose comprises the following steps: soaking wood pulp in hydrochloric acid solution for 10-60 s, pressing the soaked wood pulp to dryness, aging for 24-48 hours at 30-60 ℃, then soaking the aged wood pulp in water, adding sodium hydroxide solution to neutralize to pH 5-8, homogenizing by using a high-speed homogenizer to obtain microcrystalline cellulose suspension, and performing filter pressing, washing and drying on the microcrystalline cellulose suspension to obtain microcrystalline cellulose.
Preferably, the microcrystalline cellulose has an average length of no more than 10 μm; further preferably, the microcrystalline cellulose has an average length of no more than 5 μm.
Preferably, the mass concentration of the hydrochloric acid solution is 7.5-15.0%.
Preferably, the viscosity of the hydroxyethyl carboxymethyl cellulose is 50-6000, the substitution degree is 1.5-2.0, and the molar substitution degree is 2.0-2.5. The viscosity of hydroxyethyl carboxymethyl cellulose herein refers to the viscosity of its 2% aqueous solution.
Preferably, when preparing microcrystalline cellulose, a plate-and-frame filter press is used to filter the microcrystalline cellulose suspension, and the plate-and-frame filter press is used to wash until the difference between the conductivity of the effluent and the conductivity of the wash inlet is less than 70 mu S/cm.
Preferably, the solid content of the slurry is 15-25%.
Preferably, the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product has a particle size of no more than 100 mesh.
Preferably, the spray drying treatment is accomplished by a centrifugal spray dryer.
Preferably, the spray drying treatment specifically includes the steps of: starting a centrifugal spray dryer, setting the air inlet temperature to be 160-180 ℃, starting to pump the slurry prepared in the step S1 when the air outlet temperature reaches 100 ℃, controlling the feeding speed to keep the air outlet temperature to be 90-100 ℃, collecting the sprayed material, and sieving the material with a 100-mesh sieve to obtain the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product.
It is another object of the present invention to provide a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product produced by the above method.
The invention also aims to provide a solid preparation containing the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product, in particular to a dry suspension preparation.
In summary, the following beneficial effects can be obtained by applying the scheme of the invention:
1. The microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed by the method has good fluidity, can form stable suspension in aqueous solution, is not easy to generate coagulation, is uniformly mixed with the hydroxyethyl carboxymethyl cellulose, has good dispersibility, has better performance when being used as auxiliary materials, and is particularly suitable for preparing dry suspension preparations.
2. Compared with microcrystalline cellulose-sodium carboxymethyl cellulose co-processed matters in the prior art, the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed matters provided by the invention have higher hydration binding capacity and better flocculation effect on suspended solids, and meanwhile, the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed matters have better chemical stability and chemical compatibility when being used together with other reagents, and the risk of forming precipitates due to side reaction is reduced, so that the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed matters have better universality, can be matched with more kinds of pharmaceutically active matters for use, and can be also used in the food fields such as beverages, sauces and the like.
Detailed Description
The invention will be further described with reference to specific examples for a better understanding of the invention by those skilled in the relevant art. It should be understood that the specific examples described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
The present example provides a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product, which is prepared by the following method:
(1) Microcrystalline cellulose preparation: the wood pulp is put into hydrochloric acid with the concentration of 8 percent for soaking for 30 seconds, then the wood pulp is pressed by a roller squeezer until the wood pulp content is 30 percent, the pressed wood pulp is aged for 36 hours at the temperature of 45 ℃, then water is added for soaking, the pH is neutralized to be 6.5 by sodium hydroxide solution, and a microcrystalline cellulose suspension is obtained after homogenizing for 15 minutes at 18000rpm by a high-speed homogenizer. Pumping the microcrystalline cellulose suspension into a plate-and-frame filter press for filter pressing, washing with purified water and drying to obtain a microcrystalline cellulose filter cake for later use;
(2) Mixing and pulping: adding 900 parts of purified water, 90 parts of microcrystalline cellulose filter cake (dry materials are calculated after removing water) and 10 parts of hydroxyethyl carboxymethyl cellulose (DS: 2.0, MS:2.5, viscosity: 50 cps) into a stirring kettle, and stirring for 3 hours to obtain uniformly dispersed and stable slurry for later use;
(3) Spray drying: starting a cleaned centrifugal spray dryer, setting the air inlet temperature to 180 ℃, controlling and adjusting the frequency of a centrifugal high-speed motor to 30HZ, starting pumping slurry when the air outlet temperature reaches 100 ℃, controlling the feeding speed to keep the air outlet temperature at 90-100 ℃, collecting the sprayed material, and passing through 100 meshes to obtain a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product.
Example 2
This example provides another microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-treatment prepared in substantially the same manner as in example 1, except that the hydroxyethyl carboxymethyl cellulose has a viscosity of 200cps.
Example 3
This example provides another microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-treatment prepared in substantially the same manner as in example 1, except that the hydroxyethyl carboxymethyl cellulose has a viscosity of 800cps.
Example 4
This example provides another microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-treatment prepared in substantially the same manner as in example 1, except that the hydroxyethyl carboxymethyl cellulose has a viscosity of 2000cps.
Example 5
This example provides another microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-treatment prepared in substantially the same manner as in example 1, except that the hydroxyethyl carboxymethyl cellulose has a viscosity of 5000cps.
Performance test one: the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product samples prepared in examples 1 to 5 were prepared as aqueous solutions, the viscosity of the co-processed aqueous solutions was tested, and the suspension stability of the co-processed product aqueous solutions was observed, and the results are shown in table 1.
TABLE 1
According to the results in table 1, it can be seen that the viscosity of the co-processed product is positively correlated with the viscosity of the hydroxyethyl carboxymethyl cellulose, and in specific application, the viscosity of the hydroxyethyl carboxymethyl cellulose can be adjusted according to the viscosity requirement in the application scene to change the overall viscosity of the co-processed product, thereby meeting the application requirement. In examples 1 to 5, hydroxyethyl carboxymethyl cellulose with the viscosity of 50 to 5000 is selected to prepare the co-processed product, and from the aspect of the suspension stability result, examples 1 to 5 can reach the standard, so that uniformity and stability of the co-processed product are not affected when the viscosity of the co-processed product is changed by adjusting the hydroxyethyl carboxymethyl cellulose within a certain range.
Example 6
The present example provides a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product, which is prepared by the following method:
(1) Microcrystalline cellulose preparation: the pulp was soaked in 8% hydrochloric acid for 40 seconds, then pressed dry by a roller press, the pressed dry pulp was aged at 35 ℃ for 48 hours, then soaked in water and neutralized to pH6.5 with sodium hydroxide solution, and homogenized for 15 minutes at 18000rpm with a high speed homogenizer to obtain microcrystalline cellulose suspension. Pumping the microcrystalline cellulose suspension into a plate-and-frame filter press for filter pressing, washing with purified water and drying to obtain a microcrystalline cellulose filter cake for later use;
(2) Mixing and pulping: adding 900 parts of purified water and 100 parts of microcrystalline cellulose filter cake (dry materials are calculated by removing water) into a stirring kettle, and stirring for 3 hours to obtain uniformly dispersed and stable slurry for later use, wherein 0 part of hydroxyethyl carboxymethyl cellulose (DS: 2.0, MS:2.5, viscosity: 2000 cps);
(3) Spray drying: starting a cleaned centrifugal spray dryer, setting the air inlet temperature to 180 ℃, controlling and adjusting the frequency of a centrifugal high-speed motor to 30HZ, starting pumping slurry when the air outlet temperature reaches 100 ℃, controlling the feeding speed to keep the air outlet temperature at 90-100 ℃, and collecting the sprayed material and passing through a 100-mesh sieve to obtain the microcrystalline cellulose treated matter.
Example 7
This example provides another microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product prepared in substantially the same manner as in example 6, except that the microcrystalline cellulose cake was added in an amount of 95 parts and the hydroxyethyl carboxymethyl cellulose was added in an amount of 5 parts in step (2).
Example 8
This example provides another microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product prepared in substantially the same manner as in example 6, except that the microcrystalline cellulose cake was added in an amount of 90 parts and the hydroxyethyl carboxymethyl cellulose was added in an amount of 10 parts in step (2).
Example 9
This example provides another microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product prepared in substantially the same manner as in example 6, except that the microcrystalline cellulose cake was added in an amount of 85 parts and the hydroxyethyl carboxymethyl cellulose was added in an amount of 15 parts in step (2).
Example 10
This example provides another microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product prepared in substantially the same manner as in example 6, except that the microcrystalline cellulose cake was added in an amount of 80 parts and the hydroxyethyl carboxymethyl cellulose was added in an amount of 20 parts in step (2).
Example 11
This example provides another microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product prepared in substantially the same manner as in example 6, except that the microcrystalline cellulose cake was added in an amount of 75 parts and the hydroxyethyl carboxymethyl cellulose was added in an amount of 25 parts in step (2).
And II, performance test: the co-processed products prepared in examples 6 to 11 were prepared as 5% aqueous solutions, and the suspension stability of the aqueous solutions was observed, and the results are shown in table 2.
TABLE 2
From the results shown in table 2, it was found that the suspension stability of microcrystalline cellulose in an aqueous solution can be improved after the co-processed product is obtained by mixing hydroxyethyl carboxymethyl cellulose with microcrystalline cellulose, and that the hydroxyethyl carboxymethyl cellulose content is optimal when it is 15 to 25%.
Example 12
The present example provides a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product, which is prepared by the following method:
(1) Microcrystalline cellulose preparation: the pulp was soaked in 8% hydrochloric acid for 60 seconds, then pressed dry by a roller press, the pressed dry pulp was aged at 45 ℃ for 36 hours, then soaked in water and neutralized to pH6.5 with sodium hydroxide solution, and homogenized for 15 minutes at 18000rpm with a high speed homogenizer to obtain microcrystalline cellulose suspension. Pumping the microcrystalline cellulose suspension into a plate-and-frame filter press for filter pressing, washing with purified water and drying to obtain a microcrystalline cellulose filter cake for later use;
(2) Mixing and pulping: adding 900 parts of purified water, 80 parts of microcrystalline cellulose filter cake (dry materials are calculated after removing water) and 20 parts of hydroxyethyl carboxymethyl cellulose (DS: 1.8, MS:2.3, viscosity: 50 cps) into a stirring kettle, and stirring for 3 hours to obtain uniformly dispersed and stable slurry for later use; the microcrystalline cellulose has an average length of 25 μm;
(3) Spray drying: starting a cleaned centrifugal spray dryer, setting the air inlet temperature to 180 ℃, controlling and adjusting the frequency of a centrifugal high-speed motor to 40HZ, starting pumping slurry when the air outlet temperature reaches 100 ℃, controlling the feeding speed to keep the air outlet temperature at 90-100 ℃, collecting the sprayed material, and passing through 100 meshes to obtain a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product.
Example 13
This example provides another microcrystalline cellulose-hydroxyethylcarboxylmethylcellulose co-treatment prepared in substantially the same manner as in example 12, except that the microcrystalline cellulose produced in step (1) has an average length of 20. Mu.m.
Example 14
This example provides another microcrystalline cellulose-hydroxyethylcarboxylmethylcellulose co-treatment prepared in substantially the same manner as in example 12, except that the microcrystalline cellulose produced in step (1) has an average length of 15. Mu.m.
Example 15
This example provides another microcrystalline cellulose-hydroxyethylcarboxylmethylcellulose co-treatment prepared in substantially the same manner as in example 12, except that the microcrystalline cellulose produced in step (1) has an average length of 10. Mu.m.
Example 16
This example provides another microcrystalline cellulose-hydroxyethylcarboxylmethylcellulose co-treatment prepared in substantially the same manner as in example 12, except that the microcrystalline cellulose produced in step (1) has an average length of 5. Mu.m.
And (3) performance test: the co-processed products prepared in examples 12 to 16 were prepared as aqueous solutions, and the suspension stability of the aqueous solutions was observed, and the results are shown in table 3.
TABLE 3 Table 3
As can be seen from Table 3, the co-processed product has a good suspension stability when the average length of the microcrystalline cellulose is 5 to 15. Mu.m.
Example 17
In the embodiment, the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product prepared in the embodiment 16 is used as an auxiliary material to prepare a dry suspension preparation, and the preparation method comprises the following steps:
firstly, mixing microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed powder with powder to obtain a mixed raw material, then spraying an adhesive into the mixed raw material for granulating, and drying the prepared granules at 45 ℃ for 10min to obtain a dry suspension preparation;
the mixed raw materials comprise the following components in parts by mass: 10 parts of cefaclor, 50 parts of sucrose, 2.5 parts of microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed matter and 0.2 part of essence; the adhesive comprises the following components in parts by mass: sodium dodecyl sulfate 0.1 part, citric acid 0.1 part and deionized water 15 parts.
Performance test: and adding a proper amount of the dry suspension preparation into a 100mL measuring cylinder, adding water, stirring for 1min, standing, and observing the sedimentation condition, wherein the sedimentation condition is shown in Table 4.
TABLE 4 Table 4
As can be seen from Table 4, the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product prepared by the method has good dispersibility and suspension effect when being used as auxiliary materials of a dry suspension preparation, the dry suspension preparation solution does not generate sediment within 5 hours of water, the solution is beneficial to taking, a small amount of sediment is generated after 7 hours, the dry suspension preparation can be redispersed uniformly after being stirred slowly at 20 revolutions per minute, and the sediment can be redispersed by manual stirring when in use.
Comparative example 1
The comparative example uses microcrystalline cellulose-hydroxyethyl cellulose co-processed matters as auxiliary materials to prepare a dry suspension preparation, and the preparation method comprises the following steps:
Firstly, mixing microcrystalline cellulose-hydroxyethyl cellulose co-processed powder with powder to obtain a mixed raw material, then spraying an adhesive into the mixed raw material for granulating, and drying the obtained granules at 45 ℃ for 10min to obtain a dry suspension preparation;
The mixed raw materials comprise the following components in parts by mass: 10 parts of cefaclor, 50 parts of sucrose, 2.5 parts of microcrystalline cellulose-hydroxyethyl cellulose co-processed matter and 0.2 part of essence; the adhesive comprises the following components in parts by mass: sodium dodecyl sulfate 0.1 part, citric acid 0.1 part and deionized water 15 parts.
The microcrystalline cellulose-hydroxyethylcellulose co-processed preparation method example 12 is essentially the same, except that hydroxyethylcellulose is used instead of hydroxyethylcarboxymethylcellulose.
Comparative example 2
The comparative example uses microcrystalline cellulose-carboxymethyl cellulose co-processed matters as auxiliary materials to prepare a dry suspension preparation, and the preparation method comprises the following steps:
Firstly, mixing microcrystalline cellulose-carboxymethyl cellulose co-processed powder with powder to obtain a mixed raw material, then spraying an adhesive into the mixed raw material for granulating, and drying the obtained granules at 45 ℃ for 10min to obtain a dry suspension preparation;
the mixed raw materials comprise the following components in parts by mass: 10 parts of cefaclor, 50 parts of sucrose, 2.5 parts of microcrystalline cellulose-carboxymethyl cellulose co-processed matter and 0.2 part of essence; the adhesive comprises the following components in parts by mass: sodium dodecyl sulfate 0.1 part, citric acid 0.1 part and deionized water 15 parts.
The microcrystalline cellulose-carboxymethyl cellulose co-processed preparation method example 12 is substantially the same except that carboxymethyl cellulose is used in step (2) instead of hydroxyethyl carboxymethyl cellulose.
Comparative example 3
The comparative example uses microcrystalline cellulose-carboxymethyl cellulose-hydroxyethyl cellulose co-processed matters as auxiliary materials to prepare a dry suspension preparation, and the preparation method comprises the following steps:
Firstly, mixing microcrystalline cellulose-carboxymethyl cellulose-hydroxyethyl cellulose co-processed powder with powder to obtain a mixed raw material, then spraying an adhesive into the mixed raw material for granulating, and drying the obtained granules at 45 ℃ for 10min to obtain a dry suspension preparation;
The mixed raw materials comprise the following components in parts by mass: 10 parts of cefaclor, 50 parts of sucrose, 2.5 parts of microcrystalline cellulose-carboxymethyl cellulose-hydroxyethyl cellulose co-processed matter and 0.2 part of essence; the adhesive comprises the following components in parts by mass: sodium dodecyl sulfate 0.1 part, citric acid 0.1 part and deionized water 15 parts.
The microcrystalline cellulose-carboxymethyl cellulose-hydroxyethyl cellulose co-processed preparation method example 12 is substantially the same except that carboxymethyl cellulose and hydroxyethyl cellulose are used instead of hydroxyethyl carboxymethyl cellulose in step (2), wherein the carboxymethyl cellulose is 55 parts and the hydroxyethyl cellulose is 25 parts.
Performance test: and adding a proper amount of the dry suspension preparation into a 100mL measuring cylinder, adding water, stirring for 1min, standing, and observing the sedimentation condition, wherein the sedimentation condition is shown in Table 5.
TABLE 5
In some existing dry suspension agents, hydroxyethyl cellulose or carboxymethyl cellulose or both may be added, and according to table 5, it is known that the solution of either hydroxyethyl cellulose or carboxymethyl cellulose alone or hydroxyethyl cellulose and carboxymethyl cellulose blended is poor in effect compared with the solution of the present invention, so that the present invention has better effect compared with the existing product when applied to the field of dry suspension preparations.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the present invention, and those skilled in the art should not depart from the spirit of the present invention and should also fall within the scope of the appended claims.
Claims (8)
1. A method for preparing microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed matter, comprising the following steps:
s1, mixing and stirring microcrystalline cellulose, purified water and hydroxyethyl carboxymethyl cellulose to obtain slurry;
S2, carrying out spray drying treatment on the slurry obtained in the step S1 to obtain microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed matter; the content of hydroxyethyl carboxymethyl cellulose in the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product is 15-25%, and the content of microcrystalline cellulose is not less than 75%;
the preparation method of the microcrystalline cellulose comprises the following steps: soaking wood pulp in a hydrochloric acid solution with the concentration of 7.5-15.0% for 10-60 s, pressing the soaked wood pulp to dryness, aging for 24-48 hours at the temperature of 30-60 ℃, then soaking the aged wood pulp in water, adding a sodium hydroxide solution to neutralize to pH 5-8, homogenizing by a high-speed homogenizer to obtain microcrystalline cellulose suspension, and performing filter pressing, washing and drying on the microcrystalline cellulose suspension to obtain microcrystalline cellulose.
2. The method for producing a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product according to claim 1, wherein: the average length of the microcrystalline cellulose is not more than 10 mu m, and the particle size of the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product is not more than 100 meshes.
3. The method for producing a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product according to claim 1, wherein: the viscosity of the hydroxyethyl carboxymethyl cellulose is 50-6000 cps, the substitution degree is 1.5-2.0, and the molar substitution degree is 2.0-2.5.
4. The method for producing a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product according to claim 1, wherein: the solid content of the slurry is 15-25%.
5. The method for producing a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product according to claim 1, wherein: the spray drying treatment is completed by a centrifugal spray dryer; the spray drying process comprises the steps of: starting a centrifugal spray dryer, setting the air inlet temperature to be 160-180 ℃, starting to pump the slurry prepared in the step S1 when the air outlet temperature reaches 100 ℃, controlling the feeding speed to keep the air outlet temperature to be 90-100 ℃, collecting the sprayed material, and sieving the material with a 100-mesh sieve to obtain the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product.
6. The method for producing a microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product according to claim 1, wherein: the viscosity of the 1% aqueous solution of the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product is 40-5000 cps, and the pH is 5-8.
7. A microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product produced by the method of any of claims 1 to 6.
8. A solid formulation characterized in that: comprising the microcrystalline cellulose-hydroxyethyl carboxymethyl cellulose co-processed product of claim 7.
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| JPS5535047A (en) * | 1978-09-06 | 1980-03-11 | Asahi Chem Ind Co Ltd | Dry syrup |
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| CN105085992B (en) * | 2015-09-16 | 2017-12-29 | 珠海市东辰医药科技有限公司 | A kind of preparation technology of modified microcrystalline cellulose |
| CN106146675B (en) * | 2016-08-16 | 2019-01-18 | 河南正弘药用辅料有限公司 | A kind of microcrystalline cellulose production technology |
| RU2669845C1 (en) * | 2018-01-25 | 2018-10-16 | Общество с ограниченной ответственностью "Петровский фарватер" | Method of continuous hydrolysis for the production of microcrystalline cellulose |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5535047A (en) * | 1978-09-06 | 1980-03-11 | Asahi Chem Ind Co Ltd | Dry syrup |
| CN104592400A (en) * | 2015-01-23 | 2015-05-06 | 湖州展望天明药业有限公司 | Preparation method of microcrystalline cellulose |
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