CN117205334B - Berberine-loaded montmorillonite composite material and preparation method and application thereof - Google Patents
Berberine-loaded montmorillonite composite material and preparation method and application thereof Download PDFInfo
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- CN117205334B CN117205334B CN202311299669.0A CN202311299669A CN117205334B CN 117205334 B CN117205334 B CN 117205334B CN 202311299669 A CN202311299669 A CN 202311299669A CN 117205334 B CN117205334 B CN 117205334B
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- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 title claims abstract description 159
- 229910052901 montmorillonite Inorganic materials 0.000 title claims abstract description 134
- YBHILYKTIRIUTE-UHFFFAOYSA-N berberine Chemical compound C1=C2CC[N+]3=CC4=C(OC)C(OC)=CC=C4C=C3C2=CC2=C1OCO2 YBHILYKTIRIUTE-UHFFFAOYSA-N 0.000 title claims abstract description 98
- QISXPYZVZJBNDM-UHFFFAOYSA-N berberine Natural products COc1ccc2C=C3N(Cc2c1OC)C=Cc4cc5OCOc5cc34 QISXPYZVZJBNDM-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229940093265 berberine Drugs 0.000 title claims abstract description 98
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011159 matrix material Substances 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 10
- 239000003814 drug Substances 0.000 claims abstract description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 34
- -1 cation modified montmorillonite Chemical class 0.000 claims description 32
- 238000006243 chemical reaction Methods 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 27
- 150000001768 cations Chemical class 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 20
- 238000000926 separation method Methods 0.000 claims description 20
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000011780 sodium chloride Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- 238000005470 impregnation Methods 0.000 claims description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 12
- 229920000858 Cyclodextrin Polymers 0.000 claims description 11
- 238000006482 condensation reaction Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 235000019270 ammonium chloride Nutrition 0.000 claims description 10
- 238000009830 intercalation Methods 0.000 claims description 10
- 230000002687 intercalation Effects 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001694 spray drying Methods 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 7
- 230000006698 induction Effects 0.000 claims description 7
- 230000010355 oscillation Effects 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- 235000019353 potassium silicate Nutrition 0.000 claims description 7
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical group [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- 239000003093 cationic surfactant Substances 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 208000004429 Bacillary Dysentery Diseases 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 208000005577 Gastroenteritis Diseases 0.000 claims description 3
- 206010017915 Gastroenteritis shigella Diseases 0.000 claims description 3
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 claims description 3
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 3
- 229920002961 polybutylene succinate Polymers 0.000 claims description 3
- 239000004631 polybutylene succinate Substances 0.000 claims description 3
- 201000005113 shigellosis Diseases 0.000 claims description 3
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 claims description 3
- 206010010741 Conjunctivitis Diseases 0.000 claims description 2
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- 201000002014 Suppurative Otitis Media Diseases 0.000 claims description 2
- 125000002091 cationic group Chemical group 0.000 claims description 2
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- 239000011229 interlayer Substances 0.000 abstract description 18
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
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- 241000894006 Bacteria Species 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 229910052622 kaolinite Inorganic materials 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 1
- 241000224489 Amoeba Species 0.000 description 1
- 241001480043 Arthrodermataceae Species 0.000 description 1
- 239000001263 FEMA 3042 Substances 0.000 description 1
- 238000012404 In vitro experiment Methods 0.000 description 1
- 241000589902 Leptospira Species 0.000 description 1
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 1
- 206010057190 Respiratory tract infections Diseases 0.000 description 1
- 206010039587 Scarlet Fever Diseases 0.000 description 1
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- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
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- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 150000001767 cationic compounds Chemical class 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 238000001246 colloidal dispersion Methods 0.000 description 1
- 230000037304 dermatophytes Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
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- 239000001257 hydrogen Substances 0.000 description 1
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- 238000000338 in vitro Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
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- 229930013397 isoquinoline alkaloid Natural products 0.000 description 1
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- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000000242 pagocytic effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
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- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
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- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
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- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
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- JFJZZMVDLULRGK-URLMMPGGSA-O tubocurarine Chemical compound C([C@H]1[N+](C)(C)CCC=2C=C(C(=C(OC3=CC=C(C=C3)C[C@H]3C=4C=C(C(=CC=4CCN3C)OC)O3)C=21)O)OC)C1=CC=C(O)C3=C1 JFJZZMVDLULRGK-URLMMPGGSA-O 0.000 description 1
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Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
- Nitrogen Condensed Heterocyclic Rings (AREA)
Abstract
The invention relates to the technical field of montmorillonite modification, and particularly discloses a berberine-loaded montmorillonite composite material, and a preparation method and application thereof. The invention carries out surface activation treatment on montmorillonite to obtain montmorillonite with uniform performance and a certain micropore structure; na + and NH 4 + are passively embedded into montmorillonite in an electrode pressurizing mode, so that interlayer distance of the montmorillonite is greatly increased; the water washing is followed by dehydration treatment to remove the attached water and free water, thereby facilitating the water absorption in the later stage; the loading capacity of berberine is further improved by constructing a supermolecular network; and (3) immersing the montmorillonite matrix in berberine solution to embed berberine into montmorillonite, so as to obtain the berberine-loaded montmorillonite composite material. When the berberine-loaded montmorillonite composite material is used for preparing medicines, the local concentration of the main component berberine can be increased, the acting time can be prolonged, the treatment effect can be improved, and the berberine-loaded montmorillonite composite material has important clinical application value and wide application prospect.
Description
Technical Field
The invention relates to the technical field of montmorillonite modification, in particular to a berberine-loaded montmorillonite composite material, and a preparation method and application thereof.
Background
Berberine, also called berberine, is a quaternary ammonium alkaloid separated from rhizoma Coptidis, and is a main effective component of rhizoma Coptidis for resisting bacteria. The antibacterial agent has broad antibacterial spectrum, has antibacterial effect on various gram-positive and gram-negative bacteria in vitro, and can be used for inhibiting bacteria at low concentration and bacteria at high concentration; has certain inhibiting effects on influenza virus, amoeba protozoa, leptospira and certain dermatophytes; in vitro experiments prove that berberine can enhance phagocytic capacity of leucocytes and hepatic reticuloendothelial system; can be used for treating gastroenteritis, bacillary dysentery, etc., and also has therapeutic effect on pulmonary tuberculosis, scarlet fever, acute tonsillitis, and respiratory tract infection. Berberine belongs to isoquinoline alkaloid, is indissolvable in water, and has low bioavailability; berberine is a cationic compound and is a substrate for bacterial multidrug resistance pumps (MDRs), and is therefore very easily excreted by MDRs, making it difficult to enter cells. Therefore, although the berberine-containing traditional Chinese medicine preparation has been applied to clinical antimicrobial treatment, the berberine as an active ingredient has very limited antibacterial capability, poor oral absorption, short retention in tissues after injection administration and short blood concentration maintenance time.
Montmorillonite is a layered mineral composed of superfine hydrous aluminosilicate particles, also called kaolinite and microcrystalline kaolinite, is a main component of bentonite which is formed by alteration of igneous rocks such as volcanic coagulants in alkaline environment, has a molecular formula of (Na, ca) 0.33(Al,Mg)2[Si4O10](OH)2·nH2 O, is an aluminum oxide octahedron in the middle, and is a clay mineral with a three-layer lamellar structure composed of silicon oxide tetrahedron up and down, contains water and some exchange cations between crystal structures, has higher ion exchange capacity and higher water absorption expansion capacity. The montmorillonite crystal belongs to a monoclinic water-containing layered structure silicate mineral. The montmorillonite has fine particles of about 0.2-1 μm and colloidal dispersion property. Montmorillonite has a larger surface area, a stronger adsorption capacity, a higher cation exchange capacity and a larger layer space (0.9-1.3 nm) to accommodate organic drug molecules than other clay minerals. Montmorillonite powder is a pure natural preparation, is not absorbed after being taken, does not enter blood circulation, is very safe to take, and has been developed into an adjuvant with multiple purposes from a simple antidiarrheal.
However, due to the aggregation state and the hydrophilic oleophobicity of the self-stacking crystals of the montmorillonite, the montmorillonite is difficult to effectively disperse, and release and absorption of active ingredients are affected, so that the use and application effects of the montmorillonite are limited. In the prior art, the interlayer spacing of montmorillonite is improved by modifying montmorillonite with tannic acid, quaternary ammonium salt and the like, but the modifying effect is still required to be further improved.
Disclosure of Invention
Aiming at the problems, the invention provides a berberine-loaded montmorillonite composite material, and a preparation method and application thereof, so as to improve the interlayer spacing of montmorillonite, increase the embedding amount and uniformity of berberine in a montmorillonite structure, and further improve the antibacterial effect and the time of the drug effect.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
The invention provides a preparation method of a berberine-loaded montmorillonite composite material, which comprises the following steps:
S1, adding montmorillonite and a cationic surfactant into an alkaline water solution, performing first impregnation, performing solid-liquid separation, adding a dispersing agent, grinding, and freeze-drying to obtain surface modified montmorillonite;
S2, cold press molding the surface modified montmorillonite, taking the surface modified montmorillonite as one end of an electrode, putting the surface modified montmorillonite and a platinum electrode into a mixed aqueous solution of sodium chloride and ammonium chloride, applying voltage to perform cation induction intercalation reaction, performing solid-liquid separation, performing cation dealkalization reaction on the obtained solid, washing with water, and drying to obtain cation modified montmorillonite;
s3, dissolving the cation modified montmorillonite and carboxymethyl cyclodextrin in polybutylene succinate, uniformly mixing, performing condensation reaction, and performing solid-liquid separation to obtain a montmorillonite matrix;
S4, adding berberine and a dispersing agent into absolute ethyl alcohol, and uniformly mixing to obtain berberine solution;
S5, adding the montmorillonite matrix into the berberine solution, performing second impregnation, and spray drying to obtain the berberine-loaded montmorillonite composite material.
The steps S1 to S3 and the step S4 are not in sequence.
Compared with the prior art, the preparation method of the berberine-loaded montmorillonite composite material provided by the invention comprises the steps of firstly carrying out surface modification on montmorillonite, and carrying out surface activation treatment on montmorillonite to obtain montmorillonite with uniform performance and a certain microporous structure, and improving the specific surface area of the montmorillonite by grinding to obtain more regular montmorillonite with uniform fineness; then, na + and NH 4 + are passively induced and embedded into the montmorillonite in an electrode pressurizing mode, and meanwhile, alkali adsorbed in a part of surface modification process is removed, so that the interlayer distance of the montmorillonite is greatly increased; then the dissolution effect of Na +、NH4 + and residual alkali is improved through the cation dealkalization reaction, and the interlayer substances are emptied; then Na + and NH 4 + are washed off, and a dehydration effect (removing attached water and free water) is achieved through drying, so that water absorption in the later period is facilitated; the supramolecular network is constructed through the condensation reaction of carboxymethyl cyclodextrin and cationic modified montmorillonite, so that the loading capacity of the subsequent berberine is further improved, the local concentration of the berberine is relatively increased and the action time is prolonged in the release process of the berberine, the concentration of the drug acting on bacteria is further improved, and the antibacterial effect is enhanced; finally, the montmorillonite matrix is immersed in the berberine solution to embed the berberine into the interlayer and micropore of the montmorillonite and the supermolecular network, thus obtaining the berberine-loaded montmorillonite composite material. The preparation method of the berberine-loaded montmorillonite composite material provided by the invention is simple and convenient to operate, safe and nontoxic, and has excellent intercalation effect.
Preferably, in step S1, the cationic surfactant includes at least one of cetyltrimethylammonium bromide, tetradecyltrimethylammonium chloride, dodecyltrimethylammonium chloride or dodecyltrimethylammonium bromide.
Preferably, in step S1, the aqueous alkali solution is 3wt% to 8wt% sodium hydroxide solution.
Preferably, in step S1, the mass volume ratio of the montmorillonite, the cationic surfactant and the alkali aqueous solution is 100g (3-8 g) (0.8-1.2) L.
The preferred surface modifying substance and the specific dosage thereof of the invention finish the activation treatment of the montmorillonite, further increase the specific surface area of the montmorillonite, obtain a more stable micropore structure and a more uniform interlayer spacing, and provide preconditions for the subsequent treatment.
Preferably, in step S1, the first impregnation is ultrasonic oscillation impregnation, the ultrasonic frequency is 20-30 kHz, the temperature is 30-50 ℃, and the time is 30-50 min.
The invention can further reduce the agglomeration of montmorillonite and increase the fluidity and diffusion effect while improving the surface modification efficiency through ultrasonic oscillation treatment.
Preferably, in step S1, the dispersant is water glass.
Preferably, in the step S1, the addition amount of the dispersant is 1.0% to 1.5% of the mass of the montmorillonite.
According to the invention, water glass is added as a structure protective agent during grinding, so that the agglomeration of montmorillonite can be effectively prevented, and the dispersibility of montmorillonite is improved.
Preferably, in step S1, the rotational speed of the polishing is 2500 to 2900rpm, and the time is 30 to 50 minutes.
Preferably, in step S1, the temperature of the freeze-drying is-40 to-20 ℃ and the time is 24 to 30 hours.
Preferably, in step S1, the surface-modified montmorillonite has a particle size of 150 to 180nm.
Illustratively, in step S2, the surface-modified montmorillonite is cold-pressed into an annular cake shape. The annular cake-shaped surface modified montmorillonite can increase the embedding amount of subsequent Na + and NH 4 +.
In step S2, the pressure of the cold press molding is 30 to 50MPa.
The invention can ensure that the surface modified montmorillonite keeps the shape of a ring cake and is not loose in the process of cation dealkalization reaction by controlling the pressure of cold press molding; meanwhile, the catalyst is easy to loosen to powder after the cation dealkalization reaction.
Preferably, in the step S2, the concentration of NaCl in the mixed aqueous solution of sodium chloride and ammonium chloride is 15wt% to 20wt%, and the concentration of NH 4 Cl is 5wt% to 8wt%.
According to the invention, by limiting the concentration of NaCl and NH 4 Cl, na + and NH 4 + can be embedded into the microporous structure and interlayer of montmorillonite as much as possible in an electrode pressurizing mode, so that alkali adsorbed in the surface modification process is replaced, and the interlayer distance of the montmorillonite is further increased.
In the step S2, the amount of the mixed aqueous solution is not required, and the surface-modified montmorillonite formed by cold pressing can be immersed.
Preferably, in step S2, the voltage of the cation-induced intercalation reaction is 3 to 5V, and the time is 3 to 6 hours.
Preferably, in the step S2, the cationic dealkalization reaction is performed under an inert atmosphere, the temperature is 120-150 ℃, and the time is 30-60 min.
In step S2, the inert atmosphere is an argon atmosphere.
According to the invention, through controlling the conditions of the cation dealkalization reaction, under an inert atmosphere and a certain pressure, the dissolution efficiency of Na + and NH 4 + can be improved, the dissolution effect can be further increased, the substances between layers can be emptied, and a space is provided for the subsequent embedding of berberine.
In step S2, the termination condition of the water washing is exemplified by a pH of 7.5 to 7.2.
Preferably, in step S2, the drying temperature is 120-140 ℃ and the drying time is 8-10 hours.
Na + and NH 4 + are removed through water washing, and montmorillonite with a microporous structure and an enlarged interlayer spacing is obtained; the dehydration effect is achieved by controlling the drying condition so as to remove the attached water and free water in the montmorillonite, thereby facilitating the water absorption in the later stage.
Preferably, in the step S3, the mass volume ratio of the cationic modified montmorillonite, the carboxymethyl cyclodextrin and the polybutylene succinate is 10g (1.0-1.5 g) and 2-4 mL.
Preferably, in step S3, the temperature of the condensation reaction is 50-80 ℃, the pH is 7.5-8.5, and the time is 90-120 min.
According to the invention, by controlling the addition amount of each raw material and the condition of condensation reaction in the step S3, a supermolecular network structure can be further self-assembled through intermolecular hydrogen bonds on the basis of not changing the micropore structure and interlayer distance of the cation modified montmorillonite, the modified structure of the montmorillonite is taken as a main part, the supermolecular network structure is taken as an auxiliary part, and the supermolecular network structure is used for loading berberine, and the montmorillonite and cyclodextrin can be simultaneously taken as drug carriers. The inventor finds through a large number of experiments that if the dosage of carboxymethyl cyclodextrin is increased, the micropore structure and part of the layer structure of the cation modified montmorillonite are blocked, the obtaining of the supermolecular network structure is insufficient to compensate the damage loss of the cation modified montmorillonite structure, the embedding amount of the subsequent berberine is further adversely affected, and the action effect is poor.
Preferably, in step S4, the dispersing agent includes polyethylene glycol.
Preferably, in the step S4, the mass volume ratio of the berberine, the dispersing agent and the absolute ethyl alcohol is 10g (2-3 g) (50-80) mL.
Preferably, in the step S5, the mass volume ratio of the montmorillonite matrix to the berberine solution is 1g (15-20) mL.
Preferably, in step S5, the temperature of the second impregnation is 50-60 ℃ and the time is 30-60 min.
Preferably, in step S5, the spray drying conditions include: the inlet temperature is 200-240 ℃, the outlet temperature is 110-120 ℃, and the feeding amount is 1800-1850 ml/h.
The second aspect of the invention provides the berberine-loaded montmorillonite composite material prepared by the preparation method of the berberine-loaded montmorillonite composite material.
Compared with the prior art, the berberine-loaded montmorillonite composite material provided by the invention increases the interlayer spacing of montmorillonite, increases the embedding amount and uniformity of berberine in a montmorillonite structure, and further improves the antibacterial effect and the time of the drug effect. The example results show that the interlayer spacing of montmorillonite in the berberine-loaded montmorillonite composite material provided by the invention can reach more than 2.14.
Preferably, the mass ratio of montmorillonite to berberine in the berberine-loaded montmorillonite composite material is 1 (1.5-2.0).
The third aspect of the invention provides the berberine-loaded montmorillonite composite material prepared by the preparation method of the berberine-loaded montmorillonite composite material or the application of the berberine-loaded montmorillonite composite material in preparing medicines for treating gastroenteritis, bacillary dysentery intestinal infection, conjunctivitis or suppurative otitis media.
When the berberine-loaded montmorillonite composite material is applied to corresponding medicaments, the invention can increase the local concentration of the main component berberine, prolong the acting time and improve the treatment effect, and has important clinical application value and wide application prospect.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In order to better illustrate the present invention, the following examples are provided for further illustration.
Example 1
The embodiment provides a preparation method of a berberine-loaded montmorillonite composite material, which comprises the following steps:
S1, adding 100g of montmorillonite and 5g of cetyltrimethylammonium bromide into 1L of 5wt% sodium hydroxide solution, carrying out ultrasonic oscillation (ultrasonic frequency is 24 kHz), carrying out first impregnation at 38 ℃ for 45min, carrying out solid-liquid separation, putting into an aqueous sand mill (model ZW-0.3L, kunshan Kagaku mechanical science and technology Co., ltd.), adding water glass with the mass of 1.2% of montmorillonite, grinding at 2800rpm for 35min, and carrying out freeze drying at-35 ℃ for 26h to obtain the surface modified montmorillonite with the particle size of 160 nm.
S2, cold pressing the surface modified montmorillonite into a ring cake shape under the pressure of 45MPa, taking one end of the electrode, putting the ring cake shape and the platinum electrode into a mixed aqueous solution of sodium chloride and ammonium chloride (the concentration of NaCl is 17wt percent and the concentration of NH 4 Cl is 6wt percent), adding 4V voltage to carry out cation induction intercalation reaction for 5h, carrying out solid-liquid separation, putting the obtained ring cake-shaped montmorillonite matrix into a reaction kettle, introducing argon, carrying out cation dealkalization reaction at 140 ℃ for 40min, washing with water until the pH value is 7.3, grinding the mixture into powder with the particle size of 160nm, and drying at 133 ℃ for 9h to obtain the cation modified montmorillonite.
S3, dissolving 100g of the cation modified montmorillonite and 12g of carboxymethyl cyclodextrin in 25mL of PBS, regulating the pH value to 8.0, uniformly mixing, carrying out condensation reaction at 60 ℃ for 110min, and carrying out solid-liquid separation to obtain a montmorillonite matrix.
S4, adding 10g of berberine and 2.2g of polyethylene glycol into 60mL of absolute ethyl alcohol, and uniformly mixing to obtain berberine solution.
Steps S1 to S3 and step S4 are not in sequence.
S5, adding 1g of the montmorillonite matrix into 17mL of the berberine solution, carrying out second soaking for 50min at 53 ℃, and putting into a small spray dryer (model GY9000, guarson biotechnology (Shanghai) limited company) for spray drying (inlet temperature is 210 ℃, outlet temperature is 113 ℃, and feeding amount is 1820 mL/h) to obtain the berberine-loaded montmorillonite composite material.
Example 2
The embodiment provides a preparation method of a berberine-loaded montmorillonite composite material, which comprises the following steps:
S1, adding 100g of montmorillonite and 7g of tetradecyl trimethyl ammonium chloride into 1.1L of 6wt% sodium hydroxide solution, carrying out ultrasonic oscillation (ultrasonic frequency is 27 kHz), carrying out first impregnation at 44 ℃ for 35min, carrying out solid-liquid separation, putting into an aqueous sand mill (model ZW-0.3L, kunshan Kagaku mechanical science and technology Co., ltd.), adding water glass with the mass of 1.3% of montmorillonite, grinding for 45min at 2600rpm, and carrying out freeze drying at-28 ℃ for 28h to obtain the surface modified montmorillonite with the particle size of 170 nm.
S2, cold pressing the surface modified montmorillonite into a ring cake shape under the pressure of 38MPa, taking one end of the electrode, putting the ring cake shape and the platinum electrode into a mixed aqueous solution of sodium chloride and ammonium chloride (the concentration of NaCl is 19wt percent and the concentration of NH 4 Cl is 7wt percent), adding 4V voltage to carry out cation induction intercalation reaction for 4 hours, carrying out solid-liquid separation, putting the obtained ring cake-shaped montmorillonite matrix into a reaction kettle, introducing argon, carrying out cation dealkalization reaction at 130 ℃ for 50 minutes, washing with water until the pH value is 7.4, grinding the mixture into powder with the particle size of 170nm, and drying at 137 ℃ for 9 hours to obtain the cation modified montmorillonite.
S3, dissolving 100g of the cation modified montmorillonite and 13.5g of carboxymethyl cyclodextrin in 33mL of PBS, regulating the pH value to 8.0, uniformly mixing, carrying out condensation reaction at 70 ℃ for 100min, and carrying out solid-liquid separation to obtain a montmorillonite matrix.
S4, adding 10g of berberine and 2.7g of polyethylene glycol into 70mL of absolute ethyl alcohol, and uniformly mixing to obtain berberine solution.
Steps S1 to S3 and step S4 are not in sequence.
S5, adding 1g of the montmorillonite matrix into 18mL of the berberine solution, performing second soaking at 57 ℃ for 40min, and placing into a small spray dryer (model GY9000, guarson biotechnology (Shanghai) limited company) for spray drying (inlet temperature is 230 ℃, outlet temperature is 117 ℃, and feeding amount is 1840 mL/h) to obtain the berberine-loaded montmorillonite composite material.
Example 3
The embodiment provides a preparation method of a berberine-loaded montmorillonite composite material, which comprises the following steps:
S1, adding 100g of montmorillonite and 3g of dodecyl trimethyl ammonium chloride into 0.8L of 3wt% sodium hydroxide solution, carrying out ultrasonic oscillation (ultrasonic frequency is 20 kHz), carrying out first impregnation at 30 ℃ for 50min, carrying out solid-liquid separation, putting into an aqueous sand mill (model ZW-0.3L, kunshan Kagaku mechanical science and technology Co., ltd.) and adding water glass with the mass of 1.0% of montmorillonite, grinding for 50min at a rotating speed of 2500rpm, and carrying out freeze drying at-20 ℃ for 30h to obtain the surface modified montmorillonite with the particle size of 150 nm.
S2, cold pressing the surface modified montmorillonite into a ring cake shape under the pressure of 32MPa, taking one end of the electrode, putting the ring cake shape and the platinum electrode into a mixed aqueous solution of sodium chloride and ammonium chloride (the concentration of NaCl is 15wt percent and the concentration of NH 4 Cl is 8wt percent), adding 3V voltage to carry out cation induction intercalation reaction for 6h, carrying out solid-liquid separation, putting the obtained ring cake-shaped montmorillonite matrix into a reaction kettle, introducing argon, carrying out cation dealkalization reaction at 120 ℃ for 60min, washing with water until the pH value is 7.2, grinding the mixture into powder with the particle size of 150nm, and drying at 120 ℃ for 10h to obtain the cation modified montmorillonite.
S3, dissolving 100g of the cation modified montmorillonite and 10g of carboxymethyl cyclodextrin in 20mL of PBS, regulating the pH value to 7.6, uniformly mixing, carrying out condensation reaction at 50 ℃ for 120min, and carrying out solid-liquid separation to obtain a montmorillonite matrix.
S4, adding 10g of berberine and 2.0g of polyethylene glycol into 50mL of absolute ethyl alcohol, and uniformly mixing to obtain berberine solution.
Steps S1 to S3 and step S4 are not in sequence.
S5, adding 1g of the montmorillonite matrix into 15mL of the berberine solution, carrying out second soaking for 30min at 50 ℃, and putting into a small spray dryer (model GY9000, coron Biotechnology (Shanghai) limited) for spray drying (inlet temperature is 200 ℃, outlet temperature is 110 ℃, and feeding amount is 1800 mL/h) to obtain the berberine-loaded montmorillonite composite material.
Example 4
The embodiment provides a preparation method of a berberine-loaded montmorillonite composite material, which comprises the following steps:
S1, adding 100g of montmorillonite and 8g of dodecyl trimethyl ammonium bromide into 1.2L of 8wt% sodium hydroxide solution, carrying out ultrasonic oscillation (ultrasonic frequency is 30 kHz), carrying out first impregnation at 50 ℃ for 30min, carrying out solid-liquid separation, putting into an aqueous sand mill (model ZW-0.3L, kunshan Kagaku mechanical science and technology Co., ltd.), adding water glass with the mass of 1.5% of montmorillonite, grinding at 2900rpm for 30min, and freeze-drying at-40 ℃ for 24h to obtain the surface modified montmorillonite with the particle size of 180 nm.
S2, cold pressing the surface modified montmorillonite into a ring cake shape under the pressure of 50MPa, taking one end of the electrode, putting the ring cake shape and the platinum electrode into a mixed aqueous solution of sodium chloride and ammonium chloride (the concentration of NaCl is 20wt%, and the concentration of NH 4 Cl is 5wt%) together, adding 5V voltage to carry out cation induction intercalation reaction for 3h, carrying out solid-liquid separation, putting the obtained ring cake-shaped montmorillonite matrix into a reaction kettle, introducing argon, carrying out cation dealkalization reaction for 30min at 150 ℃, washing with water until the pH value is 7.5, grinding the mixture into powder with the particle size of 180nm, and drying at 140 ℃ for 8h to obtain the cation modified montmorillonite.
S3, dissolving 100g of the cation modified montmorillonite and 15g of carboxymethyl cyclodextrin in 40mL of PBS, regulating the pH value to 8.4, uniformly mixing, carrying out condensation reaction at 80 ℃ for 90min, and carrying out solid-liquid separation to obtain a montmorillonite matrix.
S4, adding 10g of berberine and 3.0g of polyethylene glycol into 80mL of absolute ethyl alcohol, and uniformly mixing to obtain berberine solution.
Steps S1 to S3 and step S4 are not in sequence.
S5, adding 1g of the montmorillonite matrix into 20mL of the berberine solution, performing second soaking at 60 ℃ for 30min, and placing into a small spray dryer (model GY9000, guarson biotechnology (Shanghai) limited company) for spray drying (inlet temperature is 240 ℃, outlet temperature is 120 ℃, and feeding amount is 1850 mL/h) to obtain the berberine-loaded montmorillonite composite material.
Comparative example 1
This comparative example provides a method for preparing berberine-loaded montmorillonite composite material, similar to example 1, except that step S1 is omitted. The method comprises the following specific steps:
S1, cold pressing montmorillonite into annular cake shape under 45MPa pressure, taking one end of the electrode, putting the annular cake shape and the platinum electrode into a mixed aqueous solution of sodium chloride and ammonium chloride (the concentration of NaCl is 17wt percent, the concentration of NH 4 Cl is 6wt percent), adding 4V voltage to carry out cation induction intercalation reaction for 5h, carrying out solid-liquid separation, putting the obtained annular cake-shaped montmorillonite matrix into a reaction kettle, introducing argon, carrying out cation adsorption reaction at 140 ℃ for 40min, washing until the pH value is 7.3, grinding to powder with the particle size of 160nm, and drying at 133 ℃ for 9h to obtain the cation modified montmorillonite.
S2 to S4 are the same as steps S3 to S5 of example 1, and will not be described again.
Comparative example 2
This comparative example provides a method for preparing berberine-loaded montmorillonite composite material, similar to example 1, except that step S2 is omitted. The method comprises the following specific steps:
S1, the same as step S1 of embodiment 1, will not be repeated.
S2, dissolving 100g of the surface modified montmorillonite and 12g of carboxymethyl cyclodextrin in 25mL of PBS, regulating the pH value to 8.0, uniformly mixing, carrying out condensation reaction at 60 ℃ for 110min, and carrying out solid-liquid separation to obtain a montmorillonite matrix.
S3 to S4 are the same as steps S4 to S5 of example 1, and will not be described again.
Comparative example 3
This comparative example provides a method for preparing berberine-loaded montmorillonite composite material, similar to example 1, except that step S3 is omitted. The method comprises the following specific steps:
S1 to S2 are the same as steps S1 to S2 of example 1, and will not be described again.
S3, the same as step S4 of embodiment 1, will not be repeated.
S4, adding 1g of the cation modified montmorillonite (serving as a montmorillonite matrix) into 17mL of the berberine solution, carrying out second soaking for 50min at 53 ℃, and carrying out spray drying (with an inlet temperature of 210 ℃ and an outlet temperature of 113 ℃ and a feeding amount of 1820 mL/h) by a small spray dryer (model GY9000, coron Biotechnology (Shanghai) Co., ltd.) to obtain the berberine-loaded montmorillonite composite material.
Effect example
XRD detection is carried out on the berberine-loaded montmorillonite composite materials prepared in examples 1-4 and comparative examples 1-3 and raw montmorillonite, and the detection wavelength is 0.15406nm. The montmorillonite has a characteristic peak on a 001 crystal face, d (001) value represents interlayer spacing of the montmorillonite, and the peak position of the mapping interlayer spacing of the berberine-loaded montmorillonite composite material and the calculated interlayer spacing are shown in Table 1. As can be seen from Table 1, the berberine-loaded montmorillonite composite material provided by the invention has larger embedding amount and interlayer spacing.
TABLE 1
| Project | 2θ(°) | Interlayer distance (nm) |
| Example 1 | 4.05 | 2.18 |
| Example 2 | 4.03 | 2.20 |
| Example 3 | 4.11 | 2.14 |
| Example 4 | 4.09 | 2.16 |
| Comparative example 1 | 6.12 | 1.44 |
| Comparative example 2 | 6.01 | 1.60 |
| Comparative example 3 | 5.84 | 1.82 |
| Raw montmorillonite | 6.96 | 1.27 |
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and principles of the invention.
Claims (9)
1. The preparation method of the berberine-loaded montmorillonite composite material is characterized by comprising the following steps of:
S1, adding montmorillonite and a cationic surfactant into an alkaline water solution, performing first impregnation, performing solid-liquid separation, adding a dispersing agent, grinding, and freeze-drying to obtain surface modified montmorillonite;
S2, cold press molding the surface modified montmorillonite, taking the surface modified montmorillonite as one end of an electrode, putting the surface modified montmorillonite and a platinum electrode into a mixed aqueous solution of sodium chloride and ammonium chloride, applying voltage to perform cation induction intercalation reaction, performing solid-liquid separation, performing cation dealkalization reaction on the obtained solid, washing with water, and drying to obtain cation modified montmorillonite;
S3, dissolving the cation modified montmorillonite and carboxymethyl cyclodextrin in polybutylene succinate, uniformly mixing, performing condensation reaction, and performing solid-liquid separation to obtain a montmorillonite matrix; the temperature of the condensation reaction is 50-80 ℃, the pH is 7.5-8.5, and the time is 90-120 min;
S4, adding berberine and a dispersing agent into absolute ethyl alcohol, and uniformly mixing to obtain berberine solution;
S5, adding the montmorillonite matrix into the berberine solution, performing second impregnation, and spray drying to obtain the berberine-loaded montmorillonite composite material.
2. The method for preparing berberine-loaded montmorillonite composite material according to claim 1, wherein in step S1, the cationic surfactant comprises at least one of cetyltrimethylammonium bromide, tetradecyltrimethylammonium chloride, dodecyltrimethylammonium chloride or dodecyltrimethylammonium bromide.
3. The method for preparing berberine-loaded montmorillonite composite material according to claim 1 or 2, wherein in step S1, the aqueous alkali solution is 3wt% to 8wt% sodium hydroxide solution; and/or
In the step S1, the mass volume ratio of the montmorillonite, the cationic surfactant and the alkaline aqueous solution is 100g (3-8 g) (0.8-1.2) L.
4. The method for preparing berberine-loaded montmorillonite composite material according to claim 1, wherein in the step S1, the first impregnation is ultrasonic oscillation impregnation, the ultrasonic frequency is 20-30 khz, the temperature is 30-50 ℃ and the time is 30-50 min; and/or
In the step S1, the dispersing agent is water glass; and/or
In the step S1, the addition amount of the dispersing agent is 1.0% -1.5% of the mass of montmorillonite; and/or
In the step S1, the particle size of the surface modified montmorillonite is 150-180 nm.
5. The method for preparing berberine-loaded montmorillonite composite material according to claim 1, wherein in the step S2, the concentration of NaCl in the mixed aqueous solution of sodium chloride and ammonium chloride is 15wt% to 20wt%, and the concentration of NH4Cl is 5wt% to 8wt%; and/or
In the step S2, the voltage of the cation induced intercalation reaction is 3-5V, and the time is 3-6 h; and/or
In the step S2, the cationic dealkalization reaction is carried out in an inert atmosphere, the temperature is 120-150 ℃, and the time is 30-60 min.
6. The method for preparing berberine-loaded montmorillonite composite material according to claim 1, wherein in step S4, the dispersing agent comprises polyethylene glycol; and/or
In the step S4, the mass volume ratio of the berberine, the dispersing agent and the absolute ethyl alcohol is 10g (2-3 g) (50-80 mL); and/or
In the step S5, the mass volume ratio of the montmorillonite matrix to the berberine solution is 1g (15-20) mL; and/or
In the step S5, the temperature of the second impregnation is 50-60 ℃ and the time is 30-60 min.
7. The berberine-loaded montmorillonite composite material is characterized by being prepared by the preparation method of the berberine-loaded montmorillonite composite material according to any one of claims 1-6.
8. The berberine-loaded montmorillonite composite material according to claim 7, wherein the mass ratio of montmorillonite to berberine in the berberine-loaded montmorillonite composite material is 1 (1.5-2.0).
9. The use of the berberine-loaded montmorillonite composite material prepared by the preparation method of the berberine-loaded montmorillonite composite material of any one of claims 1-6 or the berberine-loaded montmorillonite composite material of any one of claims 7-8 in preparing a medicament for treating gastroenteritis, bacillary dysentery intestinal infection, conjunctivitis or suppurative otitis media.
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