CN108606988A - 一种纳米中药粉的制备方法 - Google Patents
一种纳米中药粉的制备方法 Download PDFInfo
- Publication number
- CN108606988A CN108606988A CN201810218557.0A CN201810218557A CN108606988A CN 108606988 A CN108606988 A CN 108606988A CN 201810218557 A CN201810218557 A CN 201810218557A CN 108606988 A CN108606988 A CN 108606988A
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- chinese medicine
- medicine powder
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- powder
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- 239000003814 drug Substances 0.000 title claims abstract description 43
- 239000000843 powder Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 238000007710 freezing Methods 0.000 claims abstract description 7
- 230000008014 freezing Effects 0.000 claims abstract description 7
- 239000008187 granular material Substances 0.000 claims abstract description 6
- 239000006194 liquid suspension Substances 0.000 claims abstract description 6
- 238000012216 screening Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- -1 polyoxyethylene Polymers 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 241001248610 Ophiocordyceps sinensis Species 0.000 claims description 10
- 235000003143 Panax notoginseng Nutrition 0.000 claims description 9
- 241000180649 Panax notoginseng Species 0.000 claims description 9
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 9
- 229920004890 Triton X-100 Polymers 0.000 claims description 5
- 239000013504 Triton X-100 Substances 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 150000001408 amides Chemical class 0.000 claims description 4
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 4
- 235000019864 coconut oil Nutrition 0.000 claims description 4
- 239000003240 coconut oil Substances 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 150000004665 fatty acids Chemical class 0.000 claims description 4
- 150000002191 fatty alcohols Chemical class 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229920001451 polypropylene glycol Polymers 0.000 claims description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical class CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 3
- 229920001992 poloxamer 407 Polymers 0.000 claims description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 3
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 3
- 229920000053 polysorbate 80 Polymers 0.000 claims description 3
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 240000004638 Dendrobium nobile Species 0.000 claims description 2
- 244000197580 Poria cocos Species 0.000 claims description 2
- 235000008599 Poria cocos Nutrition 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 2
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 235000011132 calcium sulphate Nutrition 0.000 claims description 2
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 2
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 239000004323 potassium nitrate Substances 0.000 claims description 2
- 235000010333 potassium nitrate Nutrition 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 239000001587 sorbitan monostearate Substances 0.000 claims description 2
- 235000011076 sorbitan monostearate Nutrition 0.000 claims description 2
- 229940035048 sorbitan monostearate Drugs 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 2
- 239000011734 sodium Substances 0.000 claims 2
- 229910052708 sodium Inorganic materials 0.000 claims 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims 1
- 239000005642 Oleic acid Substances 0.000 claims 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- PSLWZOIUBRXAQW-UHFFFAOYSA-M dimethyl(dioctadecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC PSLWZOIUBRXAQW-UHFFFAOYSA-M 0.000 claims 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims 1
- 239000012528 membrane Substances 0.000 claims 1
- 235000015424 sodium Nutrition 0.000 claims 1
- 239000000600 sorbitol Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract description 2
- 239000011858 nanopowder Substances 0.000 abstract description 2
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- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000001954 sterilising effect Effects 0.000 description 4
- 239000002562 thickening agent Substances 0.000 description 4
- 241000305492 Gastrodia Species 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
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- 238000000605 extraction Methods 0.000 description 3
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- 239000012535 impurity Substances 0.000 description 3
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
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- ONJQDTZCDSESIW-UHFFFAOYSA-N polidocanol Chemical compound CCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO ONJQDTZCDSESIW-UHFFFAOYSA-N 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
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- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- IEQAICDLOKRSRL-UHFFFAOYSA-N 2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-(2-dodecoxyethoxy)ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethanol Chemical compound CCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO IEQAICDLOKRSRL-UHFFFAOYSA-N 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
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- 239000002202 Polyethylene glycol Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
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- 239000004480 active ingredient Substances 0.000 description 1
- HRHBQGBPZWNGHV-UHFFFAOYSA-N azane;bromomethane Chemical compound N.BrC HRHBQGBPZWNGHV-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- HQPMKSGTIOYHJT-UHFFFAOYSA-N ethane-1,2-diol;propane-1,2-diol Chemical compound OCCO.CC(O)CO HQPMKSGTIOYHJT-UHFFFAOYSA-N 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
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- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 229910017604 nitric acid Inorganic materials 0.000 description 1
- ZPIRTVJRHUMMOI-UHFFFAOYSA-N octoxybenzene Chemical compound CCCCCCCCOC1=CC=CC=C1 ZPIRTVJRHUMMOI-UHFFFAOYSA-N 0.000 description 1
- 229920001993 poloxamer 188 Polymers 0.000 description 1
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- 229910052700 potassium Inorganic materials 0.000 description 1
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- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
Classifications
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- A61K47/26—Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
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Abstract
本发明涉及一种纳米中药粉的制备方法,包括以下步骤:(1)将中药材初步粉碎、筛选,重复多次,得到中药颗粒,烘干待用;(2)将步骤(1)所得的中药颗粒进行冷冻粉碎,同时加入无机盐一起粉碎,得到中药粉;(3)将步骤(2)得到的中药粉用水进行清洗并过滤,然后加入到水中,并添加修饰剂,搅拌得到粉液态混悬液,浓缩,并冷冻干燥,得到所述纳米中药粉。与现有技术相比,本发明的反应温度低,含有的无机盐在低温下结晶后能起到摩擦剂的作用,使得破壁率大大增加;且本发明中制备的纳米粉可以避免中药材高温加工带来的活性成分的损失,又可以充分粉碎,增加吸收效果。
Description
技术领域
本发明涉及中医药技术领域,具体涉及一种纳米中药粉的制备方法。
背景技术
中药材是人们用以防病、治病的特殊商品,如何增加中药材的疗效是当前研究的热点问题。破壁和纳米化已成为流行的加工方式。
超微粉碎技术近十多年在各领域得到了广泛的应用并迅速发展,它能把原材料加工成微米甚至纳米级的微粉。超微粉碎技术在近几年应用于中医药传统领域也得到了广泛的研究与实践,中药材经超微粉碎成微粉后,药材利用率大幅度提高,研究表明超微细化后的中药用量,只相当于原方剂用药量的三分之一甚至十分之一,是有效节省中药材资源的方法,特别是对于稀少珍贵的药用资源具有更大的意义。当前超微粉碎在中药材加工中有应用主是指细胞级微粉碎,主要是将中药材细胞破壁为目的进行粉碎,因此,也称超微粉为破壁粉。中药细胞破壁后,表现出如下优势:大幅度提高其生物利用度;药用利用率提高;节省原料便于应用;药材的均匀度高。与此同时也表现出一些不确定的因素,主要表现为破壁药材中的有效成分的稳定性降低,易吸潮,易氧化,破壁率低、不易长期保存,这是超微粉存在的首要问题。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种稳定性好、吸收度高的纳米中药粉的制备方法。
本发明的目的可以通过以下技术方案来实现:一种纳米中药粉的制备方法,包括以下步骤:
(1)将中药材初步粉碎、筛选,重复多次,得到中药颗粒,烘干待用;
(2)将步骤(1)所得的中药颗粒进行冷冻粉碎,同时加入无机盐一起粉碎,得到中药粉;机盐在低温下结晶后能起到摩擦剂的作用,使得破壁率大大增加。
(3)将步骤(2)得到的中药粉用水进行清洗并过滤,然后加入到水中,并添加修饰剂,搅拌得到粉液态混悬液,浓缩,并冷冻干燥,得到所述纳米中药粉。
所述的初步粉碎在粉碎机中进行,筛选采用500目的筛网,直至所以中药材全部被粉碎透过筛网。先通过粉碎机进行初步粉碎,一方面减少了后续粉碎的负担,另一方面可以使得粉碎更加完全。
所述冷冻粉碎在超低温粉碎仪中进行,利用液氮作为媒介进行冷却,温度为 -60~-30℃,冷冻粉碎的时间为0.5~5h。采用低温粉碎,避免粉碎过程中高温加工带来的活性成分的损失。
所述无机盐包括氯化钠、氯化钾、氯化镁、氯化钙、氯化铝、氯化铵、硝酸钠、硝酸钾、硝酸镁、硝酸钙、硝酸铵、硫酸钠、硫酸钾、硫酸镁、硫酸钙或硫酸铵中的一种或几种混合物。
所述修饰剂包括十六烷基三甲基溴化铵、十二烷基三甲基溴化铵、双十八烷基二甲基溴化铵、十二烷基硫酸钠、十二烷基磺酸钠、十二烷基苯磺酸钠、Triton X-100 (聚乙二醇辛基苯基醚)、Tu-80(聚氧乙烯山梨醇酐单油酸酯),Span-60(山梨醇酐单硬脂酸酯),6501(椰油脂肪酸二乙醇酰胺),AEO-9(脂肪醇聚氧乙烯醚), Brij-35(月桂醇聚氧乙烯醚),Pluronic F68(聚氧乙烯80-聚氧丙烯30-聚氧乙烯80), Pluronic F127(聚氧乙烯100-聚氧丙烯70-聚氧乙烯100)或Pluronic P123(聚氧乙烯20-聚氧丙烯70-聚氧乙烯20)、Tu-80(聚氧乙烯山梨醇酐单油酸酯),6501 (椰油脂肪酸二乙醇酰胺),AEO-9(脂肪醇聚氧乙烯醚),Brij-35(月桂醇聚氧乙烯醚)或Triton X-100(聚乙二醇辛基苯基醚)中的一种或几种混合物。加入无机盐增加摩擦力,粉碎后可以通过水洗去除;加入修饰剂为了表面覆盖有机分子,在水溶液中不易团聚。
所述搅拌的转速为大于1000-10000转/min。
所述浓缩在真空薄膜浓缩机中进行,温度为60~100℃。
所述冷冻干燥在真空冷冻干燥机中进行,温度为-60~-30℃,真空度为 20~100Pa,干燥时间为10~50h。
所述中药材包括三七、天麻、砂仁、云木香、当归、茯苓、石斛或冬虫夏草中的一种。
与现有技术相比,本发明的有益效果体现在以下几方面:
(1)本发明的反应温度低,含有的无机盐在低温下结晶后能起到摩擦剂的作用,使得破壁率大大增加;
(2)本发明中制备的纳米粉可以避免中药材高温加工带来的活性成分的损失,又可以充分粉碎,增加吸收效果;
(3)本发明无需特殊设备,可操作性强,能进一步满足生产和应用的需求。
具体实施方式
下面对本发明的实施例作详细说明,本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
实施例1
将300g鲜三七剪口预处理干净后,使用辐照对鲜三七进行20分钟消毒,灭菌为γ-辐射灭菌,辐照剂量为5KGy。消毒后再用用去离子水洗净,剥去杂质,得到 285g鲜三七。将处理好的285g鲜三七送入粉碎机机进行粉碎,均匀铺平在破壁管道底部,工作时间设置35-40min,完成后使用500目筛对产物进行筛选,如有团聚颗粒物可使用平铲压碎后重复此操作,直至三七粉颗粒均匀无杂质,过筛后得到 260g破壁粉体。然后使用干燥烘箱设置工作温度为60℃之间,烘干时间为1.5-2 小时。待三七粉完全干燥后,将所得产物送入超低温粉碎仪中,使用液氮媒介冷却,设置操作温度-110℃,延时工作时间0.5小时,加入氯化钠,在超低温状态下的粉碎、分散以及萃取后得到250g产物。将产物用水清洗过滤后,配置成质量浓度为50%水溶液,加入250g Span-60,进行10000转/分以上转速的高速搅拌,得到纳米三七粉液态混悬液500g。对混悬液使用真空薄膜浓缩机进行浓缩,浓缩重量比例为2:1,约得到浓缩液245-250g,后置于真空冷冻干燥机中,设置急冻-60℃、真空度100Pa后,干燥10小时,得到纳米化三七干燥粉240-245g。粒径为150纳米。
实施例2
将500g鲜天麻剪口预处理干净后,使用辐照对鲜天麻进行20分钟消毒,灭菌为γ-辐射灭菌,辐照剂量为5KGy。消毒后再用用去离子水洗净,剥去杂质,得到 485g鲜天麻。将处理好的485g鲜天麻送入粉碎机机进行粉碎,均匀铺平在破壁管道底部,工作时间设置35-40min,完成后使用500目筛对产物进行筛选,如有团聚颗粒物可使用平铲压碎后重复此操作,直至天麻粉颗粒均匀无杂质,过筛后得到 460g破壁粉体。然后使用干燥烘箱设置工作温度为100℃之间,烘干时间为1.5-2 小时。待天麻粉完全干燥后,将所得产物送入超低温粉碎仪中,使用液氮媒介冷却,设置操作温度-130℃,延时工作时间0.5小时,加入硝酸钾,在超低温状态下的粉碎、分散以及萃取,后得到450g产物。将产物用水清洗过滤后,配置成质量浓度为30%水溶液,将产物加入450g Pluronic F127,进4000转/分以上转速的高速搅拌,得到纳米天麻粉液态混悬液900g。对混悬液使用真空薄膜浓缩机进行浓缩,浓缩重量比例为2:1,约得到浓缩液445-450g,后置于真空冷冻干燥机中,设置急冻-60℃、真空度100Pa后,干燥10小时,得到纳米化天麻干燥粉440-445g。粒径为68纳米。
实施例3
将1000g鲜冬虫夏草剪口预处理干净后,使用辐照对鲜冬虫夏草进行20分钟消毒,灭菌为γ-辐射灭菌,辐照剂量为5KGy。消毒后再用用去离子水洗净,剥去杂质,得到985g鲜冬虫夏草。将处理好的985g鲜冬虫夏草送入粉碎机机进行粉碎,均匀铺平在破壁管道底部,工作时间设置35-40min,完成后使用500目筛对产物进行筛选,如有团聚颗粒物可使用平铲压碎后重复此操作,直至冬虫夏草粉颗粒均匀无杂质,过筛后得到960g破壁粉体。然后使用干燥烘箱设置工作温度为30℃之间,烘干时间为1.5-2小时。待冬虫夏草粉完全干燥后,将所得产物送入超低温粉碎仪中,使用液氮媒介冷却,设置操作温度-100℃,延时工作时间0.5小时,加入硫酸钠,便于超低温状态下的粉碎、分散以及萃取,后得到950g产物。将产物用水清洗过滤后,配置成质量浓度为30%水溶液,将产物加入950g Tu-80,进行 5000转/分以上转速的高速搅拌,得到纳米冬虫夏草液态混悬液1900g。对混悬液使用真空薄膜浓缩机进行浓缩,浓缩重量比例为2:1,约得到浓缩液945-950g,后置于真空冷冻干燥机中,设置急冻-60℃、真空度100Pa后,干燥10小时,得到纳米化冬虫夏草干燥粉940-945g。粒径为230纳米。
Claims (9)
1.一种纳米中药粉的制备方法,其特征在于,包括以下步骤:
(1)将中药材初步粉碎、筛选,重复多次,得到中药颗粒,烘干待用;
(2)将步骤(1)所得的中药颗粒进行冷冻粉碎,同时加入无机盐一起粉碎,得到中药粉;
(3)将步骤(2)得到的中药粉用水进行清洗并过滤,然后加入到水中,并添加修饰剂,搅拌得到粉液态混悬液,浓缩,并冷冻干燥,得到所述纳米中药粉。
2.根据权利要求1所述的一种纳米中药粉的制备方法,其特征在于,所述的初步粉碎在粉碎机中进行,筛选采用500目的筛网,直至所以中药材全部被粉碎透过筛网。
3.根据权利要求1所述的一种纳米中药粉的制备方法,其特征在于,所述冷冻粉碎在超低温粉碎仪中进行,利用液氮作为媒介进行冷却,温度为-60~-30℃,冷冻粉碎的时间为0.5~5h。
4.根据权利要求1所述的一种纳米中药粉的制备方法,其特征在于,所述无机盐包括氯化钠、氯化钾、氯化镁、氯化钙、氯化铝、氯化铵、硝酸钠、硝酸钾、硝酸镁、硝酸钙、硝酸铵、硫酸钠、硫酸钾、硫酸镁、硫酸钙或硫酸铵中的一种或几种混合物。
5.根据权利要求1所述的一种纳米中药粉的制备方法,其特征在于,所述修饰剂包括十六烷基三甲基溴化铵、十二烷基三甲基溴化铵、双十八烷基二甲基溴化铵、十二烷基硫酸钠、十二烷基磺酸钠、十二烷基苯磺酸钠、聚乙二醇辛基苯基醚、聚氧乙烯山梨醇酐单油酸酯、山梨醇酐单硬脂酸酯、椰油脂肪酸二乙醇酰胺、脂肪醇聚氧乙烯醚、月桂醇聚氧乙烯醚、聚氧乙烯80-聚氧丙烯30-聚氧乙烯80、聚氧乙烯100-聚氧丙烯70-聚氧乙烯100、聚氧乙烯20-聚氧丙烯70-聚氧乙烯20、聚氧乙烯山梨醇酐单油酸酯、椰油脂肪酸二乙醇酰胺、脂肪醇聚氧乙烯醚、月桂醇聚氧乙烯醚或聚乙二醇辛基苯基醚中的一种或几种混合物。
6.根据权利要求1所述的一种纳米中药粉的制备方法,其特征在于,所述搅拌的转速为大于1000-10000转/min。
7.根据权利要求1所述的一种纳米中药粉的制备方法,其特征在于,所述浓缩在真空薄膜浓缩机中进行,温度为60~100℃。
8.根据权利要求1所述的一种纳米中药粉的制备方法,其特征在于,所述冷冻干燥在真空冷冻干燥机中进行,温度为-60~-30℃,真空度为20~100Pa,干燥时间为10~50h。
9.根据权利要求1~8任一所述的一种纳米中药粉的制备方法,其特征在于,所述中药材包括三七、天麻、砂仁、云木香、当归、茯苓、石斛或冬虫夏草中的一种。
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CN115429849A (zh) * | 2022-08-23 | 2022-12-06 | 江西大自然制药有限公司 | 一种固本延龄丸的制备方法 |
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CN115445738B (zh) * | 2022-09-22 | 2023-11-28 | 上海纳米技术及应用国家工程研究中心有限公司 | 一种中草药根茎叶整株的微纳米固态粉体的制备方法及其产品 |
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