CN113577027A - 一种聚合物稳定无机抗菌纳米粒子的强化制备方法 - Google Patents

一种聚合物稳定无机抗菌纳米粒子的强化制备方法 Download PDF

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CN113577027A
CN113577027A CN202110647152.0A CN202110647152A CN113577027A CN 113577027 A CN113577027 A CN 113577027A CN 202110647152 A CN202110647152 A CN 202110647152A CN 113577027 A CN113577027 A CN 113577027A
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徐益升
张卯升
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Nantong Zhongsheng Industry And Trade Co ltd
East China University of Science and Technology
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East China University of Science and Technology
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K9/00—Medicinal preparations characterised by special physical form
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    • A61K9/141—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
    • A61K9/146—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with organic macromolecular compounds
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    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • A01N25/10—Macromolecular compounds
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/06—Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
    • A61K33/10—Carbonates; Bicarbonates
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/24—Heavy metals; Compounds thereof
    • A61K33/34—Copper; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00—Medicinal preparations containing inorganic active ingredients
    • A61K33/24—Heavy metals; Compounds thereof
    • A61K33/38—Silver; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract

本发明涉及一种聚合物稳定无机抗菌纳米粒子的强化制备方法，包括如下步骤：通过FNP法制备1号溶液，2号溶液，通过设置一定流速，在泵的推动下，将该两溶液以两股流体在双通道射流混合器中发生瞬间碰撞混合获得聚合物稳定无机抗菌纳米粒子。本发明运用瞬时纳米沉淀法制备一系列不同粒径的球形含银纳米粒子，通过调控流速实现对纳米粒子尺寸的调控，进而对纳米粒子的抗菌性能进行控制，该方法简单高效，在抗菌领域具有潜在的应用价值与研发前景。

Description

一种聚合物稳定无机抗菌纳米粒子的强化制备方法
技术领域
本发明涉及一种纳米载药体系制备技术，具体为运用瞬时纳米沉淀法制备一系列具有抗菌性能的纳米粒子，属于新材料领域。
背景技术
近年来，纳米材料与纳米技术以其独特的优势迅速发展并获得广泛应用，其中，纳米抗菌材料除纳米材料的基本性能如表面效应、小尺寸效应、量子尺寸效应和宏观隧道效应外，还能在与病原微生物接触时发挥显著的生物效应，比同类抗菌材料有更强的抗菌活性，且安全性高、加工方便、耐热性好、不易产生抗药性及广谱抗菌性，在抗菌材料领域有着广泛的应用前景与发展潜力。
传统的纳米粒子制备方法有共沉淀法、水热法、溶剂热法、溶胶-凝胶法，这些方法具备耗时长、纳米粒子尺寸分布不均匀的缺点，瞬时纳米沉淀法自2003年被报到以来，在纳米粒子的制备与载药粒子的包覆方面均发挥着重要作用，该方法利用高剪切力快速混合纳米粒子，操作简单，大大缩短纳米粒子的制备时间，制备的纳米粒子尺寸均一，得到广泛应用。
本发明利用瞬时纳米沉淀法强化制备聚合物稳定无机抗菌纳米粒子，使得纳米粒子的制备时长大大缩短，且纳米粒子尺寸及性能可得到有效控制。该方法操作简单，易于控制，具有广阔的发展前景与研发价值。
发明内容
鉴于以上问题，本发明的目的在于提供一种聚合物稳定无机抗菌纳米粒子的强化制备方法及其在抗菌领域的重要应用。
本发明的具体技术方案是：
一种聚合物稳定无机抗菌纳米粒子的强化制备方法，包括如下步骤：
通过FNP法制备1号溶液，2号溶液，通过设置一定流速，在泵的推动下，将该两溶液以两股流体在双通道射流混合器中发生瞬间碰撞混合获得聚合物稳定无机抗菌纳米粒子；
所述1号溶液为AgNO3、AgCl、CuCl2、MgCl2、FeCl2或FeCl3的一种与透明质酸、丙烯酸或羧基化的葡聚糖中的一种聚合物的混合液，2号溶液是NaCl、Na2CO3、Na2SO4或Na2S的一种。
优选的，所述1号溶液是透明质酸和AgNO3的混合液；2号溶液为NaCl。
进一步的，1号溶液的透明质酸分子量范围为5000～450000。
进一步的，所述流速为5～30mL/min。
进一步的，所述瞬间碰撞的混合时间为30～180ms.
本发明制备得到的纳米粒子应用于无机抗菌材料的应用。
本发明的优点体现在：制备出的聚合物稳定无机抗菌纳米粒子粒径分布均匀，稳定性好，耗时短，用于抗菌实验，表现出优良的抗菌活性。
附图说明
图1是制备聚合物稳定无机抗菌纳米粒子的实验装置示意图；
图2是聚合物稳定无机抗菌纳米粒子的透射电子显微镜图；
图3是通过流速调控纳米粒子的粒径；
图4是使用聚合物稳定无机抗菌纳米粒子前后抗菌效果的对比图，左图为涂覆PAA-AgCl纳米粒子的基板，右图为涂覆PAA-AgCl纳米粒子的基板。
具体实施方式
下面，用实施例来进一步说明本发明内容，但本发明的保护范围并不仅限于实施例，对本领域的技术人员在不背离发明精神和保护范围的情况下做出的其他的变化和修改，仍包括在本发明保护范围之内。
实施例1：
制备1、2号液，分别为聚丙烯酸(PAA，1mol/L)与0.01mol/L AgNO3，0.01mol/LNaCl，以24mL/min的流速经过数控注射泵(Harvard Apparatus，PHD 2000)并进入混合器内发生瞬间碰撞混合约为30ms，得到聚丙烯酸稳定的无机纳米粒子PAA-AgCl纳米粒子。
实施例2：
制备1、2号液，分别为透明质酸(1mol/L)与0.015mol/L MgCl2，0.01mol/L Na2CO3，以36mL/min的流速经过数控注射泵(Harvard Apparatus，PHD 2000)并进入混合器内发生瞬间碰撞混合约为20ms，得到聚丙烯酸稳定的无机纳米粒子PAA-MgCO3纳米粒子。
实施例3：
制备1、2号液，分别为葡聚糖(1mol/L)与0.005mol/L CuCl2，0.005mol/L Na2S，以12mL/min的流速经过数控注射泵(Harvard Apparatus,PHD 2000)并进入混合器内发生瞬间碰撞混合约为60ms，得到聚丙烯酸稳定的无机纳米粒子PAA-CuS纳米粒子。
实施例1所使用制备PAA-AgCl纳米粒子的仪器为双通道射流混合器(CID)，如附图1所示。
实施例1产品PAA-AgCl纳米粒子制备完成后进行透射电子显微镜(TEM)分析，结果显示PAA-AgCl纳米粒子粒径分布均匀，在5nm(核结构)左右，有良好的分散性，无明显团聚现象，如附图2所示。
实施例4产品PAA-AgCl纳米粒子制备完成后对其进行抗菌性能测试，采用大肠杆菌为模型细菌对PAA-AgCl纳米粒子的抗菌性能进行研究，首先将未涂布PAA-AgCl纳米粒子的塑料板及涂布PAA-AgCl纳米粒子的塑料板放入121℃的高压灭菌釜中进行灭菌处理，取出后冷却至室温。在1L烧杯中加入自制的载玻片固定器，加入500mL无菌培养液，再将以上两组基板垂直浸入无菌液体培养基中，加入5mL大肠杆菌菌株，将烧杯置于75rpm的振荡器中进行震荡，在28℃下培养24h，将两组基板小心取出，在垂直状态下用滤纸洗掉表面的液体，并在空气中干燥10min以出去表面的水分，随后将5μL 10mg/mL 4，6-二氨基二苯基吲哚水溶液滴加在样品表面对大肠杆菌细胞进行染色，在暗处培育10min后放置在荧光显微镜下进行观察，放大倍数为100倍，根据这些图像分别统计细胞总数。可以观察得到，没有纳米粒子涂覆的塑料板放大10倍，细菌生长快；涂覆纳米粒子塑料板放大10倍无明显细菌，抗菌效果好。如附图4所示。
本发明运用瞬时纳米沉淀法(FNP)制备一系列不同粒径的球形含银纳米粒子，通过调控流速实现对纳米粒子尺寸的调控，进而对纳米粒子的抗菌性能进行控制，该方法简单高效，在抗菌领域具有潜在的应用价值与研发前景。

Claims (6)

1.一种聚合物稳定无机抗菌纳米粒子的强化制备方法，其特征在于，包括如下步骤：
通过FNP法制备1号溶液，2号溶液，通过设置一定流速，在泵的推动下，将该两溶液以两股流体在双通道射流混合器中发生瞬间碰撞混合获得聚合物稳定无机抗菌纳米粒子；
所述1号溶液为AgNO3、AgCl、CuCl2、MgCl2、FeCl2或FeCl3的一种与透明质酸、丙烯酸或羧基化的葡聚糖中的一种聚合物的混合液，2号溶液是NaCl、Na2CO3、Na2SO4或Na2S的一种。
2.根据权利要求1所述的一种聚合物稳定无机抗菌纳米粒子的强化制备方法，其特征在于：所述1号溶液是透明质酸和AgNO3的混合液；2号溶液为NaCl。
3.根据权利要求2所述的一种聚合物稳定无机抗菌纳米粒子的强化制备方法，其特征在于：1号溶液的透明质酸分子量范围为5000～450000。
4.根据权利要求1所述一种聚合物稳定无机抗菌纳米粒子的强化制备方法，其特征在于:所述流速为5～30mL/min。
5.根据权利要求1所述一种聚合物稳定无机抗菌纳米粒子的强化制备方法，其特征在于:所述瞬间碰撞的混合时间为30～180ms。
6.根据权利要求1所述一种聚合物稳定无机抗菌纳米粒子的强化制备方法所制备得到的纳米粒子的应用，其特征在于，将制得的纳米粒子应用于无机抗菌材料的应用。
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