CN107348507A - 载β‑胡萝卜素聚乳酸(PLA)纳米粒的制备 - Google Patents
载β‑胡萝卜素聚乳酸(PLA)纳米粒的制备 Download PDFInfo
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Abstract
本发明主要涉水处理领域,设计出一种方案,具体是制备了可食用性,生物可降解性的载β‑胡萝卜素的聚乳酸纳米粒。该方法包括以下步骤:(1)聚乳酸(PLA)的制备;(2)乳化剂(PVA)的制备;(3)载β胡萝卜素的聚乳酸(PLA)纳米粒的制备,最终得到产物。此方法具有对设备要求低,操作简单,制作周期短,可食用,无毒无害,有良好的生物可降解性和生物相容性等优点。该方法可以制备出的可食用载β‑胡萝卜素的聚乳酸纳米粒。
Description
技术领域
本发明主要应用于为了制备了可食用性,生物可降解性的载β-胡萝卜素的聚乳酸纳米粒。
背景技术
水是生命之源,水资源安全和处理与地球健康、能源产品和经济发展有千丝万缕的关系。 20世纪以来,在提供公众饮水健康,农业发展等方面,水供应***和废水处理技术取得了长足进步,与之同时,随着我国人民的生活水平迅速提高,受西方国家文化和消费观念的影响,我国城镇居民的生活习惯逐渐接受了西方科学的生活方式,饮用水源污染引发的饮用水水质问题日益受到人们的重视,采用家用***是目前人们解决用水水质问题普遍的选择。而众多水处理应用的材料中,纳米材料作为尖端材料的代表,一起优越的性能,广阔的发展空间,尤其引人注目。
目前常用的饮用水净水深度处理技术有深层接触过滤技术、膜过滤技术、复合金属滤料过滤技术。其中膜过滤技术是最近几年在我国开始投入工程应用的一种水处理技术。根据膜孔径不同,可分为微滤、超滤、反渗透技术。根据滤膜的材料,可分为有机滤膜和无机滤膜。膜处理技术主要利用膜的物理截留作用去除水中污染物,该技术的去除对象主要取决于物质的几何尺寸。有机膜和无机膜相比,具有过流面积大,处理能力大,制造工艺成熟的优点。无机膜耐冲击性能差,易破碎、易堵塞、难清洗。所以我们的荧光PLA作为新型的纳米粒,可以更好的检验膜孔径,以此达到产品的优化和改进。
随着社会经济的发展,目前世界水污染的问题越来越严重,水处理问题也变得越来越严峻。中国的废、污水排放量极大,约占世界的10%以上,而在我国,国内的生产总值约占世界的5.5%。但是,中国城市的污水处理率只有36%,未经处理的污水大多数都是直接排放到江河湖海,破坏了生态环境,使环境愈发恶劣,所以,污水处理技术尤为重要。另外,我们的饮用水源污染引起的饮用水水质问题也日益收到人们的重视,采用家用***是目前人们解决用水水质问题普遍的选择。
β-胡萝卜素即维他命A,可随时转换成维生素A在身体需要的时候,有助维持眼睛健康。增强身体免疫***,对心脏和其他器官提供抗氧化保护,有助于保持皮肤和头发的健康,食用油溶性色素,可以作为可食用性的示踪器。
聚乳酸[Poly(lactic Acid),PLA]是一种高分子聚合物,分子式为(C3H4O2)n,聚乳酸则是由丙交酯开环聚合,或者是乳酸直接聚合而成。聚乳酸具有良好的生物可降解性和生物相容性,能被降解成二氧化碳和水,中间产物乳酸也是体内正常的糖代谢产物,不会在重要器官聚集,在生物医学、材料等方面都有广泛的应用,是理想的绿色高分子材料。
目前,膜过滤技术在很多方面都具有极其广泛的应用,它的原理和特点能够帮我们解决一些实际生活中存在的问题。除了应用在水处理方面,纳米膜过滤技术在处理化工合成废液中的应用还可以有效的回收无法生物降解的有机物,浓缩有价值的有机物等等;膜处理技术主要利用膜的物理截留作用去除水中污染物,该技术的去除对象主要取决于物质的几何尺寸。
通过结合β-胡萝卜素、聚乳酸和膜过滤的优点,我们做出了可食用性,生物可降解性的载β-胡萝卜素的聚乳酸纳米粒。
本发明一种载β-胡萝卜素的聚乳酸纳米粒,在用膜过滤水问题上提供了新思路。
发明内容
为了解决现有技术中存在的问题,本的发明发明人进行了广泛深入的研究,最终得到了本发明。
本发明的一个目的是用在膜过滤水问题上,制备了可食用性,生物可降解性的载β-胡萝卜素的聚乳酸纳米粒。
本发明的目的是通过以下技术方案实现的。
步骤1、载β胡萝卜素的聚乳酸(PLA)纳米粒的制备:
1)天平称取PLA,红棕色β胡萝卜素加入到溶剂二氯甲烷中,超声约5分钟至完全溶解,此时溶液呈橘黄色,备用;
2)天平称取乳化剂(PVA或TPGS),加蒸馏水,搅拌加热至完全溶解,备用;
3)室温下,将步骤1)缓慢倒入步骤2)中,可以肉眼看到橘黄色油状液滴产生,使用超声波细胞粉粹机对其进行超声搅拌约2min,至不再有油滴残留,制得橘黄色均匀乳液,备用;
4)将步骤3)所得乳液旋转蒸发约30分钟,至溶剂完全挥发,此时,溶液变为稍微浅一点的桔黄色,备用;
5)室温下,使用离心机将步骤4)离心,使用去离子水洗涤所得沉淀,洗涤三次,离心三次,第三次洗涤离心之后,离心所得的清液几乎没有颜色,呈白色透明状,说明洗涤干净,备用;
6)将得到的沉淀溶于约少许纯水中,所得溶液冷冻干燥2天,即得到桔黄色粉末状的载β胡萝卜素的PLA纳米粒;
本发明所采用的方法为改良的单乳法,但并不限于单乳法,也可以采用复乳法。
本发明提供的纳米粒的制备方法简单易控,重复性好,可实现工业化规模,高效率生产出质量稳定的产品。纳米粒的稳定性可通过粒径和电位的测定结果得到证明。取载β胡萝卜素的PLA纳米粒适量,自然干燥后在热场扫描电镜下(SEM)下观察,粒径在100~300nm之间,如图1、图2、图3所示。
本发明的纳米粒与现有技术相比,创新点是:纳米粒稳定性好,且具有可食用性,生物可降解性的载β-胡萝卜素的纳米粒。
附图说明
图1为载β胡萝卜素的PLA纳米粒的粒径分布图;
图2为载β胡萝卜素的PLA纳米粒的电位分布图;
图3为载β胡萝卜素的PLA纳米粒的扫描电镜图片;
图4为载β胡萝卜素的PLA纳米粒的蒸馏水中的分散图片;
图5为载β胡萝卜素的PLA纳米粒的从中空纤维膜过滤后的图片;
图6为载β胡萝卜素的PLA纳米粒通过0.45微米滤膜过滤后的图片;
具体实施方式
下面结合实例对本发明作进一步说明。
实施例1
称取20mg PLA、1mgβ胡萝卜素,加入6ml二氯甲烷,超声使材料和β胡萝卜素充分溶解,天平称取乳化剂PVA 0.5g,溶于100ml蒸馏水中,使其完全溶解,将配置好的材料倒入30ml乳化剂中,使用超声波细胞粉粹机对其进行超声搅拌约2min,制得橘黄色均匀乳液,旋转蒸发乳液30min,后用蒸馏水洗涤三次再离心,加入少许蒸馏水,4℃密封保存。
冻干工艺:用0.45μm微孔滤膜过滤除菌,过滤后得混悬液装入培养皿中,置冰箱中-20℃预冻2h,然后放入冷冻干燥机中-50℃、48h,得桔黄色疏松状载β胡萝卜素的PLA纳米粒,该冻干材料加入2mL蒸馏水经超声可于1min内完全分散。
结果:制得载β胡萝卜素的PLA纳米粒的平均粒径为340.7±6.1nm平均电位为-19.5mV
实施例2
称取20mg PLA、1mgβ胡萝卜素,加入6ml二氯甲烷,超声使材料和β胡萝卜素充分溶解,天平称取乳化剂TPGS 0.5g,溶于100ml蒸馏水中,使其完全溶解,将配置好的材料倒入30ml乳化剂中,使用超声波细胞粉粹机对其进行超声搅拌约2min,制得橘黄色均匀乳液,旋转蒸发乳液30min,后用蒸馏水洗涤三次再离心,加入少许蒸馏水,4℃密封保存。
冻干工艺:用0.45μm微孔滤膜过滤除菌,过滤后得混悬液装入培养皿中,置冰箱中-20℃预冻2h,然后放入冷冻干燥机中-50℃、48h,得桔黄色疏松状载β胡萝卜素的PLA纳米粒,该冻干材料加入2mL蒸馏水经超声可于1min内完全分散。
结果:制得载β胡萝卜素的PLA纳米粒的平均粒径为319.1±4.4nm平均电位为-36.4mV
实施例3
称取20mg PLA、1mgβ胡萝卜素,加入6ml二氯甲烷,超声使材料和β胡萝卜素充分溶解,天平称取乳化剂PVA 0.66g,溶于100ml蒸馏水中,使其完全溶解,将配置好的材料倒入30ml乳化剂中,使用超声波细胞粉粹机对其进行超声搅拌约2min,制得橘黄色均匀乳液,旋转蒸发乳液30min,后用蒸馏水洗涤三次再离心,加入少许蒸馏水,4℃密封保存。
冻干工艺:用0.45μm微孔滤膜过滤除菌,过滤后得混悬液装入培养皿中,置冰箱中-20℃预冻2h,然后放入冷冻干燥机中-50℃、48h,得桔黄色疏松状载β胡萝卜素的PLA纳米粒,该冻干材料加入2mL蒸馏水经超声可于1min内完全分散。
结果:制得载β胡萝卜素的PLA纳米粒的平均粒径为211.2±3.4nm平均电位为-19.8mV
实施例4
称取20mg PLA、1mgβ胡萝卜素,加入6ml二氯甲烷,超声使材料和β胡萝卜素充分溶解,天平称取乳化剂TPGS 0.66g,溶于100ml蒸馏水中,使其完全溶解,将配置好的材料倒入30ml乳化剂中,使用超声波细胞粉粹机对其进行超声搅拌约2min,制得橘黄色均匀乳液,旋转蒸发乳液30min,后用蒸馏水洗涤三次再离心,加入少许蒸馏水,4℃密封保存。
冻干工艺:用0.45μm微孔滤膜过滤除菌,过滤后得混悬液装入培养皿中,置冰箱中-20℃预冻2h,然后放入冷冻干燥机中-50℃、48h,得桔黄色疏松状载β胡萝卜素的PLA纳米粒,该冻干材料加入2mL蒸馏水经超声可于1min内完全分散。
结果:制得载β胡萝卜素的PLA纳米粒的平均粒径为209.1±2.3nm平均电位为-39.4mV
实施例5
称取40mg PLA、1mgβ胡萝卜素,加入6ml二氯甲烷,超声使材料和β胡萝卜素充分溶解,天平称取乳化剂TPGS 0.66g,溶于100ml蒸馏水中,使其完全溶解,将配置好的材料倒入30ml乳化剂中,使用超声波细胞粉粹机对其进行超声搅拌约2min,制得橘黄色均匀乳液,旋转蒸发乳液30min,后用蒸馏水洗涤三次再离心,加入少许蒸馏水,4℃密封保存。
冻干工艺:用0.45μm微孔滤膜过滤除菌,过滤后得混悬液装入培养皿中,置冰箱中-20℃预冻2h,然后放入冷冻干燥机中-50℃、48h,得桔黄色疏松状载β胡萝卜素的PLA纳米粒,该冻干材料加入2mL蒸馏水经超声可于1min内完全分散。
结果:制得载β胡萝卜素的PLA纳米粒的平均粒径为340.5.1±5.3nm平均电位为-30.1mV
实施例6
称取40mg PLA、4mgβ胡萝卜素,加入6ml二氯甲烷,超声使材料和β胡萝卜素充分溶解,天平称取乳化剂TPGS 0.66g,溶于100ml蒸馏水中,使其完全溶解,将配置好的材料倒入30ml乳化剂中,使用超声波细胞粉粹机对其进行超声搅拌约2min,制得橘黄色均匀乳液,旋转蒸发乳液30min,后用蒸馏水洗涤三次再离心,加入少许蒸馏水,4℃密封保存。
冻干工艺:用0.45μm微孔滤膜过滤除菌,过滤后得混悬液装入培养皿中,置冰箱中-20℃预冻2h,然后放入冷冻干燥机中-50℃、48h,得桔黄色疏松状载β胡萝卜素的PLA纳米粒,该冻干材料加入2mL蒸馏水经超声可于1min内完全分散。
结果:制得载β胡萝卜素的PLA纳米粒的平均粒径为437.7±6.3nm平均电位为-27.1mV。
Claims (8)
1.为了制备了可食用性,生物可降解性的载β-胡萝卜素的聚乳酸(PLA)纳米粒,一种新型的可食用性的纳米粒,包括以下步骤:
步骤1、载β胡萝卜素的聚乳酸(PLA)纳米粒的制备:
1)天平称取PLA,红棕色β胡萝卜素加入到溶剂二氯甲烷中,超声约5分钟至完全溶解,此时溶液呈橘黄色,备用;
2)天平称取乳化剂(PVA或TPGS),加蒸馏水,搅拌加热至完全溶解,备用;
3)室温下,将步骤1)缓慢倒入步骤2)中,可以肉眼看到橘黄色油状液滴产生,使用超声波细胞粉粹机对其进行超声搅拌约2min,至不再有油滴残留,制得橘黄色均匀乳液,备用;
4)将步骤3)所得乳液旋转蒸发约30分钟,至溶剂完全挥发,此时,溶液变为稍微浅一点的桔黄色,备用;
5)室温下,使用离心机将步骤4)离心,使用去离子水洗涤所得沉淀,洗涤三次,离心三次,第三次洗涤离心之后,离心所得的清液几乎没有颜色,呈白色透明状,说明洗涤干净,备用;
6)将得到的沉淀溶于约少许纯水中,所得溶液冷冻干燥2天,即得到桔黄色粉末状的载β胡萝卜素的PLA纳米粒;
步骤2、载β胡萝卜素的聚乳酸(PLA)纳米粒的表征:
采用纳米粒度、Zeta电位、扫描电子显微镜对载β胡萝卜素的聚乳酸(PLA)纳米粒进行检测:根据纳米粒度来表征粒度的大小,Zeta电位来测其稳定性,扫描电子显微镜使我们可以直观的观测到纳米微粒的原始粒径和形貌。
2.根据权利要求1所述的制备方法,其特征在于:包载的是可食用性,生物可降解性β-胡萝卜素。
3.根据权利要求1所述的制备方法,其特征在于:乳化剂包括TPGS和PVA,配得得到的乳化剂质量百分浓度为0.33%、0.5%、0.66%,优选乳化剂为TPGS质量百分浓度为0.66%。
4.根据权利要求1所述的制备方法,其特征在于:所述的聚乳酸(PLA)和β胡萝卜素混合物其质量比为20∶1。
5.根据权利要求1所述的制备方法,其特征在于:所述的载β胡萝卜素的聚乳酸(PLA)纳米粒的制备中,适宜的超声条件为70W-80W。
6.根据权利要求1所述的制备方法,其特征在于:离心分离后的产物用去离子水洗涤3次,除去未反应的物质。
7.根据权利要求1所述的制备方法,其特征在于:制备得到的载β胡萝卜素的聚乳酸(PLA)纳米粒。
8.根据权利要求1所述的制备方法,其特征在于:制备得到的载β胡萝卜素的聚乳酸(PLA)纳米粒冻干粉末。
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