CN116570551A - 适用于3d打印的草药温敏凝胶组合物及其制备方法和应用 - Google Patents

适用于3d打印的草药温敏凝胶组合物及其制备方法和应用 Download PDF

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CN116570551A
CN116570551A CN202310528357.6A CN202310528357A CN116570551A CN 116570551 A CN116570551 A CN 116570551A CN 202310528357 A CN202310528357 A CN 202310528357A CN 116570551 A CN116570551 A CN 116570551A
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powder
herbal
printing
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蔡萌萌
张丽
朱悦
耿婷
李澄琦
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Nanjing University of Chinese Medicine
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Abstract

本发明公开了一种适用于3D打印的草药温敏凝胶组合物，其按质量百分计，所述的组合物包括：草药粉8‑60％；萃提性凝胶剂38‑91.9％；稳定剂0.1‑2％；其中，所述萃提性凝胶剂为非水溶性凝胶剂。制备步骤为：将草药材用粉碎机粉碎、过筛40目以上筛网，得草药粉；将萃提性凝胶剂加热至高于熔点以上5‑20℃区间，加入草药粉和稳定剂，充分混匀至无肉眼可视颗粒或块状物，凝胶中草药粉粒径缩小50％以上，冷却至室温，即得适用于3D打印的草药温敏凝胶组合物。

Description

适用于3D打印的草药温敏凝胶组合物及其制备方法和应用
技术领域
本发明属于中药药剂学、3D打印及日用化学品领域，具体涉及一种适用于3D打印的草药温敏凝胶组合物及其制备方法和应用。
背景技术
凝胶是一类含有两组分或两组分以上的包含液体的半固体胶冻和其干燥体系(干凝胶)的大分子网络体系的通称。《中国药典》2000版二部中定义了凝胶剂：“凝胶剂是指药物与能形成凝胶的辅料制成的均一、混悬或乳剂型的乳胶稠厚液体或半固体制剂。常见凝胶基质一般由水与甘油、丙二醇、纤维素衍生物、卡波姆、海藻酸盐、果胶、明胶、黄原胶、琼脂、丙烯酸树脂和聚乙烯醇等水溶或水溶胀型物质混合而成。在现代药学中以凝胶为基质的缓释、控释剂型,如胃滞留控释系统、凝胶骨架片、外用凝胶剂等得到了全面的研究，适用于凝胶给药系统的药物可以从口腔、鼻腔、眼粘膜、消化道粘膜、阴道、直肠、皮肤等多种途径给药[中成药,2003,25(4):328]。低纤维含量的水果浆料也可与食品胶制成复合水凝胶以用于食品3D打印[现代食品科技,2020,36(8):202]。
草药(草本中药材)中含有大量的纤维素类物质，中成药制剂一般先将其有效成分提取出来再进行制剂加工。中国专利CN110075080A公开了一种中药提取物的3D打印速溶片，先将中药有效成分以水提取为浸膏、通过喷雾干燥制备为粉剂，再与山梨醇、棉籽糖、聚维酮粘合剂和羧甲基淀粉钠崩解剂等混合制粒为3D打印药剂材料。该类工艺过程冗长，且只利用了中药材中少量的水溶性分子，而大量的非水溶性和大分子有效成分，如生物碱、黄酮、精油、糖甙、蛋白质和纤维素类等，均未得到充分利用，造成了中药资源的极大浪费，还造成了固体废弃物污染环境。
因此，草药粉的直接3D打印则成为3D中药药剂学的挑战，其存在的主要技术难点，则是植物性草药粉体的高密度纤维网络中普遍含有大量的水溶解和水溶胀性物质，如小分子药物、淀粉、多糖、木质素、单宁等，使用含水量高的常规凝胶剂，很容易使草药粉体颗粒团聚或溶胀[高校化学工程学报,2009,23(2):199]，甚至事先粉碎至微米级的草药粉也会溶胀至毫米级，如用于3D打印墨水配方中，极易造成打印头的堵塞[Small,2020,16(31):1907212]。
发明内容
为解决上述技术问题，本发明提出一种用于3D打印的草药温敏凝胶组合物及其制备方法和应用。
本发明的目的是通过以下技术方案来实现的：
一种适用于3D打印的草药温敏凝胶组合物，按质量百分计，所述的组合物包括：
草药粉 8-60％；
萃提性凝胶剂 38-91.9％；
稳定剂 0.1-2％；
其中，所述萃提性凝胶剂为非水溶性凝胶剂。
所述草药粉的粒径为100-500μm的草药粉。
所述草药粉包括艾叶粉、藿香粉、佩兰粉、青蒿粉、板蓝根粉、金银花粉、连翘粉、野菊花粉、蒲公英粉中的一种或几种。
所述萃提性凝胶剂包括蜂蜡、棕榈蜡、米糠蜡、脂肪酸、脂肪酸甘油酯、神经酰胺、月桂酰二乙醇胺、谷甾醇、谷维素中的一种或几种。
所述稳定剂包括生育酚乙酸酯、维生素C、维生素E、特丁基对苯二酚、丁基羟基茴香醚、没食子酸丙酯中的一种或几种。
所述的适用于3D打印的草药温敏凝胶组合物的制备方法，包括如下步骤：
A、将草药材粉碎、过筛，得草药粉；
B、将萃提性凝胶剂加热至高于熔点以上5-20℃区间，加入草药粉和稳定剂，充分混匀至无肉眼可视颗粒或块状物凝胶，草药粉粒径缩小50％以上；
C、冷却至环境温度，即得适用于3D打印的草药温敏凝胶组合物。
所述的适用于3D打印的草药温敏凝胶组合物在制备抗菌和抗病毒摆件或饰品中的应用也属于本发明的保护范围。
3D打印所用设备为热熔型3D打印机，所述热熔型3D打印机的打印头孔径为0.1～0.5mm。
与现有技术相比，本发明具有如下有益效果：
1)由于草药粉中含有大量的纤维素物质，在含水凝胶作用下产生众多强氢键结合，很容易团聚或溶胀，即使粉碎至微米级的草药粉也会溶胀至毫米级，黏结性亦会增大导致结团，在3D打印中极易造成打印头(Φ0.1～0.5mm)的堵塞。而本发明所述萃提性凝胶剂包括蜂蜡、棕榈蜡、米糠蜡、脂肪酸、脂肪酸甘油酯、神经酰胺、月桂酰二乙醇胺、谷甾醇和谷维素等，基本不与草药粉中纤维素产生氢键结合，不会溶胀草药粉体，并且因其熔体具有萃提草药粉中小分子物质作用，使草药粉内容物质减少而产生收缩作用，草药粉粒径缩小50％以上，确保不堵塞3D打印机的打印头(Φ0.1～0.5mm)；且具有原位萃提草药粉中小分子物质和温敏凝固化性能；
2)选材主要来源于天然物质，对家居环境友好安全；
3)制备工艺简单、无资源浪费与废料排放；
4)可利用其温敏热熔特点进行3D打印，打印件可作为摆件或饰品应用于抗菌和抗病毒领域。
附图说明
通过阅读参照以下附图对非限制性实施例所作的详细描述，本发明的其它特征、目的和优点将会变得更明显：
图1为实施例1草药温敏凝胶组合物的扫描电子显微镜照片；
图2为各组实施例和对比实施例的粒径变化比较图。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明，但不以任何形式限制本发明。应当指出的是，对本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变化和改进,包括各实例间的任意组合。
下述实施例和对比例中：
蜂蜡熔点63℃；
脂肪酸甘油酯熔点34℃；
棕榈蜡熔点82℃。
实施例1-3
实施例1-3提供一种适用于3D打印的草药温敏凝胶组合物，分别按表1中的组分及含量进行备料。
表1实施例1-3各组分及组分含量(质量百分比；％)
实施例1的制备方法如下：
A、将艾叶用粉碎机粉碎、过筛40目筛网，得艾叶粉(粒径425μm以下)；
B、将蜂蜡加热至75℃，加入艾叶粉和生育酚乙酸酯，充分混匀至无肉眼可视颗粒或块状物；
C、冷却至室温，即得适用于3D打印的草药温敏凝胶组合物。
实施例2的制备方法如下：
A、将藿香用粉碎机粉碎、过筛80目筛网，得藿香粉(粒径180μm以下)。
B、将棕榈蜡加热至95℃，加入藿香粉和维生素E，充分混匀至无肉眼可视颗粒或块状物。
C、冷却至室温，即得适用于3D打印的草药温敏凝胶组合物。
实施例3的制备方法如下：
A、将复合草药材(艾叶:藿香:佩兰:青蒿＝1:1:1:1)用粉碎机粉碎、过筛80目筛网，得复合草药粉(粒径180μm以下)。
B、将脂肪酸甘油酯加热至40℃，加入复合草药粉和丁基羟基茴香醚，充分混匀至无肉眼可视颗粒或块状物。
C、冷却至室温，即得适用于3D打印的草药温敏凝胶组合物。
对比例1
本对比例与实施例1的区别在于，将蜂蜡替换为3％质量浓度卡拉胶水凝胶
制备步骤为：
(1)将艾叶用粉碎机粉碎、过筛40目筛网，得艾叶粉粒径425μm以下；
(2)在卡拉胶水凝胶(3％浓度)中加入艾叶粉和生育酚乙酸酯，混合20min。
对比例1中，步骤(2)混合后发现粉体明显溶胀，粒径高达2mm，较凝胶化前增大了371％，完全不能符合WiibooxSweetin 3D打印机的打印头(Φ0.1～0.5mm)挤出要求。
测试例1
电子显微镜观察将实施例1-3和对比例的草药温敏凝胶组合物置于电子显微镜下观察。相关测试结果见下表2和图1-2。
根据表2中实施例1-3的结果来看，采用本发明的配方和工艺制备的草药温敏凝胶组合物都具有较小的粒径，不易溶胀。因为本发明采用的萃提性凝胶剂为不溶胀草药粉体，用于3D打印时不易堵塞打印头，且具有原位萃提草药粉中小分子物质和温敏凝固化性能。
图1为实施例1将草药温敏凝胶组合物置于电子显微镜观察，粉体粒径为50μm以下，较凝胶化前缩小了88％，达到了WiibooxSweetin 3D打印机的打印头(Φ0.2mm)挤出要求。
实施例2所制备的草药温敏凝胶组合物置于电子显微镜观察，粉体粒径为45μm以下，较凝胶化前缩小了75％，达到了WiibooxSweetin 3D打印机的打印头(Φ0.1mm)挤出要求。
实施例3所制备的草药温敏凝胶组合物置于电子显微镜观察，粉体粒径为70μm以下，较凝胶化前缩小了61％，达到了WiibooxSweetin 3D打印机的打印头(Φ0.3mm)挤出要求。
图2为各组实施例和对比例的粒径变化比较图。
需要理解的是，本发明并不局限于上述特定实施方式，本领域技术人员可以在权利要求的范围内做出各种变形或修改，这并不影响本发明的实质内容。

Claims (9)

1.一种适用于3D打印的草药温敏凝胶组合物，其特征在于，按质量百分计，所述的组合物包括：
草药粉 8-60％；
萃提性凝胶剂 38-91.9％；
稳定剂 0.1-2％；
其中，所述萃提性凝胶剂为非水溶性凝胶剂。
2.根据权利要求1所述的适用于3D打印的草药温敏凝胶组合物，其特征在于，所述草药粉的粒径为100-500μm。
3.根据权利要求1所述的适用于3D打印的草药温敏凝胶组合物，其特征在于，所述草药粉包括艾叶粉、藿香粉、佩兰粉、青蒿粉、板蓝根粉、金银花粉、连翘粉、野菊花粉、蒲公英粉中的一种或几种。
4.根据权利要求1所述的适用于3D打印的草药温敏凝胶组合物，其特征在于，所述萃提性凝胶剂包括蜂蜡、棕榈蜡、米糠蜡、脂肪酸、脂肪酸甘油酯、神经酰胺、月桂酰二乙醇胺、谷甾醇、谷维素中的一种或几种。
5.根据权利要求1所述的适用于3D打印的草药温敏凝胶组合物，其特征在于，所述稳定剂包括生育酚乙酸酯、维生素C、维生素E、特丁基对苯二酚、丁基羟基茴香醚、没食子酸丙酯中的一种或几种。
6.根据权利要求1所述的适用于3D打印的草药温敏凝胶组合物，其特征在于，3D打印所用设备为热熔型3D打印机。
7.根据权利要求6所述的适用于3D打印的草药温敏凝胶组合物，其特征在于，所述热熔型3D打印机的打印头孔径为0.1～0.5mm。
8.一种如权利要求1-7中任一项所述的适用于3D打印的草药温敏凝胶组合物的制备方法，其特征在于，包括如下步骤：
A、将草药材粉碎、过筛，得草药粉；
B、将萃提性凝胶剂加热至高于熔点以上5-20℃区间，加入草药粉和稳定剂，充分混匀至无肉眼可视颗粒或块状物凝胶，草药粉粒径缩小50％以上；
C、冷却至环境温度，即得适用于3D打印的草药温敏凝胶组合物。
9.一种如权利要求1-7中任一项所述的适用于3D打印的草药温敏凝胶组合物在制备抗菌和抗病毒摆件或饰品中的应用。
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