CN107961363B - 一种贝壳粉纳米抗菌足浴泡腾片及其制备方法 - Google Patents
一种贝壳粉纳米抗菌足浴泡腾片及其制备方法 Download PDFInfo
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- CN107961363B CN107961363B CN201711183420.8A CN201711183420A CN107961363B CN 107961363 B CN107961363 B CN 107961363B CN 201711183420 A CN201711183420 A CN 201711183420A CN 107961363 B CN107961363 B CN 107961363B
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- Medicinal Preparation (AREA)
Abstract
本发明公开了一种贝壳粉纳米抗菌足浴泡腾片及其制备方法，泡腾片的成分及其重量份为：纳米贝壳粉80‑98份、中药抗菌活性组分2‑20份、PEG6000 5‑10份、酒石酸钠14‑18份、碳酸氢钠20‑30份、聚维酮0.02‑0.04份、水0.8‑1.2份。泡腾片的制备方法为：将贝壳用酸浸泡，洗净，烘干，研磨得粗贝壳粉；然后粉碎得纳米贝壳粉；将中药抗菌活性组分的原料粉碎，煎煮，过滤，浓缩，粉碎；将PEG6000熔融，加入碳酸氢钠，搅拌均匀，粉碎，加入剩余原料，打均匀，压片得足浴泡腾片。本发明泡腾片安全无毒、抗菌谱广、抗菌效率高、稳定性好；其制备方法能解决粘冲问题，片剂成型率高，降低生产成本。
Description
技术领域
本发明涉及环保材料技术领域，尤其是涉及一种贝壳粉纳米抗菌足浴泡腾片及其制备方法。
背景技术
近年来，足浴作为一种简单易行的养生保健方式日益兴盛起来。通过足浴，可以刺激 足部穴位，健体强身，特别是在足浴过程中加入具有特殊功效的中草药品，在保健的同时达到健体除病的作用。而足浴泡腾片因其携带便捷，释药速度快的特点受到越来越多的关注。传统的以中药为功效成分的足浴泡腾片虽使用体验较好，但其在治疗脚癣方面效果却一直不佳，真菌很难杀灭，易传染，而且由于提取物原料较为粘稠，制备泡腾片时容易出现粘冲问题，片剂成型率低。
贝类是一种营养价值很高的珍贵海产品，分布于我国辽宁、山东、浙江、福建等省沿海。贝壳粉的主要成分是动物合成的碳酸钙，是一种表面多孔材料，也是天然的美容护肤佳品。资料显示，贝类含有人体所必须的八种氨基酸及丰富的牛磺酸(36mg/kg)、饱和脂肪酸及24种对美容有益的微量元素，如锌，硒，铁，铜，钾，镁等，这些成分跟珍珠的有效成分几乎相同，具有抗菌杀菌，清热消炎、活血生肌和按摩功效。而贻贝贝壳是一种天然的有机无机杂化材料，研究表明贻贝贝壳的结构分为3层，由外向内依次是角质层、棱柱层和珍珠层，其95%的主要成分是碳酸钙，还有少量氨基酸和多糖物质。贝壳粉是由海洋贝壳粉煅烧、研磨成粉末制成的，富含各种皮肤再生需要的氨基酸和微量元素，钙、磷、锰、锌、铜、铁、钾、镁等，有保持滋润，复活再生的效果，可以改变皮肤暗沉，能预测皮肤老化，适合各种肤质。烧制的贝壳粉膜对大肠杆菌有极强的抗菌和杀菌作用，另外对沙门氏菌、黄色葡萄糖菌也有显著效果。目前，尚未有以泡腾片形式存在的贝壳粉纳米抗菌足浴用品。
发明内容
本发明的目的之一在于提供一种安全无毒、抗菌谱广、抗菌效率高、稳定性好、不变色，有效治疗脚气、脚痒、起皮、干裂、灰指甲等足部常见不适症状，对足部皮肤有滋润保护作用，携带使用方便的贝壳粉纳米抗菌足浴泡腾片。
本发明的目的之一在于提供一种能解决粘冲问题，片剂成型率高，降低生产成本，有利于治理日益严重的环境污染问题的贝壳粉纳米抗菌足浴泡腾片的制备方法。
本发明针对上述技术中提到的问题，采取的技术方案为：
一种贝壳粉纳米抗菌足浴泡腾片，成分及其重量份为：纳米贝壳粉80-98份、中药抗菌活性组分2-20份、PEG6000 5-10份、酒石酸钠14-18份、碳酸氢钠20-30份、聚维酮0.02-0.04份、水0.8-1.2份。该足浴泡腾片中使用的原料都是天然来源，无毒无刺激，安全性高，各成分配伍合理，具有活性组分含量高、水中分散性能好、环境污染小、崩解速度快、贮存稳定、效果显著等优点，可杀灭真菌等足部常见细菌，有效治疗脚气、脚痒、起皮、干裂、灰指甲等足部常见不适症状，并对足部皮肤有滋润保护作用。
优选的，中药抗菌活性组分的成分及其重量份为：薄荷12-16份、藿香21-26份、紫苏8-13、艾草5-10份、花椒2-5份、姜1.3-1.6份、马兰2.2-2.8份、红花0.3-0.7份。该种中草药抗菌活性组分属天然植物源组合，对真菌有较好的抑制作用，具有抗菌谱广、抑菌效果好，对人畜无害，资源丰富、对环境友好等显著特点。
更为优选的，泡腾片的成分及其重量份为：纳米贝壳粉85-97份、中药抗菌活性组分3-15份、PEG6000 6-8份、酒石酸钠15-17份、碳酸氢钠23-25份、聚维酮0.02-0.04份、水0.8-1.2份。
一种贝壳粉纳米抗菌足浴泡腾片的制备方法，包括粗贝壳粉制备、纳米贝壳粉制备、中药抗菌活性组分制备、泡腾片制备，具体包括以下步骤：
粗贝壳粉制备：将贝壳清洗干净，用稀酸溶液浸泡4-5h，再用稀碱液中和洗涤，去除贝壳表面杂质，最后用清水洗净，烘干，研磨后过150-200目筛得粗贝壳粉，随着人们对于贝类软体部分的开发，造成大量的废弃贝壳资源，这些贝壳被大量堆积起来，未能得到有效的利用，贝壳上残余的软体组织发生腐败变质从而产生一系列有毒有害的物质，从而对环境造成不可避免的伤害，将贝壳粉加以利用，有利于治理日益严重的环境污染问题，酸处理使得贝壳粉体中碳酸钙的含量降低，增加有机物的含量，并大大增加贝壳粉中活性官能团的含量；
纳米贝壳粉制备：向粗贝壳粉中加入粗贝壳粉重量1.7-2.2%的粉碎分散剂，然后使用纳米粉碎机粉碎，即得纳米贝壳粉，粉碎分散剂为重量比为1:1.1-1.3:0.02-0.03的PEG2000、六偏磷酸钠和右旋糖酐的混合物，该粉碎分散剂各成分能够发挥协同作用，使贝壳粉的Zeta电位绝对值增大，颗粒之间不易团聚，很容易扩散到贝壳粉粒子表面上，形成了牢固的包膜层，有效地降低粒子的表面活性，从而使外加的粉碎能量更集中于粒子的粉碎上，达到较为满意的粉碎分散状态，提高物料粉碎效率及其水分散性，纳米贝壳粉的粒径为20-100nm，该细度的纳米贝壳粉在制备泡腾片时易于分散，和中药抗菌活性组分之间易于粘结，使得泡腾片的成型率高，且溶于水后更易于进入真菌内部，进而快速灭杀真菌，提高泡腾片的抗菌性和稳定性；
中药抗菌活性组分制备：按中药抗菌活性组分的配方取薄荷、藿香、紫苏、艾草、花椒、姜、马兰、红花，粉碎过150-250目筛，按料液比为1:7-11向药粉中加水煎煮2-3次，每次2-3小时，合并煎液，过滤，滤液浓缩成相对密度为1.25-1.32的药膏，粉碎过200-300目筛，即得中药抗菌活性组分，该中药抗菌活性组分具有较强的抗菌效果，同时又含有保湿、滋养肌肤的多种营养成分，与贝壳粉共同作用，可杀灭真菌等足部常见细菌，有效治疗脚气、脚痒、起皮、干裂、灰指甲等足部常见不适症状，并对足部皮肤有滋润保护作用；
泡腾片制备：按重量份取泡腾片各组分，将PEG6000熔融，加入碳酸氢钠，搅拌均匀，放置冷却，粉碎，再加入纳米贝壳粉、中药抗菌活性组分、酒石酸钠，混合均匀，然后用打粉制粒设备打均匀，再在温度为20-30℃、压力为50-100kN的条件下压片，即得足浴泡腾片，该步骤中酒石酸钠和碳酸氢钠的重量比为1:1.43-1.58，在该比例范围内，泡腾片具有崩解时间短、吸湿率的优势，且崩解后足浴水的pH值变化不明显，对足部皮肤无不良影响，该泡腾片的制备方法能解决粘冲问题，片剂成型率高，降低生产成本，所得泡腾片的水分散性明显较好，携带使用方便。
与现有技术相比，本发明的优点在于：本发明泡腾片使用的原料都是天然来源，各成分配伍合理，可杀灭真菌等足部常见细菌，有效治疗脚气、脚痒、起皮、干裂、灰指甲等足部常见不适症状，并对足部皮肤有滋润保护作用；该泡腾片具有崩解时间短、吸湿率的优势，且崩解后足浴水的pH值变化不明显，对足部皮肤无不良影响；该泡腾片用贝壳粉为纳米级，和中药抗菌活性组分之间易于粘结，使得泡腾片的成型率高，且溶于水后更易于进入真菌内部，进而快速灭杀真菌，提高泡腾片的抗菌性和稳定性；该泡腾片的制备方法能解决粘冲问题，片剂成型率高，降低生产成本，所得泡腾片的水分散性明显较好，携带使用方便。
具体实施方式
下面通过实施例对本发明方案作进一步说明：
实施例1：
一种贝壳粉纳米抗菌足浴泡腾片，成分及其重量份为：纳米贝壳粉80-98份、中药抗菌活性组分2-20份、PEG6000 5-10份、酒石酸钠14-18份、碳酸氢钠20-30份、聚维酮0.02-0.04份、水0.8-1.2份。上述中药抗菌活性组分的成分及其重量份为：薄荷12-16份、藿香21-26份、紫苏8-13、艾草5-10份、花椒2-5份、姜1.3-1.6份、马兰2.2-2.8份、红花0.3-0.7份。
一种贝壳粉纳米抗菌足浴泡腾片的制备方法，具体包括以下步骤：
1）粗贝壳粉制备：将贝壳清洗干净，用稀酸溶液浸泡4-5h，再用稀碱液中和洗涤，去除贝壳表面杂质，最后用清水洗净，烘干，研磨后过150-200目筛得粗贝壳粉；
2）纳米贝壳粉制备：向粗贝壳粉中加入粗贝壳粉重量1.7-2.2%的粉碎分散剂，然后使用纳米粉碎机粉碎，即得粒径为20-100nm的纳米贝壳粉，粉碎分散剂为重量比为1:1.1-1.3:0.02-0.03的PEG2000、六偏磷酸钠和右旋糖酐的混合物；
3）中药抗菌活性组分制备：按中药抗菌活性组分的配方取薄荷、藿香、紫苏、艾草、花椒、姜、马兰、红花，粉碎过150-250目筛，按料液比为1:7-11向药粉中加水煎煮2-3次，每次2-3小时，合并煎液，过滤，滤液浓缩成相对密度为1.25-1.32的药膏，粉碎过200-300目筛，即得中药抗菌活性组分；
4）泡腾片制备：按重量份取泡腾片各组分，将PEG6000熔融，加入碳酸氢钠，搅拌均匀，放置冷却，粉碎，再加入纳米贝壳粉、中药抗菌活性组分、酒石酸钠，混合均匀，然后用打粉制粒设备打均匀，再在温度为20-30℃、压力为50-100kN的条件下压片，即得足浴泡腾片，该步骤中酒石酸钠和碳酸氢钠的重量比为1:1.43-1.58。
实施例2：
一种贝壳粉纳米抗菌足浴泡腾片，成分及其重量份为：纳米贝壳粉86份、中药抗菌活性组分12份、PEG6000 6份、酒石酸钠17份、碳酸氢钠23份、聚维酮0.04份、水0.8份。上述中药抗菌活性组分的成分及其重量份为：薄荷16份、藿香21份、紫苏8、艾草10份、花椒2份、姜1.6份、马兰2.2份、红花0.7份。
一种贝壳粉纳米抗菌足浴泡腾片的制备方法，具体包括以下步骤：
1）粗贝壳粉制备：将贝壳清洗干净，用稀酸溶液浸泡5h，再用稀碱液中和洗涤，去除贝壳表面杂质，最后用清水洗净，烘干，研磨后过150目筛得粗贝壳粉；
2）纳米贝壳粉制备：向粗贝壳粉中加入粗贝壳粉重量2.2%的粉碎分散剂，然后使用纳米粉碎机粉碎，即得粒径为20-100nm的纳米贝壳粉，粉碎分散剂为重量比为1:1.1:0.03的PEG2000、六偏磷酸钠和右旋糖酐的混合物；
3）中药抗菌活性组分制备：按中药抗菌活性组分的配方取薄荷、藿香、紫苏、艾草、花椒、姜、马兰、红花，粉碎过250目筛，按料液比为1:7向药粉中加水煎煮3次，每次2小时，合并煎液，过滤，滤液浓缩成相对密度为1.25的药膏，粉碎过300目筛，即得中药抗菌活性组分；
4）泡腾片制备：按重量份取泡腾片各组分，将PEG6000熔融，加入碳酸氢钠，搅拌均匀，放置冷却，粉碎，再加入纳米贝壳粉、中药抗菌活性组分、酒石酸钠，混合均匀，然后用打粉制粒设备打均匀，再在温度为30℃、压力为50kN的条件下压片，即得足浴泡腾片，该步骤中酒石酸钠和碳酸氢钠的重量比为1:1.58。
实施例3：
一种贝壳粉纳米抗菌足浴泡腾片，成分及其重量份为：纳米贝壳粉90份、中药抗菌活性组分10份、PEG6000 7份、酒石酸钠16份、碳酸氢钠25份、聚维酮0.03份、水1.0份。
上述中药抗菌活性组分的成分及其重量份为：薄荷14份、藿香23份、紫苏10、艾草7份、花椒4份、姜1.5份、马兰2.4份、红花0.5份。
一种贝壳粉纳米抗菌足浴泡腾片的制备方法，具体包括以下步骤：
1）粗贝壳粉制备：将贝壳清洗干净，用稀酸溶液浸泡4.5h，再用稀碱液中和洗涤，去除贝壳表面杂质，最后用清水洗净，烘干，研磨后过180目筛得粗贝壳粉；
2）纳米贝壳粉制备：向粗贝壳粉中加入粗贝壳粉重量2.0%的粉碎分散剂，然后使用纳米粉碎机粉碎，即得粒径为20-100nm的纳米贝壳粉，粉碎分散剂为重量比为1:1.2:0.025的PEG2000、六偏磷酸钠和右旋糖酐的混合物；
3）中药抗菌活性组分制备：按中药抗菌活性组分的配方取薄荷、藿香、紫苏、艾草、花椒、姜、马兰、红花，粉碎过200目筛，按料液比为1:9向药粉中加水煎煮2次，每次2.5小时，合并煎液，过滤，滤液浓缩成相对密度为1.3的药膏，粉碎过250目筛，即得中药抗菌活性组分；
4）泡腾片制备：按重量份取泡腾片各组分，将PEG6000熔融，加入碳酸氢钠，搅拌均匀，放置冷却，粉碎，再加入纳米贝壳粉、中药抗菌活性组分、酒石酸钠，混合均匀，然后用打粉制粒设备打均匀，再在温度为25℃、压力为80kN的条件下压片，即得足浴泡腾片，该步骤中酒石酸钠和碳酸氢钠的重量比为1:1.5。
实施例4：
一种贝壳粉纳米抗菌足浴泡腾片，成分及其重量份为：纳米贝壳粉90份、中药抗菌活性组分10份、PEG6000 7份、酒石酸钠16份、碳酸氢钠25份、聚维酮0.03份、水1.0份。
上述中药抗菌活性组分的成分及其重量份为：薄荷14份、藿香23份、紫苏10、艾草7份、花椒4份、姜1.5份、马兰2.4份、红花0.5份。
一种贝壳粉纳米抗菌足浴泡腾片的制备方法，具体包括以下步骤：
1）粗贝壳粉制备：将贝壳清洗干净，用稀酸溶液浸泡4.5h，再用稀碱液中和洗涤，去除贝壳表面杂质，最后用清水洗净，烘干，研磨后过180目筛得粗贝壳粉；
2）纳米贝壳粉制备：按重量比为100:0.38-0.52向粗贝壳粉中加入酒石酸二乙酯，搅拌1-2h，再按固液比为1:8-12加入0.1mol/L AgNO3溶液，搅拌3-5h，过滤干燥，然后向干燥粉末中加入粗贝壳粉重量2.0%的粉碎分散剂，然后使用纳米粉碎机粉碎，即得粒径为20-100nm的纳米贝壳粉，粉碎分散剂为重量比为1:1.2:0.025的PEG2000、六偏磷酸钠和右旋糖酐的混合物，上述酒石酸二乙酯中L-酒石酸二乙酯和D-酒石酸二乙酯的重量比为100:1.32-1.36，酒石酸二乙酯的加入可以与粗贝壳粉中的活性基团发生聚合反应，为贝壳粉上结合Ag离子提供更多的活性基团，同时可得到新的手性物质，大大提高贝壳粉识别真菌等细菌的能力，进而快速灭杀细菌，同时提高足浴泡腾片的清热消炎和防臭效果，而D-酒石酸二乙酯的加入提高反应的立体选择性，增加手性反应物的得率，该纳米贝壳粉的活性官能团中结合有纳米银，能够提高纳米贝壳粉的抗菌性和抗菌稳定性；
3）中药抗菌活性组分制备：按中药抗菌活性组分的配方取薄荷、藿香、紫苏、艾草、花椒、姜、马兰、红花，粉碎过200目筛，按料液比为1:9向药粉中加水，煎煮2次，每次2.5小时，合并煎液，过滤，滤液浓缩成相对密度为1.3的药膏，粉碎过250目筛，即得中药抗菌活性组分；
4）泡腾片制备：按重量份取泡腾片各组分，将PEG6000熔融，加入碳酸氢钠，搅拌均匀，放置冷却，粉碎，再加入纳米贝壳粉、中药抗菌活性组分、酒石酸钠，混合均匀，然后用打粉制粒设备打均匀，再在温度为25℃、压力为80kN的条件下压片，即得足浴泡腾片，该步骤中酒石酸钠和碳酸氢钠的重量比为1:1.5。
实施例5：
抗菌性能测试：
抗菌性能测试是采用琼脂稀释法对大肠杆菌和金黄色葡萄球菌的进行测定。将实施例3和市售足浴泡腾片在紫外线福射30min，确保灭菌，然后将他们添加到琼脂悬浮液中，保温50℃，转移到培养皿，慢慢冷却，直到形成凝胶。将大肠杆菌和金黄色葡萄球菌的初始浓度被稀释到104CFU，取出体积浓度约为100μL的细菌悬浮液，用弯曲玻璃棒将其转换到琼脂培养皿中，并将琼脂培养皿置于37℃下进行培养24小时，进行计数，计算抑菌率。实施例3对大肠杆菌和金黄色葡萄球菌的抗菌率均为99.99%，市售足浴泡腾片对大肠杆菌和金黄色葡萄球菌的抗菌率分别为90.32%和85.67%，说明本发明实施例3产品抗菌效果好。
本发明的操作步骤中的常规操作为本领域技术人员所熟知，在此不进行赘述。
以上所述的实施例对本发明的技术方案进行了详细说明，应理解的是以上所述仅为本发明的具体实施例，并不用于限制本发明，凡在本发明的原则范围内所做的任何修改、补充或类似方式替代等，均应包含在本发明的保护范围之内。
Claims (7)
1. 一种贝壳粉纳米抗菌足浴泡腾片，其特征在于：所述泡腾片的成分及其重量份为：纳米贝壳粉80-98份、中药抗菌活性组分2-20份、PEG6000 5-10份、酒石酸钠14-18份、碳酸氢钠20-30份、聚维酮0.02-0.04份、水0.8-1.2份；
所述中药抗菌活性组分的成分及其重量份为：薄荷12-16份、藿香21-26份、紫苏8-13、艾草5-10份、花椒2-5份、姜1.3-1.6份、马兰2.2-2.8份、红花0.3-0.7份。
2. 根据权利要求1所述的一种贝壳粉纳米抗菌足浴泡腾片，其特征在于：所述泡腾片的成分及其重量份为：纳米贝壳粉85-97份、中药抗菌活性组分3-15份、PEG6000 6-8份、酒石酸钠15-17份、碳酸氢钠23-25份、聚维酮0.02-0.04份、水0.8-1.2份。
3.一种权利要求1所述的贝壳粉纳米抗菌足浴泡腾片的制备方法，包括粗贝壳粉制备、纳米贝壳粉制备、中药抗菌活性组分制备、泡腾片制备，其特征在于：所述纳米贝壳粉制备步骤为：向粗贝壳粉中加入粉碎分散剂，然后使用纳米粉碎机粉碎，即得纳米贝壳粉；
所述纳米贝壳粉制备步骤中粉碎分散剂的添加量为粗贝壳粉重量1.7-2.2%，所述粉碎分散剂为重量比为1:1.1-1.3:0.02-0.03的PEG2000、六偏磷酸钠和右旋糖酐的混合物；
所述纳米贝壳粉的粒径为20-100nm。
4.根据权利要求3所述的一种贝壳粉纳米抗菌足浴泡腾片的制备方法，其特征在于：所述粗贝壳粉制备步骤为：将贝壳清洗干净，用稀酸溶液浸泡4-5h，再用稀碱液中和洗涤，最后用清水洗净，烘干，研磨后过150-200目筛得粗贝壳粉。
5.根据权利要求3所述的一种贝壳粉纳米抗菌足浴泡腾片的制备方法，其特征在于：所述中药抗菌活性组分制备步骤为：取薄荷、藿香、紫苏、艾草、花椒、姜、马兰、红花，粉碎过150-250目筛，按料液比为1:7-11向药粉中加水煎煮2-3次，每次2-3小时，合并煎液，过滤，滤液浓缩成相对密度为1.25-1.32的药膏，粉碎过200-300目筛，即得中药抗菌活性组分。
6.根据权利要求3所述的一种贝壳粉纳米抗菌足浴泡腾片的制备方法，其特征在于：所述泡腾片制备步骤为：按重量份取泡腾片各组分，将PEG6000熔融，加入碳酸氢钠，搅拌均匀，放置冷却，粉碎，再加入纳米贝壳粉、中药抗菌活性组分、酒石酸钠、聚维酮和水，混合均匀，然后用打粉制粒设备打均匀，再在温度为20-30℃、压力为50-100kN的条件下压片，即得足浴泡腾片。
7.根据权利要求3所述的一种贝壳粉纳米抗菌足浴泡腾片的制备方法，其特征在于：所述泡腾片制备步骤中酒石酸钠和碳酸氢钠的重量比为1:1.43-1.58。
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