CN114907620A - 一种具有药物缓释能力再生纤维素膜的制备方法 - Google Patents
一种具有药物缓释能力再生纤维素膜的制备方法 Download PDFInfo
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Abstract
本发明公开了一种具有药物缓释能力再生纤维素膜的制备方法,该方法是将风干的大龙竹进行脱木素和脱半纤维素处理得到干燥的纤维素,将干燥纤维素加入N,N‑二甲基乙酰胺中,在110~120℃、搅拌的条件下溶胀2~3h,加入LiCl,在100~110℃、搅拌的条件下溶解纤维素2~3h,随后在100~105℃下加入β‑环糊精继续反应0.5~2h;将反应产物转移至模具中,保鲜膜封口,在4℃下冷藏过夜,得到再生纤维素膜;将再生纤维素膜放入质量浓度4~5%的甘油水溶液中再生10~20min,随后用去离子水清洗,得到具有药物缓释能力的再生纤维素水凝胶;本发明制得的再生纤维素膜具有良好的药物包和能力,且具有良好的生物降解性。
Description
技术领域
本发明涉及一种具有药物缓释能力再生纤维素膜的制备方法,以植物纤维素和β-环糊精为原料,经N,N-二甲基乙酰胺-氯化锂溶解体系和甘油水溶液再生体系制备具有药物缓释能力再生纤维素膜的方法,属于天然高分子基纳米材料领域。
背景技术
水凝胶材料有独特的力学柔性、生物相容性及许多与有机生物体类似的独特性质,在诸多的领域发挥着不可或缺的作用。但传统水凝胶大多以石化为原料、制备方法较为繁琐、功能性单一、难以重复利用并且不可天然降解,使得水凝胶材料的发展和应用受到了一定程度上的制约。因此,开发制备工艺简单、环境友好的多功能水凝胶材料成为高分子材料前沿领域的研究热点之一。
在人类赖以生存的生态圈中,有99%以上的碳源自于植物,其中约40%的是以纤维素的形式存在。纤维素作为自然界中分布最广、含量最多的一种多糖,具有廉价、可再生、生物相容性好、可完全生物降解等优势。对纤维素的利用成为化学、化工和材料科学领域的研究热点。
纤维素的分子式为(C6H10O5)n,属于典型的环状半缩醛结构,一级结构为吡喃式葡萄糖,通过β-1,4糖苷键连接而成。纤维素结构中含有一个伯羟基和两个仲羟基,正是由于分子内存在大量活性羟基,纤维素分子链内部及分子链之间会形成大量的分子间和分子内氢键,对纤维素的物化性能产生较大影响。由于纤维素分子链间氢键的存在,以及更高级结构结晶区的存在,导致纤维素不溶于水或一般的有机溶剂。选用合适的溶解体系,将纤维素进行溶解再生处理之后可以改变纤维素原有形貌,将纤维素制备成水凝胶,提高纤维素的利用率。
环糊精作为一类环状低聚寡糖,是直链淀粉经葡萄糖转移酶降解所得到的产物。常见的环糊精种类有三种,根据其自身组成结构α-1,4-糖苷键连接的D-吡喃葡萄糖单元的数目进行区分。β-环糊精含有 7个吡喃葡萄糖单元。环糊精在空间上呈现出中空截锥的圆筒状,内部由于C-H基团的屏蔽作用形成非极性疏水空腔,而外部的极性伯羟基对水分子具有吸引作用,使其具备了独特的“外亲水,内疏水”的结构特性。该结构特性使得环糊精具有了分子识别功能,可包埋不稳定易挥发的客体小分子,提高这些小分子的稳定性或者水溶性,使其在食品、香料、医药、化妆品等领域有了极为广泛的应用。由于环糊精的内部空腔具有疏水性,外部结构具有亲水性,因此,利用环糊精的疏水空腔可以负载一些疏水性的药物小分子,提高疏水药物分子的亲水性,并对疏水药物分子产生一定的缓释作用,延长药物分子的治疗作用。
结合纤维素与β-环糊精的特性,本申请以纤维素和β-环糊精为原料制备具有药物缓释能力的水凝胶,为纤维素的综合利用提供了一条全新的途径,为β-环糊精包和药物寻找了新的载体,积极地推动了纤维素在生物医学领域的新发展。
发明内容
当前负载药物纤维素膜的制备技术手段还有较大的发展空间,对药物的封装效率和载药效率尚待提高,因此纤维素水凝胶的应用还受到了一定的限制;本发明提供了一种能够缓释药物的纤维素膜的制备方法,该方法将干燥纤维素溶解在N,N-二甲基乙酰胺(DMAc)/氯化锂(LiCl)体系中,加入不同质量的β-环糊精,得到物理交联体系,将共混溶液注入甘油水溶液再生体系中,再生得到具有缓释作用的纤维素水凝胶。
本发明中纤维素包括植物组织细胞提取得到的纤维素、细菌纤维素,采用常规方法制得,例如将竹子薄壁细胞(参照Antimicrobial cellulose hydrogels preparationwith RIF loading from bamboo parenchyma cells: A green approach towards woundhealing文献中方法制得)悬浮在去离子水中,依次加入亚氯酸钠和冰醋酸,在55~85℃下进行脱木质素处理获得综纤维素,用去离子水洗涤至滤液的pH为中性,将综纤维素加入去离子水中,再加入综纤维素质量8~12%的氢氧化钾,在20~30℃水浴中进行脱半纤维素处理,得到竹子薄壁细胞纤维素,用去离子水洗涤至滤液的pH为中性,干燥即得;亚氯酸钠的添加量为竹子薄壁细胞质量的60~65%,冰醋酸的添加量与竹子薄壁细胞体积质量比为40~45%。
实现本发明目的采用如下技术方案:
(1)将干燥纤维素加入到N,N-二甲基乙酰胺溶液中混合均匀,在110~120℃、搅拌下溶胀2~3h后,待溶胀完毕后,加入LiCl,在100~110℃、搅拌下进行纤维素溶解,时间为2~3h;
所述搅拌速度为300~800r/min,绝干纤维素与N,N-二甲基乙酰胺的质量体积比g:mL为5~10%,氯化锂与N,N-二甲基乙酰胺的质量体积比g:mL为5~10%;
(2)将β-环糊精加入步骤(1)溶解液中,在110~120℃、搅拌下继续反应0.5~2h,β-环糊精与纤维素的质量比10~30%;将反应产物转移至模具中,保鲜膜封口,在4℃下冷藏过夜,得到再生纤维素膜;将再生纤维素膜放入质量浓度4~5%的甘油水溶液中再生10~20min,随后用去离子水清洗,得到具有药物缓释能力的再生纤维素水凝胶;
所述搅拌速度为300~800r/min。
本发明的有益效果是:
以易得的纤维素和β-环糊精为原料,通过N,N-二甲基乙酰胺-氯化锂溶解体系溶解纤维素,获得具有药物缓释能力的再生纤维素膜;天然高分子基纤维素膜具有合成高分子膜的共性,且该纤维素膜具有良好药物包和的能力、环境友好性以及价格低廉等优势。此具有药物缓释能力的纤维素膜为纤维素的利用提供了可行性方案,同时为β-环糊精的利用提供新的思路。
具体实施方式
下面结合实施例对发明作进一步详细说明,但本发明保护范围不局限于所述内容。
实施例1:具有药物缓释能力再生纤维素膜的制备方法如下:
1、将18g竹子薄壁细胞悬浮在600mL去离子水中,依次加入11.25g亚氯酸钠和7.5mL冰醋酸,85℃下进行脱木质素处理,得到的综纤维素用去离子水洗涤至滤液的pH为中性,将10g综纤维素加入200mL去离子水中,再加入1g的氢氧化钾,25℃下进行脱半纤维素处理,得到竹子薄壁细胞纤维素,继续用去离子水洗涤至滤液的pH为中性,放入冻干机进行干燥处理,即得绝干的纤维素;
2、纤维素溶胀反应条件为:绝干纤维素与N,N-二甲基乙酰胺的质量体积比为5%,反应时间2h,处理温度110℃,转速300r/min;纤维素溶解反应条件为:氯化锂与N,N-二甲基乙酰胺的质量体积比为5%,处理温度100℃,反应时间3h,转速400r/min;β-环糊精与纤维素质量比为10%,100℃反应时间0.5h,转速400r/min;
具体的纤维素溶解处理步骤为:将1.5g绝干纤维素与30.0mL N,N-二甲基乙酰胺(DMAc)混合,在110℃、300r/min搅拌下进行纤维素溶胀反应2h;待溶胀完毕后加入1.5gLiCl,在100 ℃、400r/min搅拌条件下进行纤维素溶解反应3h,加入0.15 g β-环糊精,在100℃、400r/min搅拌下混合0.5h;反应产物转移至PTEF模具中,用保鲜膜封口,4℃冷藏过夜,得到再生纤维素膜;将再生纤维素膜连同PTEF模具放入4%甘油水溶液中再生10min,随后用去离子水洗净膜,得到再生纤维素水凝胶膜;
3、将11g再生纤维素膜分别剪成15×15mm的片状,在25℃下浸泡在50mL 1.0mg/mL扑热息敏溶液中1h后,将负载药物的纤维素膜装入透析袋中,24h后测定在透析袋中透析出扑热息敏的浓度,扑热息敏的释放率达到68%。
实施例2:具有药物缓释能力再生纤维素膜的制备方法如下:
1、将18g竹子薄壁细胞悬浮在600mL去离子水中,依次加入11.5g亚氯酸钠和7.7mL冰醋酸,80℃下进行脱木质素处理,得到的综纤维素用去离子水洗涤至滤液的pH为中性,将10g综纤维素加入200mL去离子水中,再加入0.9g的氢氧化钾,20℃下进行脱半纤维素处理,得到竹子薄壁细胞纤维素,继续用去离子水洗涤至滤液的pH为中性,放入冻干机进行干燥处理,即得绝干的纤维素;
2、将2.1g绝干纤维素与30.0mL N,N-二甲基乙酰胺(DMAc)混合,在115℃、400r/min搅拌下溶胀纤维素3h,待溶胀完毕后,加入2.7g LiCl,在105℃、600r/min下溶解纤维素2h,然后加入0.42g β-环糊精,在105 ℃、600r/min下混合1h;反应产物转移至PTEF模具中,用保鲜膜封口,4℃冷藏过夜,得到再生纤维素膜;将再生纤维素膜连同PTEF板放入4.5%甘油水溶液中进行再生15min,随后用去离子水洗净膜,得到具有药物包和能力的再生纤维素水凝胶膜;
3、将11g再生纤维素膜分别剪成15×15mm的片状,在25℃下浸泡在50mL1.0mg/mL扑热息敏溶液中1h,随后将负载药物的纤维素膜装入透析袋中,24h后测定在透析袋中透析出扑热息敏的浓度,扑热息敏的浓度达到63%。
实施例3:具有药物缓释能力再生纤维素膜的制备方法如下:
1、绝干的纤维素制备同实施例1;
2、将2.7g绝干纤维素与30.0mL N,N-二甲基乙酰胺(DMAc)混合,在120℃、700r/min下溶胀纤维素2h;待溶胀完毕后,加入3g LiCl,在110℃、600r/min下溶解纤维素3h,加入0.81g β-环糊精,在110℃、600r/min下混合2h;反应产物转移至PTEF模具中,用保鲜膜封口,4℃冷藏过夜,得到再生纤维素膜;将再生纤维素膜连同PTEF模具放入5%甘油水溶液中进行再生20 min,随后用去离子水洗净膜,得到具有药物包和能力的再生纤维素水凝胶膜;
3、将11g再生纤维素膜分别剪成15×15mm的片状,在25℃下浸泡在50 mL 1.0 mg/m扑热息敏溶液中1h,随后将负载药物的纤维素膜装入透析袋中,24h后测定在透析袋中透析出扑热息敏的浓度,扑热息敏的浓度达到60%。
Claims (6)
1.一种具有药物缓释能力再生纤维素膜的制备方法,其特征在于:将干燥纤维素加入N,N-二甲基乙酰胺中,在110~120℃、搅拌下溶胀2~3h后,加入LiCl,在100~110℃、搅拌下溶解纤维素2~3h,随后在100~105℃下加入β-环糊精继续反应0.5~2h;将反应产物转移至模具中,保鲜膜封口,在4℃下冷藏过夜,得到再生纤维素膜;将再生纤维素膜放入质量浓度4~5%的甘油水溶液中再生10~20min,随后用去离子水清洗,得到具有药物缓释能力的再生纤维素水凝胶。
2.根据权利要求1所述的具有药物缓释能力再生纤维素膜的制备方法,其特征在于:搅拌转速为300~800r/min。
3.根据权利要求1所述的具有药物缓释能力再生纤维素膜的制备方法,其特征在于:绝干纤维素与N,N-二甲基乙酰胺的质量体积比g:mL为5~10%,氯化锂与N,N-二甲基乙酰胺的质量体积比g:mL为5~10%,β-环糊精与纤维素的质量比10~30%。
4.根据权利要求1所述的具有药物缓释能力再生纤维素膜的制备方法,其特征在于:纤维素为植物组织细胞提取得到的纤维素或细菌纤维素。
5.根据权利要求1所述的具有药物缓释能力再生纤维素膜的制备方法,其特征在于:纤维素是将竹子薄壁细胞悬浮在去离子水中,依次加入亚氯酸钠和冰醋酸,在55~85℃下进行脱木质素处理获得综纤维素,用去离子水洗涤至滤液的pH为中性,将综纤维素加入去离子水中,再加入综纤维素质量8~12%的氢氧化钾,在20~30℃水浴中进行脱半纤维素处理,得到竹子薄壁细胞纤维素,用去离子水洗涤至滤液的pH为中性,干燥即得。
6.根据权利要求1所述的具有药物缓释能力再生纤维素膜的制备方法,其特征在于:亚氯酸钠的添加量为竹子薄壁细胞质量的60~65%,冰醋酸的添加量与竹子薄壁细胞体积质量比为40~45%。
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