CN110841103B - 一种桑叶粉-桑蚕丝胶/柞蚕丝素共混膜及其制备方法 - Google Patents
一种桑叶粉-桑蚕丝胶/柞蚕丝素共混膜及其制备方法 Download PDFInfo
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Abstract
本发明属于生物材料技术领域,公开一种桑叶粉‑桑蚕丝胶/柞蚕丝素共混膜(MLP‑MSS/TSF‑BF)及其制备方法和应用。该共混膜的制备方法是首先制备桑蚕丝胶溶液和柞蚕丝素溶液,将桑蚕丝胶溶液和柞蚕丝素溶液混合均匀,再加入明胶溶液和聚乙二醇200溶液混合均匀,最后添加桑叶粉得到桑叶粉‑桑蚕丝胶/柞蚕丝素混合液,干燥即得桑叶粉‑桑蚕丝胶/柞蚕丝素共混膜。本发明制备的共混膜具有优良的拉伸性能和抑菌活性,在医疗和化妆品领域方面具有重要的应用潜力。
Description
技术领域
本发明属于材料技术领域。更具体地,涉及一种桑叶粉-桑蚕丝胶/柞蚕丝素共混膜及其制备方法。
背景技术
皮肤是人体最大的器官,具有体温调节、感觉吸收、保护体内组织器官免受各类物理、化学伤害和病菌、微生物的侵袭等功能。皮肤受到伤害(如烧伤、机械创伤)后,需要包覆,以降低感染。促进伤口愈合,降低伤口感染率,防止疤痕的产生,是医学研究中重点关注的方向。研究发现敷料材料的性质对创面愈合至关重要。好的敷料能迅速封闭创面,促进各类细胞再生和组织生长,尽快恢复皮肤屏障功能,显著降低因感染引起的相关并发症。迄今已开发超过3000种敷料,但在临床得到广泛应用的敷料仅占其中的少部分。
蚕丝是一种蛋白质纤维,该纤维具有良好的生物相容性,机械性能和可被生物降解等特性,具备制作膜材料的潜力。如专利CN201010119912.2中给出了一种柞蚕丝素肽-明胶共混膜,既可作为包装材料应用又可作为营养物质食用,但其并不适宜用作医用敷料,由于柞蚕丝素肽是用酸、碱或酶水解后所获得的,肽键被打断了,其分子量较小,导致成膜性差,拉伸性能不足,且无抑菌性。
因此,研发一种抑菌效果好、力学性能优良的创面敷料在医疗和化妆品领域方面具有重要的应用价值。
发明内容
本发明旨在提供一种桑叶粉-桑蚕丝胶/柞蚕丝素共混膜及其制备方法,该方法工艺简单易控、条件温和,制备出的共混膜力学性能优良,抑菌效果好,在医疗及化妆品领域具有潜在的应用价值。
本发明的目的是提供一种桑叶粉-桑蚕丝胶/柞蚕丝素共混膜的制备方法。
本发明另一目的是提供制备得到的桑叶粉-桑蚕丝胶/柞蚕丝素共混膜。
本发明再一目的是提供所述共混膜在医疗及化妆品领域方面的应用。
本发明上述目的通过以下技术方案实现:
本发明提供了一种桑叶粉-桑蚕丝胶/柞蚕丝素共混膜的制备方法,是先将桑蚕丝胶溶液与柞蚕丝素溶液混合均匀;再加入明胶溶液和聚乙二醇溶液混合均匀;最后加桑叶粉混合均匀,干燥即得桑叶粉-桑蚕丝胶/柞蚕丝素共混膜。
该方法使用桑蚕丝胶和柞蚕丝素共混,并引入桑叶粉制备桑叶粉-桑蚕丝胶/柞蚕丝素共混膜。其中,柞蚕丝素(Tussah silk fibroin)蛋白富含有利于细胞黏附和生长的天然的精氨酸-甘氨酸-天门冬氨酸(RGD)三肽序列,具有优良的细胞粘附性能,因而十分适用于医药生物材料。桑蚕丝胶(mulberry silk sericin)因含亲水基团的氨基酸较多,具有很强的吸水能力,可防止水分流失,而且具有促进胶原的增殖和迁移的能力,安全性高,同时还具有交联剂的作用。桑叶粉的主要成分为纤维素,纤维素纤维具有良好的生物兼容性、可降解性、亲水性,以及广泛的化学可塑性,因此适于创面敷料,特别是作为基础性的支撑或固定结合其他材料混合使用;我们实验研究显示,桑叶粉的加入可以明显改善桑蚕丝胶/柞蚕丝素共混膜的拉伸性能;此外桑叶粉还富含有抗菌活性物质;因此在敷料中既起到支撑作用,还可降低细菌的感染。
具体地,所述桑叶粉-桑蚕丝胶/柞蚕丝素共混膜的制备方法,包括如下步骤:
S1.制备10~50mg/mL的柞蚕丝素溶液和1~50μg/mL的桑蚕丝胶溶液;
S2.将步骤S1制得的柞蚕丝素溶液与桑蚕丝胶溶液混合均匀得到桑蚕丝胶/柞蚕丝素混合液1;
S3.向步骤S2制得的混合液1中加入100~500mg/mL的明胶溶液和聚乙二醇200,混合均匀,得到桑蚕丝胶/柞蚕丝素混合液2;
S4.向步骤S3得到的混合液2中加入桑叶粉混合均匀,得到桑叶粉-桑蚕丝胶/柞蚕丝素混合液;
S5.将步骤S4制得的桑叶粉-桑蚕丝胶/柞蚕丝素混合液干燥即得桑叶粉-桑蚕丝胶/柞蚕丝素共混膜。
实验过程中发现,当桑叶粉的粒径超过500nm时无法有效结合到共混膜中,同时还会破坏膜的结构,降低共混膜的拉伸性能,因此优选地,所述桑叶粉的粒径低于500nm。
优选地,步骤S1所述柞蚕丝素溶液的浓度为27.5mg/mL,桑蚕丝胶溶液的浓度为4.50μg/mL。
优选地,步骤S3所述明胶溶液的浓度为375mg/mL。
优选地,柞蚕丝素溶液、桑蚕丝胶溶液、明胶溶液和聚乙二醇200的体积比为0.5~1.5:1~3:1~2:2~4。
更优选地,柞蚕丝素溶液、桑蚕丝胶溶液、明胶溶液和聚乙二醇200的体积比1:2:1.5:3。
优选地,步骤S4所述桑叶粉的添加量占桑叶粉-桑蚕丝胶/柞蚕丝素混合液的质量分数为0.5~2.5%。
最优选地,步骤S4所述桑叶粉的添加量占桑叶粉-桑蚕丝胶/柞蚕丝素混合液的质量分数为1%。
优选地,步骤S2、S3、S4中混合均匀为在60~80℃下搅拌1~2min混合均匀。
最优选地,步骤S2、S3、S4中混合均匀为在70℃水浴中搅拌2min混合均匀。
优选地,所述干燥为在20~60℃下干燥24~96h。
更优选地,所述干燥为在30℃干燥48h。
另外,上述方法中,优选地:
桑蚕丝胶溶液的制备方法如下:
称取桑蚕茧壳加入蒸馏水,于100℃进行回流处理30min后,过滤收集丝胶溶液,将得到的丝胶溶液在4℃冰箱保存以备使用。
柞蚕丝素溶液的制备方法如下:
称取180g的四水合硝酸钙晶体,在80℃条件下加热并搅拌30min后,得到熔融的硝酸钙。用量筒量取100mL熔融的硝酸钙,倒入圆底烧瓶中,称取柞蚕丝素纤维加入其中,然后放置于油浴锅中在120℃条件下加热搅拌溶解2h后,冷却,装入截留分子量为8~10KDa透析袋,置于流动自来水中透析两天,再于去离子水中透析一天,每2~4h换一次水,透析3天后将得到柞蚕丝素溶液,置于4℃冰箱储藏备用。
桑叶粉的制备方法如下:
取沙2×109桑叶,在200℃温度杀青至桑叶边缘翻卷,100℃左右干燥,然后用粉碎机粉碎至桑叶粒径低于500nm。
所述桑叶粉-桑蚕丝胶/柞蚕丝素共混膜在制备生物材料方面的应用,可应用于医疗及化妆品领域:本发明制备所得的共混膜可应用于医疗及化妆品领域方面,具有优良的力学拉伸性能和抑菌效果。
本发明具有以下有益效果:
1、以桑叶粉、桑蚕丝胶、柞蚕丝素为主要原料制备生物创面敷料,该方法工艺简单易控、条件温和,易于控制。
2、以桑叶粉、桑蚕丝胶、柞蚕丝素为原料制备的共混膜,因柞蚕丝素(Tussah silkfibroin)蛋白氨基酸序列中含有精氨酸-甘氨酸-天门冬氨酸(RGD)三肽序列,该序列有利于细胞的黏附和生长,同时桑叶粉具有一定的抑菌效果,有利于皮肤创面愈合,将其应用于医疗及化妆品领域将具有显著的经济效益。
3、相比于其他化学合成材料用于改善膜性能的方法,加入桑叶粉既环保又安全,得到的共混膜天然可降解、亲水性强、力学性能优良。
附图说明
图1为添加1%桑叶粉的MLP-MSS/TSF-BF;
图2为桑叶粉浓度对MLP-MSS/TSF-BF溶失率的影响;
图3为桑叶粉浓度对MLP-MSS/TSF-BF拉伸性能的影响;
图4为添加1%桑叶粉的MLP-MSS/TSF-BF对大肠杆菌(A)的抑菌效果和对金黄色葡萄糖菌(B)的抑菌效果图。
具体实施方式
以下结合说明书附图和具体实施例来进一步说明本发明,但实施例并不对本发明做任何形式的限定。除非特别说明,本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
除非特别说明,以下实施例所用试剂和材料均为市购。
1、溶失率的测定
溶失率是衡量成膜性好坏的一个重要指标,溶失率越低的膜,强力越好。
采用热水溶失率法测定:称取两份质量相同的桑叶粉-桑蚕丝胶/柞蚕丝素共混膜,其中一份在100℃烘箱中烘至衡量,称取质量为m1;另一份按共混膜和水以1g:30mL的浴比在温度为37℃条件下振荡15min,滤出剩余膜,放入100℃烘箱中烘至衡量,称取质量为m2,MLP-MSS/TSF-BF的热水溶失率按下式进行计算:
热水溶失率(%)=(m1-m2)/m1×100
2、拉伸性能的测定
用万能材料试验机进行测试,拉伸速度为10mm/min,夹距为28mm,按照GB/T1040-2006,试样是标准长条形的样条。测试前将样条在常温条件下平衡24h后测定。
3、抗菌效价测定
以大肠杆菌(革兰氏阴性菌)和金黄色葡萄球菌(革兰氏阳性菌)为指示菌,将抗菌MLP-MSS/TSF-BF贴于培养皿表面,检测其抑菌活性。
实施例1不同桑叶粉添加量的MLP-MSS/TSF-BF
1、试验方法
(1)桑蚕丝胶溶液的制备:称取桑蚕茧壳10g,放入120mL蒸馏水中,于100℃回流处理30min后,过滤收集丝胶溶液,得到浓度为4.50μg/mL的丝胶溶液,4℃冰箱保存以备使用。
(2)柞蚕丝素溶液的制备:称取180g的四水合硝酸钙晶体,在80℃条件下加热并搅拌30min后,得到熔融的硝酸钙。用量筒量取100mL熔融的硝酸钙,倒入圆底烧瓶中,称取10g柞蚕丝素纤维加入其中,然后放置于油浴锅中在120℃条件下加热搅拌溶解2h后,冷却,装入截留分子量为8~10KDa透析袋,置于流动自来水中透析两天,再于去离子水中透析一天,每2~4h换一次水,透析3天后将得到柞蚕丝素溶液,浓度为27.5mg/mL,置于4℃冰箱储藏备用。
(3)明胶溶液的制备:精密称取1.5g明胶,加入4mL蒸馏水,加热搅拌至溶解,得到375mg/mL明胶溶液。
(4)桑叶粉的制备:取沙2×109桑叶,在200℃温度杀青至桑叶边缘翻卷,100℃左右干燥,然后用粉碎机粉碎至桑叶粒径低于500nm。
(5)取丝胶溶液与丝素溶液体积比为2:1的混合液3mL,再加入3mL聚乙二醇200、1.5mL 357mg/mL明胶,然后在其配方中分别加入0.0375g、0.0750g、0.1125g、0.1500g、0.1875g的桑叶粉,使配方中桑叶粉的比例分别为0.5%、1%、1.5%、2%、2.5%,设置对照组不添加桑叶粉,其中,室温放置48h后添加1%桑叶粉的MLP-MSS/TSF-BF如图1所示。
2、实验结果
(1)MLP-MSS/TSF-BF的溶失率分析
从图2可知,随着添加桑叶粉浓度的增加,MLP-MSS/TSF-BF的溶失率呈先下降后上升的趋势。添加1%桑叶粉时,MLP-MSS/TSF-BF的溶失率达到最小,为54.82%。
(2)MLP-MSS/TSF-BF的断裂伸长率和断裂强度分析
从图3可知,随着桑叶粉浓度的增加,MLP-MSS/TSF-BF的断裂伸长率先减小后增大,表明膜的柔软性先减小后增大。而断裂强度随着桑叶粉浓度的升高先增大后减小,表明膜的硬度先增大后减小。当添加桑叶粉浓度为1%时,MLP-MSS/TSF-BF的断裂强度达到最大,表明膜的硬度达到最大。故此,添加桑叶粉浓度为1%时,TSF-MSS/TSF-BF的拉伸性能达到最优,断裂伸长率为31.93%、断裂强度为8.16KPa。
因此,综合溶失率、断裂伸长率和断裂强度,添加桑叶粉浓度为1%时,MLP-MSS/TSF-BF的性能达到最优。
(3)MLP-MSS/TSF-BF抑菌活性分析
添加桑叶粉浓度为1%的MLP-MSS/TSF-BF结果见图4,其中,图4中A为对金黄葡萄球菌抑菌图,图4中B为对大肠杆菌的抑菌效果图,1为对照组,2为实验组。从图中可看到,虽未加任何抗菌物质,MLP-MSS/TSF-BF也具有一定的抑菌活性。
实施例2
1、试验方法
(1)参照实施例1的方法,制备浓度为1μg/mL的丝胶溶液、浓度为10mg/mL柞蚕丝素溶液、浓度为500mg/mL的明胶溶液,以及桑叶粉,4℃冰箱保存以备使用。
(2)取制备的丝胶溶液与丝素溶液体积比为3:1的混合液4mL,再加入4mL聚乙二醇200、2mL 500mg/mL明胶,然后在其配方中分别加入1%桑叶粉,室温放置48h后成膜。
2、实验结果
所制备的MLP-MSS/TSF-BF共混膜的溶失率为57.4%、断裂伸长率为33.5%、断裂强度为7.85kPa,得到的MLP-MSS/TSF-BF也具有一定的抑菌活性。
实施例3
1、试验方法
(1)参照实施例1的方法,制备浓度为50μg/mL的丝胶溶液、浓度为50mg/mL柞蚕丝素溶液、浓度为100mg/mL的明胶溶液,以及桑叶粉,4℃冰箱保存以备使用。
(2)取制备的丝胶溶液与丝素溶液体积比为2:1的混合液3mL,再加入3mL聚乙二醇200、1.5mL 100mg/mL明胶,然后在其配方中分别加入1%桑叶粉,室温放置48h后成膜。
2、实验结果
所制备的MLP-MSS/TSF-BF共混膜的溶失率为61%、断裂伸长率为35.5%、断裂强度为8.05kPa,得到的MLP-MSS/TSF-BF也具有一定的抑菌活性。
以上所述实施例仅表达了本发明的部分实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。应当指出的是,对于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,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。
Claims (8)
1.一种桑叶粉-桑蚕丝胶/柞蚕丝素共混膜的制备方法,其特征在于,先将桑蚕丝胶溶液与柞蚕丝素溶液混合均匀;再加入明胶溶液和聚乙二醇溶液混合均匀;最后加桑叶粉混合均匀,干燥即得桑叶粉-桑蚕丝胶/柞蚕丝素共混膜;
具体的,所述制备方法包括如下步骤:
S1.制备10~50mg/mL的柞蚕丝素溶液和1~50μg/mL的桑蚕丝胶溶液;
S2.将步骤S1制得的柞蚕丝素溶液与桑蚕丝胶溶液混合均匀得到桑蚕丝胶/柞蚕丝素混合液1;
S3.向步骤S2制得的混合液1中加入100~500mg/mL的明胶溶液和聚乙二醇200,混合均匀,得到桑蚕丝胶/柞蚕丝素混合液2;
S4.向步骤S3得到的混合液2中加入桑叶粉混合均匀,得到桑叶粉-桑蚕丝胶/柞蚕丝素混合液;
S5.将步骤S4制得的桑叶粉-桑蚕丝胶/柞蚕丝素混合液干燥,即得桑叶粉-桑蚕丝胶/柞蚕丝素共混膜;
其中,所述桑蚕丝胶溶液的制备方法如下:
称取桑蚕茧壳加入蒸馏水,于100℃进行回流处理30min后,过滤收集丝胶溶液;
所述柞蚕丝素溶液的制备方法如下:
称取180g的四水合硝酸钙晶体,在80℃条件下加热并搅拌30min后,得到熔融的硝酸钙;用量筒量取100mL熔融的硝酸钙,倒入圆底烧瓶中,称取柞蚕丝素纤维加入其中,然后放置于油浴锅中在120℃条件下加热搅拌溶解2h后,冷却,装入截留分子量为8~10KDa透析袋,置于流动自来水中透析两天,再于去离子水中透析一天,每2~4h换一次水,透析3天后将得到柞蚕丝素溶液;
步骤S4所述桑叶粉的添加量占桑叶粉-桑蚕丝胶/柞蚕丝素混合液的质量分数为0.5~1%。
2.根据权利要求1所述方法,其特征在于,步骤S4所述桑叶粉的粒径低于500nm。
3.根据权利要求1所述方法,其特征在于,柞蚕丝素溶液与桑蚕丝胶溶液的体积比为0.5~1.5:1~3。
4.根据权利要求1所述方法,其特征在于,柞蚕丝素溶液、桑蚕丝胶溶液、明胶溶液和聚乙二醇200的体积比为0.5~1.5:1~3:1~2:2~4。
5.根据权利要求1所述方法,其特征在于,所述干燥为在20~60℃下干燥24~96h。
6.根据权利要求1所述方法,其特征在于,步骤S2、S3、S4中混合均匀为在60~80℃下搅拌1~2min混合均匀。
7.根据权利要求1~6任一所述方法制备得到的桑叶粉-桑蚕丝胶/柞蚕丝素共混膜。
8.权利要求7所述共混膜在制备生物材料方面的应用。
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