CN116217980A - 一种具有生物传感性能与抗菌作用的共析凝胶及其制备方法 - Google Patents
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Abstract
本发明公开一种共析凝胶的制备方法,包括以下步骤:S1:将氯化胆碱、甘油与氯化锌在90‑100℃下搅拌,直至形成澄清透明液体;S2:加入N‑羟乙基丙烯酰胺(HEAA)、2‑羟基‑2‑甲基‑1‑[4‑(2‑羟基乙氧基)苯基]‑1‑丙酮以及N,N‑亚甲基丙烯酰胺,在60‑70℃下搅拌,直至液体均质,紫外光下光照后得到共析凝胶。本发明制备的共析凝胶,其具体制备过程符合绿色化学的制备标准,通过将具有导电性能与抗菌性能的深共晶溶剂作为凝胶中溶剂,实现凝胶力学强度的增强以及使凝胶具有传感与抗菌性能,并且由于深共晶溶剂本身不易挥发的特性,提高了凝胶的服役时间。
Description
技术领域
本发明属于生物医用材料领域,具体涉及一种具有生物传感性能与抗菌作用的共析凝胶及其制备方法。
背景技术
水凝胶是一种能够在水中溶胀并保持一定水分而又不溶于水的具有三维网络结构的新型功能高分子材料,兼具有固体和液体的性质,由于水凝胶可以适应机械变形和导电,因此被应用于可穿戴式柔性应变传感器,用于人体运动信号监测。然而,虽然凝胶本身也具有传感性能,但是导电性较弱,在该领域的应用仍存在局限性。再者,水凝胶的细胞毒性、低灵敏度和导电性限制了它们的适用性。因此,协同改善水凝胶的伸展性、灵敏度和生物相容性,用于可穿戴柔性应变传感器仍然是一个挑战;此外,由于水分子的易挥发性,长期使用状态下水凝胶材料中的水分子不可避免地流失,从而导致水凝胶性能变化,影响水凝胶发挥作用。
深共晶溶剂是一种不易挥发,并且组分可调的,使用绿色化学方法制备的溶剂,由于其组分可调所以其本身性能可调,但是深共晶溶剂作为液体存在,应用在各个方面受到限制,因为其本身具有流动性,不易固定在使用部位。
发明内容
本发明目的是提供一种具有生物传感性能与抗菌作用的共析凝胶及其制备方法,以解决深共晶溶剂作为液体存在,应用受到限制的问题,同时进一步提升体系的导电性能。
为实现上述目的,本发明提供一种共析凝胶的制备方法,包括以下步骤:
S1:将氯化胆碱、甘油与氯化锌在90-100℃下搅拌,直至形成澄清透明液体,得到深共晶溶剂;
S2:加入N-羟乙基丙烯酰胺、引发剂以及交联剂,在60-70℃下搅拌,直至液体均质,紫外光下光照后得到共析凝胶。
优选的,所述引发剂包括2-羟基-2-甲基-1-[4-(2-羟基乙氧基)苯基]-1-丙酮;所述交联剂包括N,N-亚甲基丙烯酰胺。
优选的,氯化胆碱、甘油、氯化锌用量比为氯化胆碱、甘油、氯化锌用量质量比为1:1~2:0~0.33。
优选的,N-羟乙基丙烯酰胺与所述深共晶溶剂质量比为7:3~3:7;引发剂用量为N-羟乙基丙烯酰胺单体用量的0.2%;交联剂用量为N-羟乙基丙烯酰胺单体用量的0.03%。
优选的,步骤S1中所述搅拌方法包括在90-100℃的油浴锅中,用200-800rpm的转速磁力搅拌器搅拌。
优选的,步骤S2中所述搅拌方法包括在60-70℃的油浴锅中,用400-1000rpm的转速磁力搅拌器搅拌。
优选的,步骤S2在避光下进行。
优选的,步骤S2中所述紫外光下光照的方法包括在365nm紫外光下光照2-5min。
具体来说,所述共析凝胶的制备方法,包括以下步骤:
S1:深共晶溶剂的制备方法:将1.423g氯化胆碱、1.877g甘油与0.3g氯化锌在100℃下油浴,转速500rpm下搅拌直至形成澄清透明液体;
S2:共析凝胶的制备方法:在避光条件下,再加入8.75g的N-羟乙基丙烯酰胺、340.9mg的2-羟基-2-甲基-1-[4-(2-羟基乙氧基)苯基]-1-丙酮以及3.5mg的N,N-亚甲基丙烯酰胺,在70℃下的油浴,在转速800rpm下搅拌5min至溶液达到均质状态,然后置于365nm紫外光下光照5min后得到共析凝胶。
本发明提供一种用上述共析凝胶的制备方法制备的共析凝胶。
与现有技术相比,本发明的有益效果:
本发明提供了一种具有生物传感性能与抗菌作用的共析凝胶,其具体制备过程符合绿色化学的制备标准,通过将具有导电性能与抗菌性能的深共晶溶剂作为凝胶中溶剂,实现凝胶力学强度的增强以及使凝胶具有传感与抗菌性能,并且由于深共晶溶剂本身不易挥发的特性,提高了凝胶的服役时间。
本发明将深共晶溶剂引入凝胶体系,作为凝胶体系的溶剂,首先,深共晶溶剂中含有可形成氢键相互作用的基团,可以提高凝胶的力学性能;其次,深共晶溶剂本身不易挥发,可以使凝胶长时间使用不脱水;由于使用的深共晶溶剂本身具有优良导电性与抗菌性能,所以将其引入凝胶体系可以使凝胶强度与导电性能提高与并提供优良的抗菌性能,二者的结合产生了协同作用。
附图说明
图1是实施例中制得的深共晶溶剂的光学图片;
图2是实施例中具有生物传感性能与抗菌作用的共析凝胶制备示意图;
图3是实施例得到的共析凝胶的应力-应变曲线图;
图4是实施例得到的共析凝胶的菌落统计图;
图5是实施例得到的共析凝胶的拉伸传感曲线图。
具体实施方式
以下结合具体实施例对本发明作进一步说明,但不以任何方式限制本发明。
本发明具有生物传感性能与抗菌作用的共析凝胶的制备方法,包括以下步骤:
S1:在50mL离心管中,加入1.423g氯化胆碱、0.9385-1.877g甘油与0.1-0.3g氯化锌,向离心管中加入磁子,将上述离心管放置到90-100℃的油浴锅中,在200-800rpm的磁力搅拌下,直至形成澄清透明液体。
S2:在避光条件下,向步骤1所述的离心管中依次加入8.75g的N-羟乙基丙烯酰胺(HEAA)、340.9mg的2-羟基-2-甲基-1-[4-(2-羟基乙氧基)苯基]-1-丙酮以及3.5mg的N,N-亚甲基丙烯酰胺,将其转移至60-70℃的油浴锅中进行磁力搅拌,转速为400-1000rpm,直至液体为均质,将上述溶液在避光条件下转移至不同形状的模具中,置于365nm紫外光下光照2-5min后得到共析凝胶。
市面上目前出现的深共晶溶剂几乎所有的都具有不挥发性,少数的会有导电性能,而本发明制备的深共晶溶剂具备抗菌性能同时兼具不挥发与导电性。
实施例1
步骤1:
深共晶溶剂的制备方法,包括以下步骤:
在50mL离心管中,加入1.423g氯化胆碱、1.877g甘油与0.3g氯化锌,向离心管中加入磁子,将上述离心管放置到100℃的油浴锅中,200-800rpm,优选值为500rpm搅拌直至形成澄清透明液体。
如图1所示,为本发明制备的深共晶溶剂的光学图片,从图中可以看出样品瓶中液体为澄清透明,证明深共晶溶剂制备成功。
步骤2:
共析凝胶的制备方法,具体如下:
在避光条件下,向步骤1所述的离心管中依次加入8.75g的N-羟乙基丙烯酰胺、340.9mg的2-羟基-2-甲基-1-[4-(2-羟基乙氧基)苯基]-1-丙酮以及3.5mg的N,N-亚甲基丙烯酰胺,将其转移至70℃的油浴锅中400-1000rpm,优选800rpm搅拌5min至溶液达到均质状态,将上述溶液在避光条件下转移至不同形状的模具中,置于365nm紫外光下光照5min后得到共析凝胶。
图2是本发明共析凝胶制备示意图,即先制备得到深共晶溶剂,然后将单体、引发剂、交联剂与深共晶溶剂加热混合,然后紫外光下照射成胶。
使用万能力学试验机测试实施例1得到的共析凝胶的力学性能。
采用哑铃型模具制得共析凝胶的标距长度为15mm,宽度为2mm,厚度为2mm。采用拉伸试验测定凝胶力学性能,拉伸速度为100mm/min,水凝胶断裂时停止测试。水凝胶拉伸强度为水凝胶断裂时的应力,拉伸模量为应力-应变曲线中线性区域的斜率,延长率为水凝胶断裂时的应变,韧性为应力-应变曲线的积分,对照组为溶剂为水,组他组分完全相同得水凝胶。如图3所示,为本发明实施例1制备的共析凝胶的应力-应变曲线图,从图3中可以看出上述共析凝胶拉伸强度、断裂伸长率以及韧性与同组分的水凝胶相比均有大幅度提升,这主要是因为深共晶溶剂与水相比有更多的氢键结合位点,与凝胶网络结合更加紧密。
本发明实施例1制备的共析凝胶对金黄色葡萄球菌与大肠杆菌的抗菌性能测试。
将金黄色葡萄球菌与大肠杆菌在-80℃超低温冰箱中取出,将其放入超净台中进行操作,待菌种融化后用灭菌接种环扣取试管中的冷冻菌块放入20mL的Luria-Bertani(LB)培养基中,37℃、150rpm过夜培养。取过夜后的菌液,用酶标仪测量其OD630,将菌液浓度稀释至106CFU/mL备用。取实施例得到的共析凝胶0.5g加入15mL样品瓶中,再加其中滴加9mL稀释好的菌液,对照组只放9mL稀释好的菌液,将上述样品瓶放入37℃孵箱孵育4h。孵育完成后进行涂板,将琼脂板平分为三份做平行样,在每一份上滴加30μL孵育后的菌液,然后用一次性涂布棒将其在这一区域内涂布均匀,将涂好的琼脂板放入37℃孵箱孵育过夜,孵育完成后将琼脂板放置在菌落计数器下进行拍照。如图4所示,是本发明实施例1制备得到的共析凝胶的菌落统计图,可以看出使用制得的共析凝胶的菌落数明显少于对照组的,由此判断制得的共析凝胶有较强的抗菌作用,这是由于共析凝胶使用的溶剂为具有抗菌作用的深共晶溶剂。
本发明实施例1得到的共析凝胶生物传感性能测试。
采用哑铃型模具制得共析凝胶的标距长度为15mm,宽度为2mm,厚度为2mm。采用拉伸试验测定凝胶力学性能,拉伸速度为100mm/min,当应变大于等于300%时停止测试。测试时在凝胶标距两端夹上导线,导线另一端接上数字源表,将拉伸机与数字源表同时开始测试。如图5所示,是本发明实施例1得到的共析凝胶的拉伸传感曲线图,从图中可以算得出拉伸传感系数为1.43,这表明制得的共析凝胶具有较好的传感性能。
对于任何熟悉本领域的技术人员而言,在不脱离本发明技术方案范围情况下,都可利用上述揭示的技术内容对本发明技术方案作出许多可能的变动和修饰,或修改为等同变化的等效实施例。因此,凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所做的任何简单修改、等同变化及修饰,均应仍属于本发明技术方案保护的范围内。
Claims (10)
1.一种共析凝胶的制备方法,其特征在于,包括以下步骤:
S1:将氯化胆碱、甘油与氯化锌在90-100℃下搅拌,直至形成澄清透明液体,得到深共晶溶剂;
S2:加入N-羟乙基丙烯酰胺、引发剂以及交联剂,在60-70℃下搅拌,直至液体均质,紫外光下光照后得到共析凝胶。
2.根据权利要求1所述共析凝胶的制备方法,其特征在于,氯化胆碱、甘油、氯化锌用量质量比为1:1~2:0~0.33。
3.根据权利要求1所述共析凝胶的制备方法,其特征在于,所述引发剂包括2-羟基-2-甲基-1-[4-(2-羟基乙氧基)苯基]-1-丙酮;所述交联剂包括N,N-亚甲基丙烯酰胺。
4.根据权利要求1所述共析凝胶的制备方法,其特征在于,N-羟乙基丙烯酰胺与所述深共晶溶剂质量比为7:3~3:7;引发剂用量为N-羟乙基丙烯酰胺单体用量的0.2%;交联剂用量为N-羟乙基丙烯酰胺单体用量的0.03%。
5.根据权利要求1所述共析凝胶的制备方法,其特征在于,步骤S1中所述搅拌方法包括在90-100℃的油浴锅中,用200-800rpm的转速磁力搅拌器搅拌。
6.根据权利要求1所述共析凝胶的制备方法,其特征在于,步骤S2中所述搅拌方法包括在60-70℃的油浴锅中,用400-1000rpm的转速磁力搅拌器搅拌。
7.根据权利要求1所述共析凝胶的制备方法,其特征在于,步骤S2在避光下进行。
8.根据权利要求1所述共析凝胶的制备方法,其特征在于,步骤S2中所述紫外光下光照的方法包括在365nm紫外光下光照2-5min。
9.根据权利要求1-7所述共析凝胶的制备方法,其特征在于,包括以下步骤:
S1:深共晶溶剂的制备方法:将1.423g氯化胆碱、1.877g甘油与0.3g氯化锌在100℃下油浴,转速500rpm下搅拌直至形成澄清透明液体;
S2:共析凝胶的制备方法:在避光条件下,再加入8.75g的N-羟乙基丙烯酰胺、340.9mg的2-羟基-2-甲基-1-[4-(2-羟基乙氧基)苯基]-1-丙酮以及3.5mg的N,N-亚甲基丙烯酰胺,在70℃下的油浴,在转速800rpm下搅拌5min至溶液达到均质状态,然后置于365nm紫外光下光照5min后得到共析凝胶。
10.一种用权利要求1-9任一所述共析凝胶的制备方法制备的共析凝胶。
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