CN116425907A - 一种医用凝胶及其在制备硫酸镁湿敷贴中的应用 - Google Patents
一种医用凝胶及其在制备硫酸镁湿敷贴中的应用 Download PDFInfo
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- CN116425907A CN116425907A CN202310197813.3A CN202310197813A CN116425907A CN 116425907 A CN116425907 A CN 116425907A CN 202310197813 A CN202310197813 A CN 202310197813A CN 116425907 A CN116425907 A CN 116425907A
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- polyacrylic acid
- magnesium sulfate
- medical gel
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Abstract
本发明公开了一种医用凝胶及其在制备硫酸镁湿敷贴中的应用,涉及医疗器械技术领域。该医用凝胶包括改性聚丙烯酸;上述改性聚丙烯酸,包括:聚丙烯酸网络结构和穿插附着于所述聚丙烯网络结构内部的网状结构;上述网状结构包括改性葫芦[n]脲;上述改性葫芦[n]脲包括4‑溴巴豆酸或3‑氯‑2‑羟基丙烷磺酸化学修饰的葫芦[n]脲。本发明提供的医用凝胶表现出更佳的物化性能,应用于制备硫酸镁湿敷贴,获得产品具有更佳的透气性,且液体吸收溶胀性能得到明显增强,为创口的恢复提供更加优异的环境。
Description
技术领域
本发明属于医疗器械技术领域,具体涉及一种医用凝胶及其在制备硫酸镁湿敷贴中的应用。
背景技术
硫酸镁属盐,其化学性质稳定,不被吸收,而50%硫酸镁溶液对组织液而言则相应地为高渗溶液,局部湿敷可产生高渗透压,由于高渗透压平衡原理,使肿胀部位组织水肿液在短时间内吸出、消肿,从而减轻水肿对局部组织的损伤,起到局部治疗作用,临床观察无副作用及不良反应,方法简便易行。硫酸镁热敷消肿原理:因为硫酸镁可以拮抗钙离子,而钙离子是参与平滑肌收缩的,因此硫酸镁可以舒张皮肤及皮下组织血管平滑肌,降低毛细血管血压,减轻局部渗出,水肿也就减轻。而大血管平滑肌含量少,所以主要用于表浅炎症。
多年以来,用水凝胶敷于患处或将硫酸镁溶液浸泡的纱布敷于患处,用于在肌肉注射、输液引起的皮下渗液肿胀、疼痛及静脉炎、软组织炎症肿胀、穿刺引起的炎症及肿胀的辅助治疗。一直为广大医生所采用,目前常用的水凝胶在辅助治疗中起到对患处组织周围降温的冷敷作用,但辅助治疗的效果没有硫酸镁湿敷好。现有的硫酸镁湿敷贴多采用无纺布浸湿硫酸镁湿敷液封装于包装袋内,使用时,将湿敷贴敷于患处,用保鲜膜包裹,防止水分蒸发或液体流出沾湿床单或衣物。病人患处皮肤在密不透气的情况下,较长时间接触高浓度盐溶液,致使皮肤免疫功能下降,易受感染或引起水泡红疹等。并且硫酸镁湿敷需要临时配制,操作不方便,耽误时间,使用过程中纱布易脱落,水分易蒸发,严重影响了硫酸镁湿敷的效果。
发明内容
本发明的目的在于提供一种医用凝胶及其在制备硫酸镁湿敷贴中的应用,该医用凝胶表现出更佳的物化性能,应用于制备硫酸镁湿敷贴,获得产品具有更佳的透气性,且液体吸收溶胀性能得到明显增强,为创口的恢复提供更加优异的环境。
本发明为实现上述目的所采取的技术方案为:
一种改性聚丙烯酸,包括:聚丙烯酸网络结构和穿插附着于所述聚丙烯网络结构内部的网状结构;上述网状结构包括改性葫芦[n]脲;上述改性葫芦[n]脲包括4-溴巴豆酸或3-氯-2-羟基丙烷磺酸化学修饰的葫芦[n]脲。本发明采用4-溴巴豆酸或3-氯-2-羟基丙烷磺酸通过化学修饰手段对葫芦[n]脲进行改性,获得改性葫芦[n]脲,作为交联剂应用于改性聚丙烯酸的制备过程中,制得的改性聚丙烯酸具有更优的物化性能。将其用于医用凝胶的制备工艺中,获得的医用凝胶具有更高的黏度,能够更好地涂覆于无纺布上,制得湿敷贴,表现出更优的水蒸气透过性能,且吸附溶胀能力得到改善,液体吸收容量增大,且水洗完整性及稳定性明显增强。其原因可能在于,采用4-溴巴豆酸或3-氯-2-羟基丙烷磺酸对葫芦[n]脲进行改性,引入更多的含氧活性官能团,能够更好地与改性聚丙烯酸主链结构之间形成分子间作用力,得到更为均匀稳定的三维网络结构,进而形成更加稳定的凝胶结构,使其吸收溶胀能力得到改善;同时改性后的葫芦[n]脲可能更加均匀、稳定的分布于三维凝胶网络结构中,得到的湿敷贴表现出更佳的透气能力。
优选地,改性葫芦[n]脲中,n=5、6或7。
优选地,改性聚丙烯酸的分子量为5万~10万。
上述改性CB[n]的制备方法,包括:
采用过硫酸钾对CB[n]进行活化处理,得到活化的CB[n];
然后在NaH作用下,活化的CB[n]与4-溴巴豆酸或3-氯-2-羟基丙烷磺酸反应获得改性CB[n]。
进一步的,上述改性CB[n]的制备方法,具体为:
取CB[n]分散于水中,加入过硫酸钾、硫酸钾,80~85℃水浴条件下搅拌10~12h,冷却至室温,过滤收集滤液,50~55℃旋蒸至体积量的1/35~1/40,冷却至室温,过滤得到滤液,加入8~12倍体积量的浓盐酸萃取,冷却后加入等体积量的甲醇,抽滤,用甲醇洗涤滤饼,40~45℃真空干燥得到活化的CB[n];
取活化的CB[n]加入DMSO,超声分散8~12min,充入氩气保护8~12min,加入NaH,再用氩气保护8~12min,然后室温下搅拌反应3~5h;之后冰水浴条件下加入4-溴巴豆酸和3-氯-2-羟基丙烷磺酸,室温下密封反应10~12h;然后将反应体系倒入乙醚中,抽滤、38~40℃甲醇洗涤,得到滤饼在40~45℃下真空干燥得到改性CB[n]。
优选地,CB[n]与水的固液比为1g:30~50mL;过硫酸钾与CB[n]的质量比为0.1~0.2:1;硫酸钾与CB[n]的质量比为0.6~0.8:1。
优选地,活化的CB[n]与DMSO的固液比为1g:300~500mL;NaH与活化的CB[n]的质量比为0.1~0.3:1;4-溴巴豆酸与CB[n]的质量比为0.2~0.3:1;4-溴巴豆酸和3-氯-2-羟基丙烷磺酸的摩尔比为0.6~0.8:1。
本发明还公开了上述改性聚丙烯酸的制备方法,包括:
取丙烯酸、改性CB[7]加入水,再加入APS、氯化钠,超声10~15min,充入氮气10~15min,然后置于60~70℃水浴条件下反应3~6h,干燥得到改性聚丙烯酸。
优选地,丙烯酸与水的体积比为1:4~6;改性CB[7]的加入量为丙烯酸的1.5~3wt%;APS与丙烯酸的质量比为0.01~0.03:1;氯化钠的加入量为丙烯酸的1~2wt%。
本发明还公开了上述改性聚丙烯酸在制备医用凝胶中的用途。
一种医用凝胶,包括:上述改性聚丙烯酸。
优选地,医用凝胶原料包括:按重量份计,12~16份甘油,3~6份改性聚丙烯酸,0.2~0.4份尼泊金乙酯,0.01~0.05份高岭土,0.1~0.15份甘羟铝,0.06~0.15份桉叶油,50~60份纯净水,15~26份硫酸镁,1~3份聚乙烯吡咯烷酮,0.2~0.3份酒石酸,0.04~0.08份乙二胺四乙酸二钠。
上述医用凝胶的制备方法,具体为:
将改性聚丙烯酸、尼泊金乙酯、高岭土、甘羟铝、桉叶油混合分散于甘油中获得油相成分;将硫酸镁、乙二胺四乙酸二钠溶于纯净水中,然后加入聚乙烯吡咯烷酮和酒石酸,搅拌均匀得到水相;
真空条件下将油相和水相充分混合,控制真空压强不小于85MPa,搅拌20~30min得到医用凝胶。
更优选地,医用凝胶的油相中还加入0.05~0.3重量份丁香酚衍生物。
需要说明的是,上述丁香酚衍生物由N-乙酰基-3-氯丙氨酸甲酯化学修饰丁香酚获得。本发明采用N-乙酰基-3-氯丙氨酸甲酯通过化学键对丁香酚进行改性,制备获得的丁香酚衍生物表现出更高的生物活性,其抗菌抑菌能力增强,且镇痛作用也得到有效增强。将其应用于应用凝胶的制备工艺中,能够使得凝胶具有更优的杀菌、镇痛作用,并且一定程度上改善了硫酸镁湿敷贴的透气性能,可能是由于改性丁香酚的加入对凝胶网络结构产生了一定的有益影响。
一种硫酸镁湿敷贴,包括防粘层、上述医用凝胶形成的水凝胶层和背衬层;上述水凝胶层位于防粘层与背衬层之间。
优选地,水凝胶层的厚度为0.1~4mm。
优选地,防粘层包括聚乙烯薄膜,厚度为0.05~0.5mm。
优选地,背衬层包括无纺布,规格为60~80g/m2。
本发明的又一目的在于,公开了上述硫酸镁湿敷贴的制备方法,包括:
取医用凝胶采用涂布机将其均匀涂覆于防粘层下表面,形成水凝胶层,之后一并贴覆于背衬层上表面,通过切割、固化12~15h、包装即得硫酸镁湿敷贴。
本发明又公开了上述医用凝胶在制备硫酸镁湿敷贴中的用途。
相比于现有技术,本发明具有如下有益效果:
本发明采用4-溴巴豆酸或3-氯-2-羟基丙烷磺酸通过化学修饰手段对葫芦[n]脲进行改性,获得改性葫芦[n]脲,制备获得改性聚丙烯酸,并将其用于医用凝胶的制备工艺中,获得的医用凝胶具有更高的黏度;应用于湿敷贴的制备工艺中,获得的产品表现出更优的水蒸气透过性能,且吸附溶胀能力得到改善,液体吸收容量增大,且水洗完整性及稳定性明显增强。同时,本发明采用N-乙酰基-3-氯丙氨酸甲酯通过化学键对丁香酚进行改性,制备获得的丁香酚衍生物表现出更强的抗菌抑菌能力和镇痛作用;将其应用于应用凝胶的制备工艺中,能够使得凝胶具有更优的杀菌、镇痛作用,并且一定程度上改善了硫酸镁湿敷贴的透气性能。本发明将传统湿敷方式的硫酸镁溶液交联在水凝胶中,通过水凝胶能自由释放分子框架结构,使其渗透至肌肤表面,发挥其高深作用和舒缓平滑肌。
因此,本发明提供了一种医用凝胶及其在制备硫酸镁湿敷贴中的应用,该医用凝胶表现出更佳的物化性能,应用于制备硫酸镁湿敷贴,获得产品具有更佳的透气性,且液体吸收溶胀性能得到明显增强,为创口的恢复提供更加优异的环境。
附图说明
图1是本发明中制备的改性CB[7]以及活化的CB[7]的红外光谱;
图2是本发明中制备的改性聚丙烯酸的红外光谱;
图3是本发明中制备的医用凝胶的黏度测试结果;
图4是本发明中制备的硫酸镁湿敷贴的水蒸气透过性测试结果。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合实施例对本发明的各实施方式进行详细的阐述。然而,本领域的普通技术人员可以理解,在本发明各实施方式中,为了使读者更好地理解本申请而提出了许多技术细节。但是,即使没有这些技术细节和基于以下各实施方式的种种变化和修改,也可以实现本申请所要求保护的技术方案。
本发明实施例所用述聚乙烯吡咯烷酮为K90。
实施例1:
一种医用凝胶,包括:按重量份计,15份甘油,4份改性聚丙烯酸,0.3份尼泊金乙酯,0.03份高岭土,0.12份甘羟铝,0.09份桉叶油,56份纯净水,24份硫酸镁,2份聚乙烯吡咯烷酮,0.25份酒石酸,0.06份乙二胺四乙酸二钠。
上述医用凝胶的制备方法,具体为:
将改性聚丙烯酸、尼泊金乙酯、高岭土、甘羟铝、桉叶油混合分散于甘油中获得油相成分;将硫酸镁、乙二胺四乙酸二钠溶于纯净水中,然后加入聚乙烯吡咯烷酮和酒石酸,搅拌均匀得到水相;
真空条件下将油相和水相充分混合,控制真空压强87MPa,搅拌30min得到医用凝胶。
上述改性CB[7]的制备:
按照固液比为1g:42mL的比例取CB[7]分散于水中,加入过硫酸钾、硫酸钾,85℃水浴条件下搅拌12h,冷却至室温,过滤收集滤液,50℃旋蒸至体积量的1/40,冷却至室温,过滤得到滤液,加入10倍体积量的浓盐酸萃取,冷却后加入等体积量的甲醇,抽滤,用甲醇洗涤滤饼,40℃真空干燥得到活化的CB[7];需要说明的是,过硫酸钾与CB[7]的质量比为0.15:1;硫酸钾与CB[7]的质量比为0.7:1;
按照固液比为1g:420mL的比例取活化的CB[7]加入DMSO,超声分散10min,充入氩气保护10min,加入NaH,再用氩气保护10min,然后室温下搅拌反应4.5h;之后冰水浴条件下加入4-溴巴豆酸和3-氯-2-羟基丙烷磺酸,室温下密封反应12h;然后将反应体系倒入乙醚中,抽滤、38℃甲醇洗涤,得到滤饼在40℃下真空干燥得到改性CB[7];需要说明的是,NaH与活化的CB[7]的质量比为0.2:1;4-溴巴豆酸与CB[7]的质量比为0.56:1。
上述改性聚丙烯酸的制备:
取丙烯酸、改性CB[7]加入水,再加入APS、氯化钠,超声10min,充入氮气10min,然后置于66℃水浴条件下反应5h,干燥得到改性聚丙烯酸(分子量7.6万);具体制备工艺中,丙烯酸与水的体积比为1:5;改性CB[7]的加入量为丙烯酸的2.1wt%;APS与丙烯酸的质量比为0.02:1;氯化钠的加入量为丙烯酸的1.4wt%。
硫酸镁湿敷贴的制备:
取医用凝胶采用涂布机将其均匀涂覆于防粘层(聚乙烯薄膜,厚度为0.3mm)下表面,形成水凝胶层(厚度为2.5mm),之后一并贴覆于背衬层(无纺布,规格为72g/m2)上表面,通过切割、固化12h、包装即得硫酸镁湿敷贴。
实施例2:
一种医用凝胶,其组分与实施例1存在区别,具体包括:按重量份计,12份甘油,3份改性聚丙烯酸,0.2份尼泊金乙酯,0.05份高岭土,0.15份甘羟铝,0.07份桉叶油,50份纯净水,16份硫酸镁,1份聚乙烯吡咯烷酮,0.2份酒石酸,0.08份乙二胺四乙酸二钠。
上述医用凝胶的制备方法与实施例1相同。
改性聚丙烯酸的制备与实施例1的区别:改性CB[7]的加入量为丙烯酸的1.7wt%;APS与丙烯酸的质量比为0.014:1;氯化钠的加入量为丙烯酸的1.2wt%;改性聚丙烯酸的分子量为7.2万。
改性CB[7]的制备与实施例1相同。
硫酸镁湿敷贴的制备与实施例1的区别:医用凝胶为本实施例制备的,水凝胶层的厚度为3.4mm。
实施例3:
一种医用凝胶,其组分与实施例1存在区别,具体包括:按重量份计,16份甘油,6份改性聚丙烯酸,0.36份尼泊金乙酯,0.02份高岭土,0.1份甘羟铝, 0.15份桉叶油,58份纯净水,24份硫酸镁,3份聚乙烯吡咯烷酮,0.28份酒石酸,0.04份乙二胺四乙酸二钠。
上述医用凝胶的制备方法与实施例1相同。
改性聚丙烯酸的制备与实施例1的区别:改性CB[7]的加入量为丙烯酸的3wt%;APS与丙烯酸的质量比为0.03:1;氯化钠的加入量为丙烯酸的2wt%;改性聚丙烯酸的分子量为8万。
改性CB[7]的制备与实施例1相同。
硫酸镁湿敷贴的制备与实施例1的区别:医用凝胶为本实施例制备的,水凝胶层的厚度为1.5mm。
实施例4:
一种医用凝胶,其组分与实施例1存在区别:改性聚丙烯酸为本实施例制备的。
上述医用凝胶的制备方法与实施例1相同。
改性聚丙烯酸的制备与实施例1的区别:改性CB[7]为本实施例制备的。
改性CB[7]的制备与实施例1的区别:采用同等摩尔量的3-氯-2-羟基丙烷磺酸替代4-溴巴豆酸。
硫酸镁湿敷贴的制备与实施例1的区别:医用凝胶为本实施例制备的。
实施例5:
一种医用凝胶与实施例1的区别:原料组分还包括0.2重量份丁香酚衍生物,在制备过程中作为油相成分。
丁香酚衍生物的制备:
取氢氧化钾加入95%浓度的乙醇中,搅拌加热溶解,然后缓慢滴加丁香酚,反应至TLC检测无丁香酚斑点,之后缓慢加入N-乙酰基-3-氯丙氨酸甲酯,升温至63℃反应12h;接着过滤、减压浓缩,加入适量苯溶解后置于分液漏斗中,依次用等体积的5%浓度氢氧化钠水溶液、饱和氯化钠水溶液洗涤,分液得到有机相与水相;水相用苯萃取(3×10mL),合并萃取液,并与有机相复混,加入无水硫酸镁干燥过夜,减压除溶剂,然后经硅胶柱(洗脱剂为石油醚:乙酸乙酯=5:1,v/v)分离纯化得到丁香酚衍生物;1H NMR(400 MHz,CDCl3):δ:6.74~6.90(3H,Ar-H),6.05(m,1H,-CH),5.07、4.80(dd,2H,-CH2),4.40~4.70(2H,-CH2),4.55(1H,-CH),3.77、3.71(s,6H,O-CH3),3.32(d,2H,-CH2),1.86(s,3H,-CH3)。需要说明的是,氢氧化钾与95%浓度乙醇的固液比为0.07g:1mL;丁香酚与氢氧化钾的质量比为1:0.35;N-乙酰基-3-氯丙氨酸甲酯与丁香酚的摩尔比为1.3:1。
上述医用凝胶的制备方法与实施例1相同。
改性聚丙烯酸的制备与实施例1相同。
改性CB[7]的制备与实施例1相同。
硫酸镁湿敷贴的制备与实施例1的区别:医用凝胶为本实施例制备的。
实施例6:
一种医用凝胶与实施例5的区别:采用聚丙烯酸替代改性聚丙烯酸。
聚丙烯酸的制备与实施例5中改性聚丙烯酸的制备区别:采用过硫酸钾替代APS,采用BIS替代改性CB[7]。
上述医用凝胶的制备方法与实施例5相同。
硫酸镁湿敷贴的制备与实施例5的区别:医用凝胶为本实施例制备的。
实施例7:
一种医用凝胶与实施例5的区别:采用聚丙烯酸替代改性聚丙烯酸。
聚丙烯酸的制备与实施例5中改性聚丙烯酸的制备区别:采用CB[7]替代改性CB[7]。
上述医用凝胶的制备方法与实施例5相同。
硫酸镁湿敷贴的制备与实施例5的区别:医用凝胶为本实施例制备的。
对比例1:
一种医用凝胶与实施例1的区别:采用聚丙烯酸替代改性聚丙烯酸。
聚丙烯酸的制备与实施例6相同。
上述医用凝胶的制备方法与实施例1相同。
硫酸镁湿敷贴的制备与实施例1的区别:医用凝胶为本对比例制备的。
对比例2:
一种医用凝胶与实施例1的区别:改性聚丙烯酸为本对比例制备的。
改性聚丙烯酸的制备与实施例7相同。
上述医用凝胶的制备方法与实施例1相同。
硫酸镁湿敷贴的制备与实施例1的区别:医用凝胶为本对比例制备的。
试验例1:
红外表征
测试采用傅里叶变换红外光谱仪进行,测试波长4000~500cm-1。
对实施例1和实施例4中制备的改性CB[7]及活化的CB[7]进行上述测试,结果如图1所示。从图中分析可知,相比于活化的CB[7]红外测试结果,在实施例1制备的改性CB[7]的红外光谱中,1600~1650cm-1范围内存在C=C键的特征吸收峰,实施例4制备的改性CB[7]的红外光谱中1150~1200cm-1范围内存在磺酸基的特征吸收峰,表明实施例1和实施例4中改性CB[7]成功制备。
对实施例1和对比例2中制备的改性聚丙烯酸进行上述测试,结果如图2所示。从图中分析可知,相比于对比例2制备的改性聚丙烯酸红外测试结果,在实施例1制备的改性聚丙烯酸的红外光谱中,1600~1700cm-1范围内存在C=C键的特征吸收峰,表明实施例1中改性聚丙烯酸成功制备。
试验例2:
医用凝胶的黏度测定
按照常规方法对对比例1~2、实施例1~7制备的医用凝胶进行黏度的测定。
测试结果如图3所示。从图中分析可知,实施例1和实施例4制备的医用凝胶的黏度要高于对比例1和对比例2的,表明采用4-溴巴豆酸或3-氯-2-羟基丙烷磺酸改性CB[7],作为交联剂应用于改性聚丙烯酸的制备工艺中,制得改性聚丙烯酸用于医用凝胶的合成,能够改善医用凝胶的黏度。实施例5的效果与实施例1相当,实施例6的效果与对比例1相当,实施例7的效果与对比例2相当,表明在医用凝胶中加入丁香酚衍生物对凝胶黏度不产生消极影响。
试验例3:
水蒸气透过性实验
测试方法依据YY/T 0471.2-2004规定的标准进行。
对对比例1~2、实施例1~7制备硫酸镁湿敷贴进行上述测试,结果如图4所示。从图中分析可知,实施例1和实施例4制备的硫酸镁湿敷贴的水蒸气透过性要高于对比例1和对比例2的,表明采用4-溴巴豆酸或3-氯-2-羟基丙烷磺酸改性CB[7],作为交联剂应用于改性聚丙烯酸的制备工艺中,制得改性聚丙烯酸用于医用凝胶的合成,获得硫酸镁湿敷贴,能够有效增加硫酸镁湿敷贴的水蒸气透气性能。实施例5的效果稍好于实施例1的,实施例6的效果好于对比例1的,实施例7的效果好于对比例2的,表明在医用凝胶中加入丁香酚衍生物,能够对水凝胶层的结构产生有益的影响,进而一定程度上改善了硫酸镁湿敷贴的透气性能。
试验例4:
湿敷贴样品技术指标测定
测定对比例1~2、实施例1~7制备的硫酸镁湿敷贴的技术指标,结果如表1所示:
表1 技术指标测试结果
样品 | 24h吸水量(g/m2) | 洗水后完整性(%) |
对比例1 | 5630 | 76 |
对比例2 | 6743 | 82 |
实施例1 | 8104 | 94 |
实施例2 | 8202 | 95 |
实施例3 | 8158 | 93 |
实施例4 | 8194 | 94 |
实施例5 | 8129 | 95 |
实施例6 | 5705 | 75 |
实施例7 | 6797 | 82 |
从表1中的数据分析可知,实施例1和实施例4制备的硫酸镁湿敷贴的24h吸水量以及水洗后完整性要好于对比例1和对比例2的,表明采用4-溴巴豆酸或3-氯-2-羟基丙烷磺酸改性CB[7],作为交联剂应用于改性聚丙烯酸的制备工艺中,制得改性聚丙烯酸用于医用凝胶的合成,获得硫酸镁湿敷贴,能够有效增加硫酸镁湿敷贴的吸收容量,改善硫酸镁湿敷贴的溶胀性能,使其能够有效吸收创面的渗出液,更有利于创口的恢复。实施例5的效果与实施例1相当,实施例6的效果与对比例1相当,实施例7的效果与对比例2相当,表明在医用凝胶中加入丁香酚衍生物对硫酸镁湿敷贴的吸收性能以及溶胀性能不产生消极影响。
试验例5:
抑菌活性测定
样品处理:取丁香酚及其丁香酚衍生物(实施例5制备的)5mg,加入丙酮2mL溶解得到样品液。
抑菌测定:取常规滤纸裁剪成直径为6mm的圆片,160℃灭菌2h后浸渍于上述样品液中,然后将菌悬液均匀涂抹于PDA培养基上,并将上述浸渍过的滤纸平放于培养基表面。实验设定无菌水、丙酮做对照,37℃条件下培养24h后观察并测定抑菌圈的大小。
实验结果分析
测试结果如表2所示:
表2 抑菌性能测试结果
样品 | 大肠杆菌抑菌圈直径(cm) | 金黄色葡萄球菌抑菌圈直径(cm) |
丁香酚 | 3.74 | 3.63 |
丁香酚衍生物 | 5.68 | 5.89 |
丙酮 | - | - |
从表2中的数据分析可知,本发明实施例5制备的丁香酚衍生物对大肠杆菌以及金黄色葡萄球菌的抑菌圈直径明显大于丁香酚的,表明制备的丁香酚衍生物表现出更高的生物活性,其抑菌性能得到明显的提升。
镇痛作用测定
实验选取健康昆明小鼠30只,雌雄各半,18~22g;随机分为3组,每组10只(雌雄各半),包括空白对照组、丁香酚组以及丁香酚衍生物组,剔除小鼠腹部毛,将各组药物分别均匀涂覆其上,1次/d,连续涂覆3d;其中,空白对照组给予适量生理盐水,丁香酚组以及丁香酚衍生物组给予5mg/cm2。末次给药40min后,每只小鼠腹腔注射0.3mL 0.6%的醋酸溶液,记录30min内小鼠的扭体次数(扭体判定标准:以腹部内凹、四肢伸展、臀部太高为扭体反应),并按照下列式子计算扭体抑制率:
抑制率%=(空白对照组扭体次数-实验组扭体次数)/空白对照组扭体次数×100%
实验结果分析
测试结果如表3所示:
表3 抑菌性能测试结果
样品组 | 抑制率(%) |
丁香酚 | 42.8 |
丁香酚衍生物 | 54.6 |
从表3中的数据分析可知,本发明实施例5制备的丁香酚衍生物对小鼠扭体次数的抑制率明显高于丁香酚的,表明制备的丁香酚衍生物表现出更高的生物活性,其镇痛作用得到明显的增强。
上述实施例中的常规技术为本领域技术人员所知晓的现有技术,故在此不再详细赘述。
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应以所述权利要求的保护范围为准。
Claims (10)
1.一种改性聚丙烯酸,包括:聚丙烯酸网络结构和穿插附着于所述聚丙烯网络结构内部的网状结构;所述网状结构包括改性葫芦[n]脲;所述改性葫芦[n]脲包括4-溴巴豆酸或3-氯-2-羟基丙烷磺酸化学修饰的葫芦[n]脲。
2.根据权利要求1所述的改性聚丙烯酸,其特征在于:所述改性葫芦[n]脲中,n=5、6或7。
3.根据权利要求1所述的改性聚丙烯酸,其特征在于:所述改性聚丙烯酸的分子量为5万~10万。
4.权利要求1所述的改性聚丙烯酸在制备医用凝胶中的用途。
5.一种医用凝胶,包括:权利要求1所述的改性聚丙烯酸。
6.根据权利要求5所述的医用凝胶,其特征在于:所述医用凝胶原料包括,按重量份计,12~16份甘油,3~6份改性聚丙烯酸,0.2~0.4份尼泊金乙酯,0.01~0.05份高岭土,0.1~0.15份甘羟铝,0.06~0.15份桉叶油,50~60份纯净水,15~26份硫酸镁,1~3份聚乙烯吡咯烷酮,0.2~0.3份酒石酸,0.04~0.08份乙二胺四乙酸二钠。
7.一种硫酸镁湿敷贴,包括防粘层、权利要求5所述的医用凝胶形成的水凝胶层和背衬层;所述水凝胶层位于防粘层与背衬层之间。
8.根据权利要求7所述的硫酸镁湿敷贴,其特征在于:所述水凝胶层的厚度为0.1~4mm。
9.根据权利要求7所述的硫酸镁湿敷贴,其特征在于:所述防粘层包括聚乙烯薄膜。
10.权利要求5所述的医用凝胶在制备硫酸镁湿敷贴中的用途。
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