CN113143845A - 一种丙烯酰胺-盐酸普奈洛尔水凝胶及其制备方法 - Google Patents
一种丙烯酰胺-盐酸普奈洛尔水凝胶及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种丙烯酰胺‑盐酸普奈洛尔水凝胶，是由丙烯酰胺水凝胶包裹盐酸普奈洛尔得到的；并提供了其制备方法。该水凝胶易于制备和保存，稳定性好，对盐酸普奈洛尔分子具有良好的缓释效果；本发明的丙烯酰胺‑盐酸普奈洛尔水凝胶具有良好的生物相容性，使得其在缓释药物分子方面有重大的意义。
Description
技术领域
本发明属于医药技术领域，具体涉及一种丙烯酰胺-盐酸普奈洛尔水凝胶及其制备方法。
背景技术
盐酸普奈洛尔，又名心得安，用于治疗多种原因所致的心律失常，心绞痛。亦可用于甲状腺机能亢进症，能迅速控制心动过速、震颤、体温升高等症状，且对高血压有一定疗效。目前，药剂学已经发展进入到了一个新的时代，新型的药物剂型正在朝着稳定储藏、纳米微粒控释缓释方向发展，这样能够更好的控制药物药量、提高药物利用率以及降低药物的毒副作用，既可以做到有效治疗疾病又能够减轻病患的痛苦。因此，药品新剂型研究的重点课题是制备具有药物缓释作用的纳米微球制剂。
水凝胶(hydrogels，HG)是有机体不可或缺的一部分，例如，许多生物的组织和器官都是水凝胶，因为它们具有很高的水合作用，而且三维(3D)微观结构与天然组织非常相似而被广泛关注。由于它们的柔韧性，出色的生物相容性，机械稳定性和对人体生物分子的高渗透性，水凝胶已被用于生物传感、柔性器件等领域，除此以外，水凝胶还可以通过非共价键结合作为药物及分子载体。
紫外可见分光光度法是基于物质分子与电磁辐射作用时，物质内部发生了量子化的能级之间的跃迁，测量由此产生的反射，吸收或散射辐射的波长和强度而进行分析的方法。荧光光谱分析法也是分子发光的一种，是物质吸收光能或者其他辐射能后发出光的过程，大多数情况下，发光波长比吸收波长长，能量低。上述两种光谱分析法具有(a)灵敏度高；(b)取样量少；(c)操作简单；(d)选择性好等特点。目前，已将该技术应用于环境分析、临床检测、食品分析以及生命科学研究等领域。
发明内容
本发明的第一个目的是提供一种丙烯酰胺-盐酸普奈洛尔水凝胶，该水凝胶具有良好的缓释效果。
本发明的第二个目的是提供上述水凝胶的制备方法。
本发明的目的通过以下技术方案来具体实现：
一种丙烯酰胺-盐酸普奈洛尔水凝胶，是由丙烯酰胺水凝胶包裹盐酸普奈洛尔得到的。
上述丙烯酰胺-盐酸普奈洛尔水凝胶的制备方法，所述方法包括如下步骤：
(1)以水为溶剂，分别将盐酸普奈洛尔、丙烯酰胺、甲叉双丙烯酰胺、过硫酸铵加入水中，超声溶解，配制相应的水溶液；
(2)将步骤(1)配制的4种水溶液混合，加入四甲基乙二胺，在70℃下放置，然后冷却至室温，得到含有盐酸普奈洛尔的丙烯酰胺水凝胶。
更进一步的，步骤(1)中，盐酸普奈洛尔浓度为3mg/mL，丙烯酰胺的质量百分比为50％，甲叉双丙烯酰胺的质量百分比为1.3％，过硫酸铵的质量百分比为10％。
更进一步的，步骤(2)中，盐酸普奈洛尔溶液：丙烯酰胺溶液：甲叉双丙烯酰胺溶液：过硫酸铵溶液：四甲基乙二胺的体积比为110：50：50：2：5；
70℃下放置的时间为10min。
本发明的水凝胶的合成方法为，丙烯酰胺作为单体材料，甲叉双丙烯酰胺作为交联剂，过硫酸铵作为加速剂，四甲基乙二胺作为启动剂，加入盐酸普奈洛尔制备而成，该水凝胶可以实现对盐酸普奈洛尔的缓释，随着时间的增加，缓释量呈现逐渐增加的趋势。
本发明具有以下有益效果：
本发明提供的丙烯酰胺-盐酸普奈洛尔水凝胶，易于制备和保存，稳定性好，对盐酸普奈洛尔分子具有良好的缓释效果；本发明的丙烯酰胺-盐酸普奈洛尔水凝胶具有良好的生物相容性，使得其在缓释药物分子方面有重大的意义。
附图说明
图1是药物分子盐酸普奈洛尔(propranolol)，丙烯酰胺水凝胶(HG)及含有盐酸普奈洛尔的丙烯酰胺水凝胶(propranolol HG)的X射线粉末衍射图。
图2是药物分子盐酸普奈洛尔(propranolol)，丙烯酰胺水凝胶(HG)及含有盐酸普奈洛尔的丙烯酰胺水凝胶(propranolol HG)的红外光谱图。
图3是含有盐酸普奈洛尔的丙烯酰胺水凝胶在对盐酸普奈洛尔缓释过程的实时紫外吸收光谱检测图。图中曲线对应的时间由下到上依次是第15min，30min,45min,60min,75min,90min,105min,120min,135min,150min。
图4是含有盐酸普奈洛尔的丙烯酰胺水凝胶在对盐酸普奈洛尔缓释过程的实时荧光光谱检测图。图中曲线对应的时间由下到上依次是第15min，30min,45min,60min,75min,90min,105min,120min,135min,150min。
具体实施方式
以下对本发明的优选实施例进行说明，应当理解，此处所描述的优选实施例仅用于说明和解释本发明，并不用于限定本发明。
实施例1
含有盐酸普奈洛尔的丙烯酰胺水凝胶的制备方法，方法如下：
(1)准确称取60mg的盐酸普奈洛尔Propranolol，移入50mL的烧杯，用移液管移取20g的超纯水于烧杯中，超声至盐酸普奈洛尔溶解。
(2)准确称取10.0g的丙烯酰胺PAM，移入50mL的离心管，移取10g的超纯水于离心管中，超声至溶解。
(3)准确称取0.1268g的甲叉双丙烯酰胺Bis，移入50mL的离心管，移取10g的超纯水于离心管中，超声至溶解。
(4)准确称取1.1112g的过硫酸铵APS，移入50mL的离心管，移取10g的超纯水于离心管中，超声至溶解。
(5)将上述1-4步骤配制的溶液和四甲基乙二胺TEMED，按照Propranolol：PAM：Bis：APS：TEMED＝110：50：50：2：5的体积比混合，搅拌均匀后放入70℃烘箱中反应10min，冷却至室温，得到含有盐酸普奈洛尔的丙烯酰胺水凝胶。
实施例1合成的含有盐酸普奈洛尔的丙烯酰胺水凝胶的X射线粉末衍射如图1所示。
从X射线粉末衍射图可以看到，所制备的含有盐酸普奈洛尔的丙烯酰胺水凝胶的X射线粉末衍射峰位置与单独的盐酸普奈洛尔分子以及丙烯酰胺水凝胶的峰位置重合，在包裹了盐酸普奈洛尔后，复合材料的X射线粉末衍射峰在11-35的角度下峰强度明显增强，说明包裹盐酸普奈洛尔分子后，丙烯酰胺水凝胶的结构并未被破坏，证明了含有盐酸普奈洛尔的丙烯酰胺水凝胶成功合成。
实施例1合成的含有盐酸普奈洛尔的丙烯酰胺水凝胶的红外光谱如图2所示。
从红外光谱图可以看到，在所制备的含有盐酸普奈洛尔的丙烯酰胺水凝胶的红外光谱与单独的盐酸普奈洛尔分子以及丙烯酰胺水凝胶的峰位置重合，在包裹了盐酸普奈洛尔后，复合材料的红外光谱峰在1750-800nm处的峰强度明显增强，说明包裹盐酸普奈洛尔分子后，丙烯酰胺水凝胶的结构并未被破坏，证明了含有盐酸普奈洛尔的丙烯酰胺水凝胶成功合成。
实施例2
对药物分子盐酸普奈洛尔缓释过程的实时检测。按照实施例1的方法制备丙烯酰胺-盐酸普奈洛尔水凝胶，然后放入500mL蒸馏水中，分别在第15min，30min,45min,60min,75min,90min,105min,120min,135min,150min时取一次上清液作为待测溶液。具体方法如下：
(1)检测待测样品溶液的紫外吸收强度
样品溶液：配置一系列不同浓度量级的(10-7mol/L、5×10-7M、10-6mol/L、5×10- 6mol/L、10-5mol/L、5×10-5mol/L、10-4mol/L、5×10-4mol/L、10-3mol/L、5×10-3mol/L、10- 2mol/L)的盐酸普奈洛尔标准溶液待用。
取2mL盐酸普奈洛尔标准溶液于两面透光的石英比色皿中，通过检测盐酸普奈洛尔溶液在290nm处的紫外吸收强度，绘制盐酸普奈洛尔溶液的标准曲线。
取实施例2中的上清液，分别进行紫外光谱的定量测定，所测的所有吸光度均在标准曲线上，即按实施例2中每15min间隔的取样顺序进行光谱测量，得到图3，可以看出，随着缓释时间的增加，290nm处的吸光度呈现逐渐增加的趋势，证明丙烯酰胺水凝胶可以实现对药物分子盐酸普奈洛尔的缓释。
2)检测待测样品溶液的荧光吸收强度
荧光光谱仪的狭缝宽度设定为10nm，设置激发光波长为290nm，检测352nm波长处的发射峰荧光强度。取实施例2中的上清液，分别进行荧光光谱的测定，即按实施例2中每15min间隔的取样顺序进行光谱测量，得到图4，可以看出随着缓释时间的增加，352nm处的荧光强度呈现逐渐增加的趋势，进一步证明丙烯酰胺水凝胶可以实现对药物分子盐酸普奈洛尔的缓释。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (4)
1.一种丙烯酰胺-盐酸普奈洛尔水凝胶，其特征在于，是由丙烯酰胺水凝胶包裹盐酸普奈洛尔得到的。
2.权利要求1所述的丙烯酰胺-盐酸普奈洛尔水凝胶的制备方法，其特征在于，所述方法包括如下步骤：
(1)以水为溶剂，分别将盐酸普奈洛尔、丙烯酰胺、甲叉双丙烯酰胺、过硫酸铵加入水中，超声溶解，配制相应的水溶液；
(2)将步骤(1)配制的4种水溶液混合，加入四甲基乙二胺，在70℃下放置，然后冷却至室温，得到含有盐酸普奈洛尔的丙烯酰胺水凝胶。
3.根据权利要求2所述的丙烯酰胺-盐酸普奈洛尔水凝胶的制备方法，其特征在于，步骤(1)中，盐酸普奈洛尔浓度为3mg/mL，丙烯酰胺的质量百分比为50％，甲叉双丙烯酰胺的质量百分比为1.3％，过硫酸铵的质量百分比为10％。
4.根据权利要求2所述的丙烯酰胺-盐酸普奈洛尔水凝胶的制备方法，其特征在于，步骤(2)中，盐酸普奈洛尔溶液：丙烯酰胺溶液：甲叉双丙烯酰胺溶液：过硫酸铵溶液：四甲基乙二胺的体积比为110：50：50：2：5；
70℃下放置的时间为10min。
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