CN110367249B - 一种具有逐级缓释功能的可降解载药膜材料及其制备方法和应用 - Google Patents
一种具有逐级缓释功能的可降解载药膜材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开的一种具有逐级缓释功能的可降解载药膜材料及其制备方法和应用,属于材料制备技术领域。将带有相反电荷的天然高分子与原药通过复凝聚方法得到载药微胶囊,并且微胶囊表面具有大小均匀的微孔,为药物初始释放提供了通道;然后将载药微胶囊分散在可生物降解的脂肪族聚酯中,通过界面化学键作用使微胶囊固定在聚酯分子中形成可生物降解材料。药物释放时,首先,药物可通过扩散作用从微胶囊微孔释放至脂肪族聚酯膜内,达到第一层释放;释放至膜内的药物会随着聚酯膜材料的降解达到第二层缓慢释放,一方面对作物起到高效缓释作用,另一方面加快了脂肪族聚酯的降解速度,减少了环境污染,且该方法工艺简单、原料易得,能够批量生产。
Description
技术领域
本发明属于材料制备技术领域,具体涉及一种具有逐级缓释功能的可降解载药膜材料及其制备方法和应用。
背景技术
作为一个农业水平发达的国家,我国的地膜和农药的生产和用量是巨大的,随着传统聚乙烯地膜覆盖栽培技术的推广和应用,残留地膜不仅污染土壤、妨碍耕作,还会造成土壤结构破坏。农药防治是控制病虫害的有效手段之一,但农药使用中的流失率可达到50%~60%,降低了农药杀灭病虫害的作用效率,且传统农药不能避免日晒、风吹、雨淋等客观因素造成药物的分解和流失易对环境造成严重污染。
近年来,关于材料降解和药物缓释的相关研究较多,大量研究者主要着重于地膜的生物降解,减少普通地膜带来的白色污染等问题。未考虑到地膜功能性的单一以及膜下虫菌、杂草等问题会给下一茬作物的产量、质量带来严重威胁。可生物降解聚合物作为绿色材料引起人们极大的兴趣,因其具有良好的生物相容性和可生物降解性,可应用于生物医疗、食品包装、医药和农业等多种领域。此外,脂肪族聚酯拥有较长的贮存和使用期内保持比较好的稳定性能并且在自然条件下缓慢降解,降解产物为低分子的酸,能够促进植物生长。
天然高分子具有来源广泛、廉价易得、降解时间短等特点,其可作为有效的药物递送载体,用于受控和靶向释放,对缓/控释农药的包膜具有重要的意义。但由于微胶囊极易吸水溶胀且溶胀后强度和模量较低等缺点,使其缓释要求有所限制。但传统的包膜材料制备包膜过程比较复杂,包膜率还不够高,持效期还待提高。
发明内容
为了解决上述问题,本发明的目的在于提供一种具有逐级缓释功能的可降解载药膜材料及其制备方法和应用,原料易得、制备工艺简单,膜中所载药物能够随膜的降解逐级缓释,减少了环境的污染。
本发明是通过以下技术方案来实现:
本发明公开了具有逐级缓释功能的可降解载药膜材料的制备方法,分为以下步骤:
步骤1:称量取料液比为(0.1~10)g:(1~100)mL的农药原药和氯仿,混合,经超声处理后制得芯材溶液待用;
步骤2:将蛋白质类天然高分子和带有负电荷的多糖类天然高分子分别放入水中,在20~60℃下搅拌至完全溶解,得到两种壁材溶液待用;蛋白质类天然高分子和带有负电荷的多糖类天然高分子与水的料液比均为(0.1~10)g:(10~150)mL;
步骤3:将乳化剂、步骤1得到的芯材溶液和步骤2得到的壁材溶液之一按照(2~8):(0.1~1):(0.01~0.05)的体积比混合后搅拌,在20~60℃下乳化5~30min,滴加步骤2得到的另一种壁材溶液,继续搅拌,得到体系A;
步骤4:将体系A的pH调节至3.0~6.0搅拌5~30min,转入2~8℃的冷水浴复凝聚0.5~3h;再将pH调节至7.0~11.0,加入交联剂进行固化6~12h,得到载药微胶囊悬浮溶液;
步骤5:称量取料液比为(1~10)g:(20~200)mL的高分子聚酯和氯仿,混合均匀静置16~30h后滴入表面活性剂,在30~60℃下搅拌分散10~30min,得到体系B;
步骤6:将步骤4得到的载药微胶囊悬浮溶液滴加在体系B中,在20~50℃下搅拌1~4h,冷却至室温后取适量置于模具中,在室温和恒定湿度下干燥,得到具有逐级缓释功能的可降解载药膜材料。
优选地,步骤1中,农药原药为噻嗪酮、毒死蜱、啶虫脒、阿维菌素、辛硫磷和哌虫啶中的一种或多种。
优选地,步骤2中,蛋白质类天然高分子为:明胶、胶原蛋白、酪蛋白和玉米醇溶蛋白中的一种或多种;带有负电荷的多糖类天然高分子为:羧甲基纤维素、阿拉伯、海藻酸钠和卡拉胶中的一种或多种。
优选地,其特征在于,步骤3中,乳化剂为十二烷基苯磺酸钠、苄基酚聚氧乙烯醚、失水山梨醇脂肪酸酯环氧乙烷、聚乙烯醇、失水山梨醇脂肪酸酯和硬脂酸聚氧乙烯酯中的一种或多种。
优选地,步骤2中,搅拌的速度为200~500r/min;步骤3中,将步骤1得到的芯材溶液、乳化剂和步骤2得到的壁材溶液之一进行搅拌的搅拌速度为100~800r/min,搅拌的时间为15~30min;滴加步骤2得到的另一种壁材溶液后搅拌的速度为300r/min搅拌时间为0.5~2h。
优选地,步骤4中,调节pH是采用盐酸、酒石酸、苹果酸、柠檬酸钠、碳酸钠、碳酸钾、磷酸氢二钠、磷酸二氢钠、氢氧化钠、碳酸氢钠、磷酸氢二钾和磷酸二氢钾中的一种或两种组成的混合溶液。
优选地,步骤5中,高分子聚酯为聚乳酸、聚己内酯、聚对苯二甲酸己二酸丁二醇酯、聚碳酸亚丙酯、聚羟基脂肪酸酯、聚丁二酸乙二醇酯、聚乙二醇硬脂酸酯、聚对苯二甲酸丙二醇酯、聚丁二酸丁二醇酯和尼龙中的一种或多种。
优选地,步骤5中,表面活性剂为质量分数为0.03%的聚醚磷酸酯,表面活性剂与氯仿的体积比为1:(2~5),滴加时逐滴滴加,滴加总时间为5~10min。
本发明还公开了采用上述方法所制备的具有逐级缓释功能的可降解载药膜材料。
本发明还公开了上述具有逐级缓释功能的可降解载药膜材料作为地膜、温室覆盖膜的应用。
与现有技术相比,本发明具有以下有益的技术效果:
本发明公开的一种具有逐级缓释功能的可降解载药膜材料的制备方法,首先将带有相反电荷的天然高分子与原药通过复凝聚方法得到载药微胶囊,并且微胶囊表面具有大小均匀的微孔,为药物初始释放提供了通道;然后将载药微胶囊分散在可生物降解的脂肪族聚酯中,通过界面化学键作用使微胶囊固定在聚酯分子中形成可生物降解材料。体系A悬浮液pH的不同,会对微胶囊的成形性和载药量产生影响;若pH过大,体系中正负电荷没有完全中和,影响凝聚物的形成。将芯材溶液与一种壁材溶液先乳化是为了形成水包油状态,然后再加入另外一种壁材溶液,使得两种壁材溶液通过静电作用和氢键作用形成具有微孔的载药微胶囊,并且此时通过搅拌速度控制微孔的大小。脂肪族聚酯溶解后,必须静置足够的时间使得聚酯分子链得到充分的舒展,提高后续微胶囊悬浮液在聚酯溶液中的分散性。置于模具中时需要缓慢控制计量,若量过多,不能在模具中有较好的流动性造成膜材料褶皱粘连的现象。在模具中干燥时,必须通过恒定湿度来调控溶剂挥发时间,防止膜炸裂。药物释放时,首先,药物可通过扩散作用从微胶囊微孔释放至脂肪族聚酯膜内,达到第一层释放;释放至膜内的药物会随着聚酯膜材料的降解达到第二层缓慢释放,一方面对作物起到高效缓释作用,另一方面加快了脂肪族聚酯的降解速度,减少了环境污染,且该方法工艺简单、原料易得,能够批量生产。
进一步地,添加表面活性剂时需要将时间控制在10min内,若时间过长,氯仿容易挥发会影响微胶囊悬浮液的流动性。
本发明公开的采用上述方法制得的具有逐级缓释功能的可降解载药膜材料,具有可降解、逐级释放所载药物的功能。
本发明公开的具有逐级缓释功能的可降解载药膜材料作为地膜、温室覆盖膜应用时,能够搭载各种功能性药物,起到杀菌、防虫、除草的作用,且可生物降解,不会对环境造成破坏。
附图说明
图1为本发明的双层缓释作用原理示意图;
图2为本发明实施例1制得载药微胶囊的SEM图;
图3为本发明实施例1制得载药微胶囊的SEM图放大图;
图4为本发明实施例1、2、3制得的载药微胶囊的缓释效果图;
图5为本发明实施例1制得的具有逐级缓释功能的可降解载药膜材料在3000倍电镜下的SEM图;
图6为本发明实施例2制得的具有逐级缓释功能的可降解载药膜材料在3000倍电镜下的SEM图;
图7为本发明实施例3制得的具有逐级缓释功能的可降解载药膜材料在3000倍电镜下的SEM图;
图8为本发明实施例3制得的具有逐级缓释功能的可降解载药膜材料在5000倍电镜下的SEM图;
图9为本发明实施例1、2、3制得的具有逐级缓释功能的可降解载药膜材料的缓释效果图。
具体实施方式
下面结合附图和具体实施例对本发明做进一步详细描述,所作是对本发明的解释而不是限定:
交联剂可以使用戊二醛、甲醛或转谷氨酰胺酶(TG),用量为体系A的0.1%~1%。
实施例1:
步骤1:称取0.5g阿维菌素溶于10mL氯仿中,在20℃超声处理20min得到芯材溶液待用;
步骤2:称取1g明胶在50℃下,以200r/min的速度进行搅拌,溶于20mL蒸馏水中至完全溶胀得到第一壁材溶液;称取1g阿拉伯胶在50℃下,以200r/min的速度进行搅拌,溶于20mL蒸馏水中至完全溶胀得到第二壁材溶液;
步骤3:将芯材溶液、第一壁材溶液和2mL失水山梨醇脂肪酸酯在30℃下,以600r/min的速度进行乳化20min,然后滴加入第二壁材溶液,在300r/min速度搅拌1.5h,得到体系A;
步骤4:使用盐酸将体系A的pH调节至4.0,以500r/min的速度进行搅拌15min,转入8℃冷水浴中进行复凝聚1h;再使用氢氧化钠将pH调节至9.0,加入0.2mL戊二醛固化8h后,得到载药微胶囊悬浮溶液;
步骤5:称取2g聚丁二酸丁二醇酯(PBS)溶于10mL氯仿溶液混合静置24h,使分子链完全舒展后在10min内滴加30mL质量分数为0.03%的聚醚磷酸酯水溶液,在50℃下搅拌分散30min后得到体系B;
步骤6:将载药微胶囊悬浮溶液滴加在体系B中,在50℃下搅拌1.5h使载药微胶囊悬浮溶液均匀分散在体系B中,然后放入聚四氟乙烯板中,在恒定湿度下室温干燥使其溶剂蒸发后得到具有逐级缓释功能的可降解载药膜材料。
实施例2
步骤1:称取0.5g阿维菌素溶于5mL氯仿中,在20℃超声处理20min得到芯材溶液待用;
步骤2:称取1g明胶在50℃下,以400r/min的速度进行搅拌,溶于50mL蒸馏水中至完全溶胀得到第一壁材溶液;称取1g阿拉伯胶在50℃下,以400r/min的速度进行搅拌,溶于50mL蒸馏水中至完全溶胀得到第二壁材溶液;
步骤3:将芯材溶液、第一壁材溶液和2mL失水山梨醇脂肪酸酯在30℃下,以600r/min的速度进行乳化5min,然后滴加入第二壁材溶液,在300r/min速度搅拌2h,得到体系A;
步骤4:使用盐酸将体系A的pH调节至5.0,以500r/min的速度进行搅拌15min,转入8℃冷水浴中进行复凝聚1h;再使用氢氧化钠将pH调节至9.0,加入0.2mL戊二醛固化8h后,得到载药微胶囊悬浮溶液;
步骤5:称取2g聚丁二酸丁二醇酯(PBS)溶于10mL氯仿溶液混合静置24h,使分子链完全舒展后在5min内滴加30mL质量分数为0.03%的聚醚磷酸酯水溶液,在50℃下搅拌分散30min后得到体系B;
步骤6:将载药微胶囊悬浮溶液滴加在体系B中,在50℃下搅拌4h使载药微胶囊悬浮溶液均匀分散在体系B中,然后放入聚四氟乙烯板中,在恒定湿度下室温干燥使其溶剂蒸发后得到具有逐级缓释功能的可降解载药膜材料。
实施例3
步骤1:称取0.5g阿维菌素溶于20mL氯仿中,在20℃超声处理20min得到芯材溶液待用;
步骤2:称取1g明胶在50℃下,以300r/min的速度进行搅拌,溶于60mL蒸馏水中至完全溶胀得到第一壁材溶液;称取1g阿拉伯胶在50℃下,以300r/min的速度进行搅拌,溶于60mL蒸馏水中至完全溶胀得到第二壁材溶液;
步骤3:将芯材溶液、第一壁材溶液和2mL失水山梨醇脂肪酸酯在30℃下,以600r/min的速度进行乳化30min,然后滴加入第二壁材溶液,在300r/min速度搅拌1h,得到体系A;
步骤4:使用酒石酸将体系A的pH调节至4.5,以500r/min的速度进行搅拌15min,转入8℃冷水浴中进行复凝聚1h;再使用碳酸钠将pH调节至9.0,加入0.2mL戊二醛固化8h后,得到载药微胶囊悬浮溶液;
步骤5:称取2g聚丁二酸丁二醇酯(PBS)溶于10mL氯仿溶液混合静置24h,使分子链完全舒展后在7min内滴加30mL质量分数为0.03%的聚醚磷酸酯水溶液,在50℃下搅拌分散30min后得到体系B;
步骤6:将载药微胶囊悬浮溶液滴加在体系B中,在50℃下搅拌2h使载药微胶囊悬浮溶液均匀分散在体系B中,然后放入聚四氟乙烯板中,在恒定湿度下室温干燥使其溶剂蒸发后得到具有逐级缓释功能的可降解载药膜材料。
实施例4
步骤1:称取1g啶虫脒溶于50mL氯仿中,在20℃超声处理20min得到芯材溶液待用;
步骤2:称取1g胶原蛋白在20℃下,以200r/min的速度进行搅拌,溶于100mL蒸馏水中至完全溶胀得到第一壁材溶液;称取1g海藻酸钠和卡拉胶在30℃下,以100r/min的速度进行搅拌,溶于100mL蒸馏水中至完全溶胀得到第二壁材溶液;
步骤3:将芯材溶液、第一壁材溶液和2mL聚乙烯醇和十二烷基苯磺酸钠,在30℃下,以600r/min的速度进行乳化15min,然后滴加入第二壁材溶液,在300r/min速度搅拌2h,得到体系A;
步骤4:使用醋酸将体系A的pH调节至6.0,以500r/min的速度进行搅拌15min,转入2℃冷水浴中进行复凝聚1h;再使用氢氧化钠将pH调节至9.0,加入0.2mL甲醛固化8h后,得到载药微胶囊悬浮溶液;
步骤5:称取2g聚对苯二甲酸己二酸丁二醇酯(PBAT)溶于20mL氯仿溶液混合静置16h,使分子链完全舒展后在10min内滴加30mL质量分数为0.03%的聚醚磷酸酯水溶液,在30℃下搅拌分散30min后得到体系B;
步骤6:将载药微胶囊悬浮溶液滴加在体系B中,在20℃下以500r/min的速度搅拌4h使载药微胶囊悬浮溶液均匀分散在体系B中,然后放入聚四氟乙烯板中,在恒定湿度下室温干燥使其溶剂蒸发后得到具有逐级缓释功能的可降解载药膜材料。
实施例5
步骤1:称取1g啶虫脒和噻嗪酮溶于50mL氯仿中,在20℃超声处理20min得到芯材溶液待用;
步骤2:称取1g酪蛋白和玉米醇溶蛋白在60℃下,以500r/min的速度进行搅拌,溶于100mL蒸馏水中至完全溶胀得到第一壁材溶液;称取1g卡拉胶在30℃下,以200r/min的速度进行搅拌,溶于100mL蒸馏水中至完全溶胀得到第二壁材溶液;
步骤3:将芯材溶液、第一壁材溶液和2mL聚乙烯醇和、硬脂酸聚氧乙烯酯,在30℃下,以800r/min的速度进行乳化30min,然后滴加入第二壁材溶液,在300r/min速度搅拌0.5h,得到体系A;
步骤4:使用醋酸和柠檬酸将体系A的pH调节至6.0,以500r/min的速度进行搅拌15min,转入2℃冷水浴中进行复凝聚1h;再使用氢氧化钠将pH调节至9.0,加入0.2mL甲醛固化8h后,得到载药微胶囊悬浮溶液;
步骤5:称取2g聚己内酯和聚丁二酸丁二醇酯溶于20mL氯仿溶液混合静置30h,使分子链完全舒展后在10min内滴加30mL质量分数为0.03%的聚醚磷酸酯水溶液,在60℃下搅拌分散10min后得到体系B;
步骤6:将载药微胶囊悬浮溶液滴加在体系B中,在50℃下以500r/min的速度搅拌1h使载药微胶囊悬浮溶液均匀分散在体系B中,然后放入聚四氟乙烯板中,在恒定湿度下室温干燥使其溶剂蒸发后得到具有逐级缓释功能的可降解载药膜材料。
相关性能测试与结果
1)载药微胶囊的形貌结构
由图2可以看出制备得到的载药微胶囊大小均匀,在图2的放大图图3中可以明显看出囊壁表面出现大小均匀的微孔,利于药物从囊孔通过扩散作用释放。
2)载药微胶囊的缓释性能
如图4所示,随着时间的增加,缓释药物阿维菌素被逐渐释放出来,在3个实施例中,实施例2的缓释效率比较高,说明pH为4.5时,复凝聚反应形成的微胶囊囊孔更加紧密,有利于缓释。基本在60h内缓释达到饱和。
3)具有逐级缓释功能的可降解载药膜材料的形貌结构
图5、图6、图7、图8分别为实施例1、2、3制备得到的具有逐级缓释功能的可降解载药膜材料的SEM图,从图5、6、7中可以看出,微胶囊悬浮液都相对均匀的分散在PBS聚酯溶液中,形成表面无孔致密的包膜材料。
在图6、7中可以看出表面较舒展,这是因为实施例2、3中滴加表面活性剂的时间短,有利于防止氯仿的挥发使得微胶囊悬浮液在聚酯溶液中具有更好的流动性。
在图8中,放大5000倍后,可以发现微胶囊始终保持完好形态分散在聚酯中,可以为后续的药物成功进行双层缓释。
4)具有逐级缓释功能的可降解载药膜材料的缓释性能
图9是实施例1、2、3制备得到的具有逐级缓释功能的可降解载药膜材料的药物缓释结果图,主要是通过紫外分光光度法测定阿维菌素在245nm处的吸收波长,从而计算药物释放的含量。由图可知,在1~4天,药物释放相对平缓,这是因为前期脱囊释放的部分药物释放在体系中,5天以后药物释放速率明显加快,这是因为包膜材料部分出现降解,药物随着材料的降解得到一定的缓释,并且在第10天药物总释放量不超过45%,起到了良好的缓释效果。
Claims (5)
1.一种具有逐级缓释功能的可降解载药膜材料的制备方法,其特征在于,包括以下步骤:
步骤1:称量取料液比为(0.1~10)g:(1~100)mL的农药原药和氯仿,混合,经超声处理后制得芯材溶液待用;农药原药为噻嗪酮、毒死蜱、啶虫脒、阿维菌素、辛硫磷和哌虫啶中的一种或多种;
步骤2:将蛋白质类天然高分子和带有负电荷的多糖类天然高分子分别放入水中,在20~60℃下搅拌至完全溶解,得到两种壁材溶液待用;蛋白质类天然高分子和带有负电荷的多糖类天然高分子与水的料液比均为(0.1~10)g:(10~150)mL;搅拌的速度为200~500r/min;蛋白质类天然高分子为:明胶、胶原蛋白、酪蛋白和玉米醇溶蛋白中的一种或多种;带有负电荷的多糖类天然高分子为:羧甲基纤维素、阿拉伯胶、海藻酸钠和卡拉胶中的一种或多种;
步骤3:将乳化剂、步骤1得到的芯材溶液和步骤2得到的壁材溶液之一按照(2~8):(0.1~1):(0.01~0.05)的体积比混合后以100~800r/min的搅拌速度进行搅拌,搅拌的时间为15~30min;在20~60℃下乳化5~30min,滴加步骤2得到的另一种壁材溶液,继续搅拌,以300r/min的搅拌速度进行搅拌,搅拌的时间为0.5~2h,得到体系A;
步骤4:将体系A的pH调节至3.0~6.0搅拌5~30min,转入2~8℃的冷水浴复凝聚0.5~3h;再将pH调节至7.0~11.0,加入交联剂进行固化6~12h,得到载药微胶囊悬浮溶液;
步骤5:称量取料液比为(1~10)g:(20~200)mL的高分子聚酯和氯仿,混合均匀静置16~30h后滴入表面活性剂,在30~60℃下搅拌分散10~30min,得到体系B;表面活性剂为质量分数为0.03%的聚醚磷酸酯,表面活性剂与氯仿的体积比为1:(2~5),滴加时逐滴滴加,滴加总时间为5~10min;高分子聚酯为聚乳酸、聚己内酯、聚对苯二甲酸己二酸丁二醇酯、聚碳酸亚丙酯、聚羟基脂肪酸酯、聚丁二酸乙二醇酯、聚乙二醇硬脂酸酯、聚对苯二甲酸丙二醇酯、聚丁二酸丁二醇酯和尼龙中的一种或多种;
步骤6:将步骤4得到的载药微胶囊悬浮溶液滴加在体系B中,在20~50℃下搅拌1~4h,冷却至室温后取适量置于模具中,在室温和恒定湿度下干燥,得到具有逐级缓释功能的可降解载药膜材料。
2.根据权利要求1所述的具有逐级缓释功能的可降解载药膜材料的制备方法,其特征在于,步骤3中,乳化剂为十二烷基苯磺酸钠、苄基酚聚氧乙烯醚、失水山梨醇脂肪酸酯环氧乙烷、聚乙烯醇、失水山梨醇脂肪酸酯和硬脂酸聚氧乙烯酯中的一种或多种。
3.根据权利要求1所述的具有逐级缓释功能的可降解载药膜材料的制备方法,其特征在于,步骤4中,调节pH是采用盐酸、酒石酸、苹果酸、柠檬酸钠、碳酸钠、碳酸钾、磷酸氢二钠、磷酸二氢钠、氢氧化钠、碳酸氢钠、磷酸氢二钾和磷酸二氢钾中的一种或两种组成的混合溶液。
4.采用权利要求1~3任意一项所述的制备方法制得的具有逐级缓释功能的可降解载药膜材料。
5.权利要求4所述的具有逐级缓释功能的可降解载药膜材料作为地膜、温室覆盖膜的应用。
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