CN115212860A - 羧基化四氧化三铁@碳磁性微球及其制备方法和应用 - Google Patents
羧基化四氧化三铁@碳磁性微球及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及一种羧基化四氧化三铁@碳磁性微球及其制备方法和应用,属于磁性微球技术领域。本发明所述的制备方法,包括以下步骤,(1)将三价铁盐、醋酸钠和稳定剂分散于乙二醇,180℃‑220℃反应6h‑48h,经分离、洗涤、酸处理得到球状四氧化三铁;(2)将球状四氧化三铁分散于碳源和羧基化试剂的混合溶液,160℃‑200℃反应4h‑12h,经分离、洗涤、干燥,得到羧基化四氧化三铁@碳磁性微球。本发明所述的磁性微球采用的Fe3O4微粒具有超顺磁性,活化后的生物质碳含有丰富的羧基,将两者结合在一起后,使得羧基化Fe3O4@C磁性微球表面含有丰富的‑COOH官能团和顺磁性等特点。
Description
技术领域
本发明属于磁性微球技术领域,尤其涉及一种羧基化四氧化三铁@碳磁性微球及其制备方法和应用。
背景技术
免疫层析技术是20世纪末发展起来的结合免疫技术和色谱层析技术的一种分析方法,该方法具有特异性、操作简单、快速等特点,广泛应用于临床诊断、环境监测、食品安全等重要领域。传统免疫层析技术以胶体金为标记物,通过条带显色对目标物定性检测或半定量分析。该方法虽然简单快速,但灵敏度较差,难以准确定量。
碳纳米材料自20世纪90年代年发现以来就引发研究人的广泛关注,主要是因为它在物理、化学、电学领域所显示出的优良性质。超顺磁材料只有在外加磁场条件下才显示出磁性,因此可以通过磁场进行分离,极大的提高分离速度。超顺磁碳纳米复合材料多用于污水治理,碳纳米材料由于齐其疏松多孔的结构,很容易吸附重金属离子和染料,磁性使其可以快速分离很反复利用。现有的超顺磁碳纳米复合材料表面缺少羧基官能团,限制了其在免疫层析方面的应用。
发明内容
为此,本发明所要解决的技术问题在于克服现有技术中用于免疫层析技术的标记物,灵敏度较差,难以准确定量等问题。
为解决上述技术问题,本发明提供了一种羧基化四氧化三铁@碳磁性微球及其制备方法和应用。
本发明的第一个目的是提供一种所述的羧基化四氧化三铁@碳磁性微球的制备方法,包括以下步骤,
(1)将三价铁盐、醋酸钠和稳定剂分散于乙二醇,180℃-220℃反应6h-48h,经分离、洗涤、酸处理得到球状四氧化三铁;
(2)将步骤(1)所述的球状四氧化三铁分散于碳源和羧基化试剂的混合溶液,160℃-200℃反应4h-12h,经分离、洗涤、干燥,得到所述羧基化四氧化三铁@碳磁性微球。
在本发明的一个实施例中,在步骤(1)中,所述三价铁盐为硫酸铁、硝酸铁和氯化铁中的一种或多种。
在本发明的一个实施例中,在步骤(1)中,所述稳定剂为聚丙烯酸和/或聚甲基丙烯酸。
在本发明的一个实施例中,在步骤(1)中,所述稳定剂的分子量为1000-5000。
在本发明的一个实施例中,在步骤(1)中,所述三价铁盐的浓度为0.01M-0.5M;醋酸钠的浓度为0.05M-2M;稳定剂的浓度为0.01-10wt%。
在本发明的一个实施例中,在步骤(1)中,所述酸处理采用的酸液为硝酸、盐酸和硫酸中的一种或多种。
在本发明的一个实施例中,在步骤(1)中,所述酸液的浓度为0.05M-1M。
在本发明的一个实施例中,在步骤(1)中,所述酸处理是将球状四氧化三铁分散在酸液中超声处理5min-15min,经磁分离、洗涤,烘干。
在本发明的一个实施例中,在步骤(2)中,所述碳源为蔗糖、果糖和葡萄糖中的一种或多种。
在本发明的一个实施例中,在步骤(2)中,所述羧基化试剂为甲基丙烯酸和/或丙烯酸,提供羧基基团。
在本发明的一个实施例中,在步骤(2)中,所述球状四氧化三铁的浓度为0.05-10wt%;碳源的浓度为0.1M-2M;羧基化试剂的浓度为0.01-20wt%。
本发明的第二个目的是提供一种羧基化四氧化三铁@碳磁性微球,包括内核四氧化三铁、外壳碳和设置于所述碳表面的羧基。
本发明的第三个目的是提供一种所述的羧基化四氧化三铁@碳磁性微球在免疫层析中的应用。
本发明的技术方案相比现有技术具有以下优点:
(1)本发明所述的四氧化三铁@碳磁性微球采用的碳纳米材料具有较大的比表面积、良好的电学和光学性质使其可以作为生物探针应用到免疫层领域。碳纳米材料具有黑色的物理属性,在检测线位置的富集后会形成黑色条带和白色的层析膜形成鲜明的对比,极大提高检测检测灵敏度。在免疫层析的应用上,碳纳米材料显示出比胶体金更高的普适性。
(2)本发明所述的四氧化三铁@碳磁性微球采用的Fe3O4微粒具有超顺磁性,活化后的生物质碳含有丰富的羧基,将两者结合在一起后,可得到羧基化的Fe3O4@C磁性微球,羧基化Fe3O4@C磁性微球表面含有丰富的-COOH官能团和顺磁性等特点。
(3)本发明所述的四氧化三铁@碳磁性微球碳壳上的羧基可以通过N-羟基丁二酰亚胺(NHS)和1-乙基-(3-二甲基氨基丙基)碳酰二亚胺(EDC)与特定物质进行结合,内核的Fe3O4微粒使得材料具有顺磁性,再外加磁场下快速分离,羧基化Fe3O4@C磁性微球在免疫层析方向具有重大的应用前景。
附图说明
为了使本发明的内容更容易被清楚地理解,下面根据本发明的具体实施例并结合附图,对本发明作进一步详细的说明,其中:
图1为本发明实施例1的羧基化Fe3O4@C磁性微球的SEM图。
图2为本发明实施例1的羧基化Fe3O4@C磁性微球的实物图;其中,(a)磁分离前;(b)磁分离后。
图3为本发明应用例的免疫层析试纸条应用图。
具体实施方式
下面结合附图和具体实施例对本发明作进一步说明,以使本领域的技术人员可以更好地理解本发明并能予以实施,但所举实施例不作为对本发明的限定。
实施例1
一种羧基化Fe3O4@C磁性微球及其制备方法,具体包括以下步骤:
(1)称取2.7g六水合氯化铁、7.2g无水醋酸钠和2.0g聚丙烯酸(2000)溶解于80mL乙二醇溶液中,搅拌30min后转移至100mL反应釜中,200℃反应12h。自然降温冷却后取出样品,磁分离,用乙醇和水分别洗涤3次得到Fe3O4微球。
(2)将制备的Fe3O4微球分散于100mL 0.1M的硝酸溶液中,超声5min,蒸馏水洗涤3次后,烘干备用。
(3)将0.5g酸处理后的Fe3O4微球和6.0g葡萄糖和1.2g丙烯酸在80mL水中超声分散30min。然后转移至100mL反应釜中,180℃反应6h。自然降温冷却后取出样品,分离产物中的磁性物质,用蒸馏水洗涤3次,干燥,得到羧基化Fe3O4@C磁性微球。
图1所示为羧基化Fe3O4@C磁性微球的SEM图,羧基化Fe3O4@C磁性微球的形貌为球形,粒径为180-400nm左右。
图2所示为羧基化Fe3O4@C磁性微球的实物图,从图2(a)可以看出其在水中的分散性良好,图2(b)显示的是5min磁分离效果,可以通过磁分离,快速分离。
实施例2
一种羧基化Fe3O4@C磁性微球及其制备方法,具体包括以下步骤:
(1)称取2.7g六水合氯化铁、7.2g无水醋酸钠和1.0g聚甲基丙烯酸(2000)溶解于80mL乙二醇溶液中,搅拌30min后转移至100mL反应釜中,200℃反应12h。自然降温冷却后取出样品,磁分离,用乙醇和水分别洗涤3次得到Fe3O4微球。
(2)将制备的Fe3O4微球分散于100mL 0.1M的硝酸溶液中,超声5min,蒸馏水洗涤3次后,烘干备用。
(3)将0.5g酸处理后的Fe3O4微球和6.0g葡萄糖和0.6g丙烯酸在80mL水中超声分散30min。然后转移至100mL反应釜中,180℃反应6h。自然降温冷却后取出样品,分离产物中的磁性物质,用蒸馏水洗涤3次,干燥,得到羧基化Fe3O4@C磁性微球。
实施例3
一种羧基化Fe3O4@C磁性微球及其制备方法,具体包括以下步骤:
(1)称取4.8g硫酸铁、11.8g无水醋酸钠和1.0g聚甲基丙烯酸(2000)溶解于80mL聚乙二醇溶液中,搅拌30min后转移至100mL反应釜中,200℃反应16h。自然降温冷却后取出样品,磁分离,用乙醇和水分别洗涤3次得到Fe3O4微球。
(2)将制备的Fe3O4微球分散于100mL 0.1M的盐酸溶液中,超声5min,蒸馏水洗涤3次后,烘干备用。
(3)将0.5g酸处理后的Fe3O4微球和6.0g蔗糖和0.6g丙烯酸在80mL水中超声分散30min。然后转移至100mL反应釜中,180℃反应6h。自然降温冷却后取出样品,分离产物中的磁性物质,用蒸馏水洗涤3次,干燥,得到羧基化Fe3O4@C磁性微球。
实施例4
一种羧基化Fe3O4@C磁性微球及其制备方法,具体包括以下步骤:
(1)称取5.8g硝酸铁、19.6g无水醋酸钠和1.0g聚丙烯酸(2000)溶解于80mL聚乙二醇溶液中,搅拌30min后转移至100mL反应釜中,200℃反应8h。自然降温冷却后取出样品,磁分离,用乙醇和水分别洗涤3次得到Fe3O4微球。
(2)将制备的Fe3O4微球分散于100mL 0.1M的硝酸溶液中,超声5min,蒸馏水洗涤3次后,烘干备用。
(3)将0.1g酸处理后的Fe3O4微球和3.0g果糖和0.5g甲基丙烯酸在80mL水中超声分散30min。然后转移至100mL反应釜中,200℃反应8h。自然降温冷却后取出样品,分离产物中的磁性物质,用蒸馏水洗涤3次,干燥,得到具有羧基化Fe3O4@C磁性微球。
应用例
采用实施例1制备的羧基化Fe3O4@C磁性微球进行免疫层析方向的应用分析:
(1)偶联抗体:羧基化Fe3O4@C磁性微球(0.5mg)用MEST(10mM,pH为6.0,0.05%Tween-20)清洗3次,加入新鲜配制的50μL EDC(5mg/mL)和50μLNHS(5mg/mL)反应30min活化磁性微球表面的羧基基团,磁分离去除未反应的EDC和NHS,加入250μLMES缓冲液(100μg山羊抗小鼠抗体GAM lgG)悬浮磁性微球,置于恒温振荡器中混匀反应3h;磁分离去除未偶联的抗体,然后加入PBST(含1%BSA)于37℃反应30min,封闭磁珠表面的自由基团;最后加入250μLPBST缓冲液(pH为7.4、含0.02%NaN3及0.5%BSA)悬浮磁珠,4℃冰箱中保存备用。
(2)免疫层析应用:免疫层析试纸条由PVC底板、样品垫、结合垫、硝化纤维膜和吸水纸构建而成;分别以PBS溶液和含0.05g/mL原肌球蛋白Tm的PBS溶液喷点在硝化纤维膜上作为检测线T线,2mg/mL羊抗鼠lgG喷点在硝化纤维膜形成控制线C线对磁珠表面修饰的抗体活性进行了评价。T线和C线的喷点量为1.0μL/cm。检测时先取5μL单抗修饰磁珠2mg/mL点于试纸条的结合垫处,然后在样品垫处加入100μLPBS溶液或者含纯化后的过敏原肌球蛋白Tm的PBS待测溶液,室温层析20min,如图3所示,肉眼观察,T线明显,羧基化Fe3O4@C磁性微球可以很好的应用在免疫层析领域。
显然,上述实施例仅仅是为清楚地说明所作的举例,并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引申出的显而易见的变化或变动仍处于本发明创造的保护范围之中。
Claims (10)
1.一种羧基化四氧化三铁@碳磁性微球的制备方法,其特征在于,包括以下步骤,
(1)将三价铁盐、醋酸钠和稳定剂分散于乙二醇,180℃-220℃反应6h-48h,经分离、洗涤、酸处理得到球状四氧化三铁;
(2)将步骤(1)所述的球状四氧化三铁分散于碳源和羧基化试剂的混合溶液,160℃-200℃反应4h-12h,经分离、洗涤、干燥,得到所述羧基化四氧化三铁@碳磁性微球。
2.根据权利要求1所述的羧基化四氧化三铁@碳磁性微球的制备方法,其特征在于,在步骤(1)中,所述三价铁盐为硫酸铁、硝酸铁和氯化铁中的一种或多种。
3.根据权利要求1所述的羧基化四氧化三铁@碳磁性微球的制备方法,其特征在于,在步骤(1)中,所述稳定剂为聚丙烯酸和/或聚甲基丙烯酸。
4.根据权利要求3所述的羧基化四氧化三铁@碳磁性微球的制备方法,其特征在于,在步骤(1)中,所述稳定剂的分子量为1000-5000。
5.根据权利要求1所述的羧基化四氧化三铁@碳磁性微球的制备方法,其特征在于,在步骤(1)中,所述三价铁盐的浓度为0.01M-0.5M;醋酸钠的浓度为0.05M-2M;稳定剂的浓度为0.01-10wt%。
6.根据权利要求1所述的羧基化四氧化三铁@碳磁性微球的制备方法,其特征在于,在步骤(2)中,所述碳源为蔗糖、果糖和葡萄糖中的一种或多种。
7.根据权利要求1所述的羧基化四氧化三铁@碳磁性微球的制备方法,其特征在于,在步骤(2)中,所述羧基化试剂为甲基丙烯酸和/或丙烯酸。
8.根据权利要求1所述的羧基化四氧化三铁@碳磁性微球的制备方法,其特征在于,在步骤(2)中,所述球状四氧化三铁的浓度为0.05-10wt%;碳源的浓度为0.1M-2M;羧基化试剂的浓度为0.01-20wt%。
9.权利要求1-8任一项所述的方法制备的羧基化四氧化三铁@碳磁性微球,其特征在于,包括内核四氧化三铁、外壳碳和设置于所述碳表面的羧基。
10.权利要求9所述的羧基化四氧化三铁@碳磁性微球在免疫层析中的应用。
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