CN114106824A - 一种基于十字花科植物的碳点的制备方法及应用 - Google Patents
一种基于十字花科植物的碳点的制备方法及应用 Download PDFInfo
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Abstract
本发明提供了一种基于十字花科植物的碳点的制备方法及应用,是将农业或生活中废弃的十字花科作物作为碳源,仅以水作为溶剂,在高温高压反应釜中进行液化,后行抽滤,收集抽滤液透析之后冻干,得到青色荧光碳点(CC‑CDs)。本发明的方法操作简单,不需要除水以外的任何化学试剂,可以快速处理大量的农业或生活中废弃的大白菜,实现了生物质废弃物的回收利用,且无毒无害符合环保理念。本发明的方法制备得到的碳点可以有效地用于水相中Fe3+含量的检测和细胞成像。
Description
技术领域
本发明属于发光纳米材料技术领域,具体涉及一种基于十字花科植物的碳点的制备方法及应用。
背景技术
碳点(Carbon dots)是一种直径小于10纳米的准球形荧光颗粒。近十年来,碳点以其独特的光学性质、良好的生物相容性、良好的水溶性等优点在相关领域引起了广泛关注。许多有机小分子、高分子聚合和天然生物质均被作为前体,通过各种方法制备成碳点。如能使用更便宜、易得的材料如各种农业及生产加工中产生的生物质废物,开发一种简单、高效、绿色的合成路线,大规模生产强荧光碳点,并且可以在实际应用中使用,是十分重要的,必将具有广泛的应用价值。而天然生物质资源富含碳水化合物、氨基酸、蛋白质等生物分子,可以为碳点丰富的元素掺杂和大量的官能团,是合成碳点的理想绿色前体。许多研究利用天然生物质资源合成了碳点,如橙汁、柚皮、大蒜、玉米秸秆等,并应用于生物传感、抗氧化、生物成像等领域。
铁离子(Fe3+)是人体和其他生物系统中必不可少的微量元素之一。它在代谢、氧运输、酶反应等生物过程中起着重要作用。铁缺乏和过量会直接或间接引起严重的疾病。例如,缺铁会引起缺铁性贫血、肌无力等症状,另外帕金森症、阿尔茨海默症、2型糖尿病等病症也与铁过量密切相关。因此,需要一种检测Fe3+含量的有效方法。目前,检测Fe3+离子的方法主要有电感耦合等离子体质谱法、原子吸收光谱法、荧光法和电化学法。但是,上述方法存在需要昂贵而复杂的设备,以及需要耗时费力的样品预处理的问题。
发明内容
本发明的目的就在于提供一种基于十字花科植物的碳点的制备方法及应用,以解决以十字花科植物简单、高效、绿色大规模生产碳点的问题。本方法以生物质废弃物为原料,仅以水作为溶剂,原料成本低且工艺绿色环保,制得碳量子点有着优异的光学性能,可以基于荧光淬灭原理实现Fe3+的灵敏检测,成本低、速度快、准确度更高。
本发明的目的是通过以下技术方案实现的:
一种基于十字花科植物的碳点的制备方法,包括以下步骤:
A、将大白菜叶用碎菜机绞碎并与水混合,其中大白菜与水的质量比为50-200:100-400;
B、将上述混合液放入高温高压反应釜中进行加热,加热温度为140~220℃,达到设定温度后恒温时间为0.1-1h,后时停止加热并自然冷却至室温;
C、取出反应釜中的物料进行抽滤,收集滤液,对超纯水透析12-48h,取透析袋中的液体冻干后得到固态青色荧光碳点(CC-CDs),并置于4℃冰箱中备用。
进一步地,所述大白菜与水的质量比为100:400。
进一步地,所述加热温度为200℃,恒温时间为0.5h。
进一步地,所述透析袋使用1kDa,透析时间为48h。
一种基于十字花科植物的碳点的应用,其特征在于:所制青色荧光大白菜碳点用于检测水相中微量Fe3+离子浓度及活细胞多色成像。
与现有技术相比,本发明的有益效果在于:
1、本发明以农业生产或生活中废弃的大白菜作为原料,整个过程只以水作为溶剂,不使用任何其他有机试剂,既实现了废物利用又绿色环保;
2、制得的碳点的量子产率较高,以硫酸奎宁(量子产率54%)为参照,所得碳点的相对量子产率达到13.6%;
3、制得的碳点在0.0-100.0μM范围内与Fe3+呈良好的线性关系,检测限低至0.42μM,且对Fe3+具有高选择性和高灵敏性,可用于水体系的检测;所制备的碳点有良好的pH耐受性、耐盐性和光稳定性。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对实施例中所需要使用的附图作简单地介绍,应当理解,以下附图仅示出了本发明的某些实施例,因此不应被看作是对范围的限定,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他相关的附图。
图1为实施例1-5制备的碳点的荧光光谱图;
图2为实施例4所制备碳点的紫外吸收光谱及荧光激发和发射光谱图;
图3为实施例4所制备碳点的激发依赖性荧光谱图;
图4为实施例4所制备碳点的X射线光电子能谱;
图5为实施例4所制备碳点稳定性表征荧光强度柱状图,其中图5a为不同NaCl浓度下碳点的荧光强度,图5b为不同的pH条件下碳点的荧光强度,图5c为12h内自然光照下碳点的荧光强度,图5d为120min内365nm紫外光照射下碳点的荧光强度;
图6为实施例4所制备碳点加入不同浓度Fe3+荧光谱图(图6a)和线性关系图(图6b);
图7为实施例4所制备碳点孵育HeLa细胞12h后的激光共聚焦成像,其中图7a为明场,图7b、图7c、图7d分别为在405nm、488nm和543nm激光激发下的成像图。
具体实施方式
下面结合具体实施案例对本发明作进一步的说明,本实施案例在以本发明技术为前提下进行实施,给出了详细的实施方式,但本发明的保护范围不限于以下的实施例。
实施例1
1、将大白菜叶用碎菜机绞碎并与水混合,其中大白菜与水的质量比为100:200。
2、将上述混合液放入高温高压反应釜中进行加热,加热温度为140℃,达到设定温度后恒温时间为0.5h,后时停止加热并自然冷却至室温。
3、取出反应釜中的物料进行抽滤,收集滤液,对超纯水透析48h,取透析袋中的液体冻干后得到固态碳量子点,并置于4℃冰箱中备用。
实施例2
1、将大白菜叶用碎菜机绞碎并与水混合,其中大白菜与水的质量比为100:200。
2、将上述混合液放入高温高压反应釜中进行加热,加热温度为160℃,达到设定温度后恒温时间为0.5h,后时停止加热并自然冷却至室温。
3、取出反应釜中的物料进行抽滤,收集滤液,对超纯水透析48h,取透析袋中的液体冻干后得到固态碳量子点,并置于4℃冰箱中备用。
实施例3
1、将大白菜叶用碎菜机绞碎并与水混合,其中大白菜与水的质量比为100:200。
2、将上述混合液放入高温高压反应釜中进行加热,加热温度为180℃,达到设定温度后恒温时间为0.5h,后时停止加热并自然冷却至室温。
3、取出反应釜中的物料进行抽滤,收集滤液,对超纯水透析48h,取透析袋中的液体冻干后得到固态碳量子点,并置于4℃冰箱中备用。
实施例4
1、将大白菜叶用碎菜机绞碎并与水混合,其中大白菜与水的质量比为100:200。
2、将上述混合液放入高温高压反应釜中进行加热,加热温度为200℃,达到设定温度后恒温时间为0.5h,后时停止加热并自然冷却至室温。
3、取出反应釜中的物料进行抽滤,收集滤液,对超纯水透析12h,取透析袋中的液体冻干后得到固态碳量子点,并置于4℃冰箱中备用。
实施例5
1、将大白菜叶用碎菜机绞碎并与水混合,其中大白菜与水的质量比为100:200。
2、将上述混合液放入高温高压反应釜中进行加热,加热温度为220℃,达到设定温度后恒温时间为0.5h,后时停止加热并自然冷却至室温。
3、取出反应釜中的物料进行抽滤,收集滤液,对超纯水透析48h,取透析袋中的液体冻干后得到固态碳量子点,并置于4℃冰箱中备用。
实施例6
1、将大白菜叶用碎菜机绞碎并与水混合,其中大白菜与水的质量比为100:300。
2、将上述混合液放入高温高压反应釜中进行加热,加热温度为200℃,达到设定温度后恒温时间为0.5h,后时停止加热并自然冷却至室温。
3、取出反应釜中的物料进行抽滤,收集滤液,对超纯水透析48h,取透析袋中的液体冻干后得到固态碳量子点,并置于4℃冰箱中备用。
实施例7
1、将大白菜叶用碎菜机绞碎并与水混合,其中大白菜与水的质量比为100:400。
2、将上述混合液放入高温高压反应釜中进行加热,加热温度为200℃,达到设定温度后恒温时间为0.5h,后时停止加热并自然冷却至室温。
3、取出反应釜中的物料进行抽滤,收集滤液,对超纯水透析24h,取透析袋中的液体冻干后得到固态碳量子点,并置于4℃冰箱中备用。
实施例8
1、将大白菜叶用碎菜机绞碎并与水混合,其中大白菜与水的质量比为100:100。
2、将上述混合液放入高温高压反应釜中进行加热,加热温度为200℃,达到设定温度后恒温时间为0.5h,后时停止加热并自然冷却至室温。
3、取出反应釜中的物料进行抽滤,收集滤液,对超纯水透析48h,取透析袋中的液体冻干后得到固态碳量子点,并置于4℃冰箱中备用。
实施例9
1、将大白菜叶用碎菜机绞碎并与水混合,其中大白菜与水的质量比为100:200。
2、将上述混合液放入高温高压反应釜中进行加热,加热温度为200℃,达到设定温度后恒温时间为1h,后时停止加热并自然冷却至室温。
3、取出反应釜中的物料进行抽滤,收集滤液,对超纯水透析48h,取透析袋中的液体冻干后得到固态碳量子点,并置于4℃冰箱中备用。
实施例10
1、将大白菜叶用碎菜机绞碎并与水混合,其中大白菜与水的质量比为100:200。
2、将上述混合液放入高温高压反应釜中进行加热,加热温度为200℃,达到设定温度后恒温时间为0.1h,后时停止加热并自然冷却至室温。
3、取出反应釜中的物料进行抽滤,收集滤液,对超纯水透析48h,取透析袋中的液体冻干后得到固态碳量子点,并置于4℃冰箱中备用。
实施例11
实施例3制备的大白菜碳点用于检测Fe3+,如图5所示,在大白菜碳点水溶液中加入不同浓度的Fe3+,随着Fe3+浓度逐渐增加(0-400μM),在480nm处的荧光峰强度逐渐降低。
实施例12
将Hela细胞(1mL,4×104细胞/mL)置于玻璃底细胞培养皿中,放入培养箱中培养24h。然后用PBS缓冲液轻轻冲洗3次。将制备好的含有碳点溶液的培养液加入玻璃底细胞培养皿中培养8h。孵育8h后,弃去培养基并用PBS缓冲液洗涤3次,再次加入相应的细胞培养液,然后用于405、488和543nm激光下的CLSM成像。
注意,上述仅为本发明的较佳实施例及所运用技术原理。本领域技术人员会理解,本发明不限于这里所述的特定实施例,对本领域技术人员来说能够进行各种明显的变化、重新调整和替代而不会脱离本发明的保护范围。因此,虽然通过以上实施例对本发明进行了较为详细的说明,但是本发明不仅仅限于以上实施例,在不脱离本发明构思的情况下,还可以包括更多其他等效实施例,而本发明的范围由所附的权利要求范围决定。
Claims (5)
1.一种基于十字花科植物的碳点的制备方法,其特征在于,包括以下步骤:
A、将大白菜叶用碎菜机绞碎并与水混合,其中大白菜与水的质量比为50-200:100-400;
B、将上述混合液放入高温高压反应釜中进行加热,加热温度为140-220℃,达到设定温度后恒温时间为0.1-1h,后时停止加热并自然冷却至室温;
C、取出反应釜中的物料进行抽滤,收集滤液,对超纯水透析12-48h,取透析袋中的液体冻干后得到固态青色荧光碳点,并置于4℃冰箱中备用。
2.根据权利要求1所述的一种基于十字花科植物的碳点的制备方法,其特征在于:所述大白菜与水的质量比为100:400。
3.根据权利要求1所述的一种基于十字花科植物的碳点的制备方法,其特征在于:所述加热温度为200℃,恒温时间为0.5h。
4.根据权利要求1所述的一种基于十字花科植物的碳点的制备方法,其特征在于:所述透析袋使用1kDa,透析时间为48h。
5.根据权利要求1所述的一种基于十字花科植物的碳点的应用,其特征在于:所制青色荧光大白菜碳点用于检测水相中微量Fe3+离子浓度及活细胞多色成像。
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CN108084998A (zh) * | 2018-01-29 | 2018-05-29 | 兴义民族师范学院 | 一种以白兰叶片为碳源的荧光碳量子点及其制备方法 |
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CN108084998A (zh) * | 2018-01-29 | 2018-05-29 | 兴义民族师范学院 | 一种以白兰叶片为碳源的荧光碳量子点及其制备方法 |
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