CN111732951A - 一种氮掺杂绿色荧光碳量子点及其制备方法和应用 - Google Patents
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Abstract
本发明提供一种氮掺杂绿色荧光碳量子点及其制备方法和应用。制备方法:将多巴胺和乙二胺溶于水中,在170~200℃下反应6~10小时以合成绿色荧光碳点。该方法制备碳点工艺简单,原料来源广泛且价格便宣,制备条件要求低。所制备的碳量子点可作为荧光探针用于比色检测姜黄素。
Description
技术领域
本发明涉及碳发光纳米材料,尤其涉及碳量子点,具体是提供一种氮掺杂绿色荧光碳量子点及其制备方法和应用。
背景技术
姜黄素(curcumin,Cur),1,7-双-(4-羟基-3-甲氧基苯基)-1,6-庚二烯-2,5-二酮,是一种天然多酚色素,来自姜黄的粉状根茎。由于其生物学和药理学活性,如抗氧化,抗癌,抗炎,抗菌和抗糖尿病作用,因此Cur引起了极大的关注。目前用于测定Cur的常规分析方法包括伏安法,高性能薄层层析(HPTLC),高效液相色谱(HPLC),超高效液相色谱(UHPLC),液相色谱-串联质谱(LC-MS/MS)联用和分光光度法。这些方法虽然具有良好的准确性和选择性,然而样品预处理复杂、操作程序繁琐、仪器昂贵、分析时间长等缺点,限制了其应用。而荧光分光光度法由于其高精度,优良的选择性和灵敏度,操作简便,经济快速等特点,已逐渐成为一种高效的检测方法。碳点由于制备方法简便,强烈的光致发光性能、优良的稳定性、水溶性和高选择性等优点,被广泛应用于荧光探针和生物成像等领域。另外比色法具有信号易输出、响应快、操作简单等优点,可实现分析物现场便携检测,但是利用荧光比色法检测姜黄素的文献鲜有报道。因此,制备检出限低、能够比色检测姜黄素的碳点是一种挑战。
发明内容
本发明的目的在于提供一种氮掺杂绿色荧光碳量子点及其制备方法,以及将该碳量子点用于比色检测姜黄素。所述碳点制备工艺简单,原料来源广泛且价格便宣,制备条件要求低且环境友好,在一般实验室均能合成,易于推广。
本发明提供的一种氮掺杂绿色荧光碳量子点的制备方法,包括如下步骤:
将多巴胺和乙二胺混合,加入去离子水;并将该溶液转移至高压釜中,并在170~200℃下反应6~10小时;冷却至室温后,将产物用滤纸过滤除去大分子颗粒,得到的溶液通过500Da的透析膜在去离子水中透析6h;最后,将其真空干燥以收集目标碳量子点;所述的多巴胺、乙二胺和去离子水的质量比为0.01-0.2:1.00-2.00:20。
所述的多巴胺、乙二胺和去离子水的质量比优选0.01-0.1:1.50-2.00:20,更优选0.08-0.1:1.80-2.00:20。
所述的反应温度优选为180~200℃,反应时间优选为9~10小时。
上述方法制备的碳量子点作为荧光探针可用于比色检测姜黄素的检测,根据公式cmin=3Sb/S求出最低检出限为7.887nM,线性范围0.08-185.68uM。
本发明的优点与效果是:
本发明通过一步水热法即可得到碳量子点溶液,合成方法简单有效,原料廉价易得,反应条件温和且环境友好,在一般实验室均能完成,易于推广。所制备的碳量子点作为探针可用于比色检测姜黄素。
附图说明
图1为实施例1制备的碳量子点的紫外吸收光谱及荧光发射光谱。
图2为实施例1制备的碳量子点的红外光谱图,图中横坐标为检测波长,纵坐标为透过率。
图3为姜黄素淬灭实施例1制备的碳量子点的荧光光谱图。
图4为姜黄素的浓度在0.08-185.68uM范围内的线性拟合曲线。
图5为实施例1制备的碳量子点荧光发射曲线随激发波长变化的光谱图。
图6为实施例1制备的碳量子点用于比色检测姜黄素的图。
具体实施方式
下面结合附图以及具体实施例对本发明做出进一步说明,实施例给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。
实施例1
步骤1,室温下,将0.1000g的多巴胺和2mL乙二胺溶于20ml水中,充分搅拌,超声得到澄清溶液。
步骤2,将溶液转移至50ml水热反应釜中。
步骤3,将水热釜置于烘箱中,200℃反应10小时。
步骤4,将产物用滤纸过滤除去大分子颗粒,得到的溶液通过500Da的透析膜在去离子水中透析6h。
步骤5,将上述荧光碳量子点水溶液冷冻干燥后得到荧光碳量子点,其相对量子产率(以硫酸奎宁为标准)为1.6%。
对所制备的荧光碳量子点进行表征:
上述制备的碳量子点的紫外吸收光谱及荧光发射光谱,见图1;
上述制备的碳量子点的红外光谱图见图2,图中横坐标为检测波长,纵坐标为透过率;
用姜黄素淬灭上述制备的碳量子点的荧光光谱见图3;
姜黄素的浓度在0.08-185.68uM范围内的线性拟合曲线见图4;
上述制备的碳量子点荧光发射曲线随激发波长变化的光谱见图5。
实施例2
除四硼酸钠的质量为0.0600g,其它均与实施例1相同。其相对量子产率(以硫酸奎宁为标准)为0.52%。
实施例3
除四硼酸钠的质量为0.0800g,其它均与实施例1相同。其相对量子产率(以硫酸奎宁为标准)为1.02%。
实施例4
除反应时间为180℃10小时,其它均与实施例1相同。其相对量子产率(以硫酸奎宁为标准)为0.97%。
实施例5
取1mL二次水与1mL的实施例1制备的碳量子点水溶液混合,在线性范围内加入不同浓度的姜黄素溶液,在日光下可以看到溶液颜色的改变。因此,可以用于比色检测姜黄素。
Claims (6)
1.一种氮掺杂绿色荧光碳量子点的制备方法,其特征在于,包括如下步骤:
将多巴胺和乙二胺混合,加入去离子水;并将该溶液转移至高压釜中,并在170~200℃下反应6~10小时;冷却至室温后,将产物用滤纸过滤除去大分子颗粒,得到的溶液通过500Da的透析膜在去离子水中透析6h;最后,将其真空干燥以收集目标碳量子点;所述的多巴胺、乙二胺和去离子水的质量比为0.01-0.2:1.00-2.00:20。
2.如权利要求1所述的氮掺杂绿色荧光碳量子点的制备方法,其特征在于,所述的多巴胺、乙二胺和去离子水的质量比为0.01-0.1:1.50-2.00:20。
3.如权利要求2所述的氮掺杂绿色荧光碳量子点的制备方法,其特征在于,所述的多巴胺、乙二胺和去离子水的质量比为0.08-0.1:1.80-2.00:20。
4.如权利要求1所述的氮掺杂绿色荧光碳量子点的制备方法,其特征在于,所述的反应温度为180~200℃,反应时间为9~10小时。
5.如权利要求1-4任一项所述方法制备的氮掺杂绿色荧光碳量子点。
6.如权利要求5所述的氮掺杂绿色荧光碳量子点用于比色检测姜黄素。
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