CN115285975A - 一种可用于环丙沙星快速检测的两亲性碳点的制备方法 - Google Patents
一种可用于环丙沙星快速检测的两亲性碳点的制备方法 Download PDFInfo
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Abstract
本发明属于碳纳米材料制备的技术领域，具体涉及一种可用于环丙沙星快速检测的两亲性碳点的制备方法。制备方法包括如下步骤：步骤1，按比例称取柠檬酸和三羟甲基氨基甲烷在烧杯中，加热一段时间；步骤2，向烧杯中加入油胺，共同加热；步骤3，加热完成后，向烧杯中依次加入甲苯和二次水，搅拌溶液，混合均匀，将混合溶液在离心机中离心；步骤4，离心完成后取出中间层，将中间层放入二次水中进行冷冻干燥，得到两亲性碳点粉末。本发明所制得的碳点在水和有机溶剂中均具有良好的溶解度和分散性；制备得到的碳点对环丙沙星具有专一性识别作用，用于环丙沙星的检测，选择性好，灵敏度高。
Description
技术领域
本发明属于碳纳米材料制备的技术领域，具体涉及一种可用于环丙沙星快速检测的两亲性碳点的制备方法。
背景技术
环丙沙星，作为目前广泛应用的药效最好的氟喹诺酮类抗生素，被用于多种胃肠、泌尿道和呼吸道感染；皮肤和眼部感染,以及与抗厌氧菌组合的腹腔感染治疗。正确使用环丙沙星可以起到灭菌的作用；但是过量使用或使用不当时,会使药物残留在牲畜产品中,人体的中枢神经系统会因环丙沙星的残留而产生不良反应。此外，地表水和地下水也已检测到环丙沙星。其在污水和地表水中的浓度估计为1μg/L，但在医院废水和制药工业废水中的浓度超过150μg/L，其对水生动植物造成重大危害。因此，准确检测环丙沙星具有重要意义。已有的环丙沙星检测方法有高效液相色谱法(HPLC)、分光光度法。但是这些方法均有操作繁琐、成本昂贵和灵敏度低的缺陷。因此建立一种方便快捷、成本低的环丙沙星检测方法是必要的。
碳点(CDs)，作为一种零维纳米材料，由于其良好的生物相容性、环境友好性、易于制备和改性、低毒性等优势被广泛应用于分析检测、药物递送、生物成像等领域。然而，目前报道的碳点多为亲水性碳点，或为亲油性碳点，导致其只能溶于单一性溶剂中且不具备表界面效应。两亲性碳点兼具亲水基团和亲油基团，在极性和非极性溶剂中均有一定溶解度，并具有独特的表界面性质。而两亲性碳点的制备会对复杂的实际环境中的抗生素的检测尤为重要。因此，制备一种两亲性碳点，并将其成功用于抗生素检测具有重要意义。
发明内容
本发明的目的在于提供一种可用于环丙沙星快速检测的两亲性碳点的制备方法。
为了达到上述目的，本发明采用了下列技术方案：
一种可用于环丙沙星快速检测的两亲性碳点的制备方法，包括如下步骤：
步骤1，按比例称取柠檬酸和三羟甲基氨基甲烷在烧杯中，加热一段时间；
步骤2，向烧杯中加入油胺，共同加热；
步骤3，加热完成后，向烧杯中依次加入甲苯和二次水，搅拌溶液，混合均匀，将混合溶液在离心机中离心；
步骤4，离心完成后取出中间层，将中间层放入二次水中进行冷冻干燥，得到两亲性碳点粉末。
进一步，步骤1中所述柠檬酸和三羟甲基氨基甲烷的质量比为6～12:0.1～2。
进一步，步骤1中所述加热一段时间为6～18min。
进一步，步骤2中的加热时间为1min。
一种可用于环丙沙星快速检测的两亲性碳点的制备方法制得的两亲性碳点。
更进一步，所述碳点由C、N、O三种元素组成。
一种可用于环丙沙星快速检测的两亲性碳点的制备方法制得的两亲性碳点在对样品进行环丙沙星检测中的应用。
与现有技术相比本发明具有以下优点：
1.本发明操作步骤简单，不需经过表面钝化剂处理或修饰即可得到两亲性碳量子点。
2.本发明所制得的碳点在水和有机溶剂中均具有良好的溶解度和分散性。
3.本发明制备得到的两亲性碳点对环丙沙星具有专一性识别作用，用于环丙沙星的检测，选择性好，灵敏度高。
附图说明
图1为本发明实施例1制备的碳点的透射电镜图(左侧)和粒径分布图(右侧)；
图2为本发明实施例1制备的碳点的红外光谱图；
图3为本发明实施例1制备的碳点的XPS光谱图；
图4为本发明实施例1制备的碳点的荧光激发发射光谱图；
图5为本发明实施例1制备的碳点对各种常见抗生素响应的选择性图；
图6为本发明实施例1制备的碳点对环丙沙星淬灭的荧光光谱图；
图7为本发明实施例1制备的碳点的环丙沙星的浓度在0-50.1μmol/L范围内的线性拟合曲线。
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
一种用于检测环丙沙星的两亲性碳点的制备方法，包括如下步骤：
1)按比例称取柠檬酸和三羟甲基氨基甲烷在烧杯中，加热11min，所述柠檬酸和三羟甲基氨基甲烷的质量比为8:1；
2)向烧杯中加入油胺，共同加热1min；
3)加热完成后，向烧杯中依次加入甲苯和二次水，搅拌溶液，混合均匀，将混合溶液在离心机中离心；
4)离心完成后取出中间层，将中间层放入二次水中进行冷冻干燥，得到两亲性碳点粉末。以硫酸奎宁为参照物，其相对量子产率是0.53。
实施例2
一种用于检测环丙沙星的两亲性碳点的制备方法，包括如下步骤：
1)按比例称取柠檬酸和三羟甲基氨基甲烷在烧杯中，加热13min，所述柠檬酸和三羟甲基氨基甲烷的质量比为6:1.5；
2)向烧杯中加入油胺，共同加热1min；
3)加热完成后，向烧杯中依次加入甲苯和二次水，搅拌溶液，混合均匀，将混合溶液在离心机中离心；
4)离心完成后取出中间层，将中间层放入二次水中进行冷冻干燥，得到两亲性碳点粉末。以硫酸奎宁为参照物，其相对量子产率是0.46。
实施例3
一种用于检测环丙沙星的两亲性碳点的制备方法，包括如下步骤：
1)按比例称取柠檬酸和三羟甲基氨基甲烷在烧杯中，加热6min，所述柠檬酸和三羟甲基氨基甲烷的质量比为10:0.5；
2)向烧杯中加入油胺，共同加热1min；
3)加热完成后，向烧杯中依次加入甲苯和二次水，搅拌溶液，混合均匀，将混合溶液在离心机中离心；
4)离心完成后取出中间层，将中间层放入二次水中进行冷冻干燥，得到两亲性碳点粉末。以硫酸奎宁为参照物，其相对量子产率是0.33。
实施例4
本发明实施例1制备的两亲性碳点的透射电子显微镜(TEM)表征如图1所示。该碳点是准球形颗粒，平均粒径为3.49nm。
实施例5
本发明实施例1制备的两亲性碳点的红外光谱表征如图2所示。该碳点在3406cm-1处峰值对应O-H/N-H伸缩振动。2923cm-1和1445cm-1处峰值对应C-H和C-N拉伸振动。1771cm-1处峰值对应C＝O的拉伸振动，1578cm-1处峰值归属于N＝O弯曲振动，1071cm-1处峰值归属于C-O的弯曲振动。
实施例6
本发明实施例1制备的两亲性碳点的X射线光电子能谱(XPS)表征如图3所示。表明该碳点由C、N、O三种元素组成。
实施例7
本发明实施例1制备的两亲性碳点在二甲亚砜中的荧光光谱如图4所示。该两亲性碳量子点的最大激发发射波长分别为329nm、406nm。
实施例8
本发明实施例1制备的两亲性碳点对环丙沙星的选择性如图5所示，在同浓度不同抗生素的影响下，环丙沙星对于碳点的荧光猝灭程度最大，荧光强度最小，表明两亲性碳量子点对环丙沙星具有好的选择性。
实施例9
本发明实施例1制备的两亲性碳点对环丙沙星的检测如图6和图7所示，其线性范围为0～16.7μmol/L和16.7～50.1μmol/L，检出限为0.14μmol/L。
实施例10
本发明实施例1制备的两亲性碳点对牛奶和盐酸环丙沙星滴眼液中环丙沙星的检测如表1和表2所示。测定牛奶中环丙沙星含量的实验结果如表1所示，其回收率在98.2％～102.3％之间，RSD值在0.47％～1.59％之间，测定盐酸环丙沙星滴眼液中环丙沙星含量的实验结果如表2所示，其回收率在97.1％～101.6％之间，RSD值在1.09％～2.06％之间，表明了该方法的准确性，即该方法可对实际样品的进行检测应用。
表1为实施例1制备的碳点测定牛奶中环丙沙星
表2为实施例1制备的碳点测定盐酸环丙沙星滴眼液中环丙沙星
本发明说明书中未作详细描述的内容属于本领域专业技术人员公知的现有技术。尽管上面对本发明说明性的具体实施方式进行了描述，以便于本技术领域的技术人员理解本发明，但应该清楚，本发明不限于具体实施方式的范围，对本技术领域的普通技术人员来讲，只要各种变化在所附的权利要求限定和确定的本发明的精神和范围内，这些变化是显而易见的，一切利用本发明构思的发明创造均在保护之列。
Claims (7)
1.一种可用于环丙沙星快速检测的两亲性碳点的制备方法，其特征在于：包括如下步骤：
步骤1，按比例称取柠檬酸和三羟甲基氨基甲烷在烧杯中，加热一段时间；
步骤2，向烧杯中加入油胺，共同加热；
步骤3，加热完成后，向烧杯中依次加入甲苯和二次水，搅拌溶液，混合均匀，将混合溶液在离心机中离心；
步骤4，离心完成后取出中间层，将中间层放入二次水中进行冷冻干燥，得到两亲性碳点粉末。
2.根据权利要求1所述的一种可用于环丙沙星快速检测的两亲性碳点的制备方法，其特征在于：步骤1中所述柠檬酸和三羟甲基氨基甲烷的质量比为6～12:0.1～2。
3.根据权利要求1所述的一种可用于环丙沙星快速检测的两亲性碳点的制备方法，其特征在于：步骤1中所述加热一段时间为6～18min。
4.根据权利要求1所述的一种可用于环丙沙星快速检测的两亲性碳点的制备方法，其特征在于：步骤2中的加热时间为1min。
5.根据权利要求1～4任意一项所述的一种可用于环丙沙星快速检测的两亲性碳点的制备方法制得的两亲性碳点。
6.根据权利要求5所述的方法制得的两亲性碳点，其特征在于：所述碳点由C、N、O三种元素组成。
7.根据权利要求5所述的方法制得的两亲性碳点在对样品进行环丙沙星检测中的应用。
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